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Page 1: March 2010 - uni- · PDF fileMarch 2010 Analytical tasks ... (ABA), 11-keto- -boswellic acid (KBA) ... quantification of the four major boswellic acids in Boswellia ser-rata extracts

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CAMAG BIBLIOGRAPHY SERVICECBS

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Analytical tasks – efficiently solved by HPTLC

Boswellia resin

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1

CAMAG BIBLIOGRAPHY SERVICE

No. 104, March 2010CAMAG Bibliography Service Planar Chromatography Edited by Gerda Morlock [email protected] published by CAMAG Switzerland

CAMAG (Switzerland) Sonnenmattstr. 11 • CH-4132 Muttenz 1 Tel. +41 61 4673434 • Fax +41 61 4610702 [email protected] • www.camag.com

CAMAG Scientific Inc. (USA) 515 Cornelius Harnett Drive Wilmington, NC 28401 Phone 800 334 3909 • Fax 910 343 1834 [email protected] • www.camagusa.com

IN THIS ISSUE

Procedures, applicationsA comparison between HPLC and HPTLC for the separation and quantification of boswellic acids in Boswellia serrata extracts ......... 2–4

Validated HPTLC method for skin lipids ............................... 5–6

Separation of common plant triterpenoids by HPTLC ........ 7–9

Validated determination of secoisolariciresinol diglucoside in flaxseed by HPTLC ................. 10–12

Determination of aloe vera gels in cosmetics .............................. 13–15

Products featured in this issue

Horizontal Developing Chamber ....... 11

Automatic TLC Sampler (ATS 4) ........ 15

New TLC Scanner 4 ....................... 16

Column: Know CAMAGOnline Coupling of HPTLC-MS on the road to success ...................... 8

Printed on FSC/PEFC-certified paper

Planar Chromatography in Practice

A comparison between HPLC and HPTLC for the separation and quantification of boswellic acids in Boswellia serrata extracts

The Department of Standardization and New Technologies of the Saint Petersburg Institute of Pharmacy was introduced in CBS 102. In their daily routine, HPTLC is especially helpful for the optimization of the extraction, determination of antiradical activity, or the study of the kinetics of active metabolites in plasma. They currently use more than 20 validated, quan-titative HPTLC methods, such as quantification of chlorogenic, caffeic and ferulic acids in coffee bean extracts, curcuminoids in plasma and dosage forms, bile acids and cholesterol in the bile of rats, etc.

IntroductionBoswellia serrata Roxb. (Indian frankincense) is an Indian medical plant and its gum resin is used as an antipyretic, analgesic, diuretic, or antidysenteric traditional medicine, among other usages. The anti-inflammatory and an-tiarthritic activity of its extracts has been tested in animal experiments and in clinical trials [1, 2]. The main active compounds of Boswellia serrata ex-tracts are triterpenic acids [2] like -boswellic acid (BA), acetyl--boswellic acid (ABA), 11-keto--boswellic acid (KBA) and acetyl-11-keto--boswellic acid (AKBA). For the analysis of boswellic acids, a nonaqueous titration method [3], HPLC [4], GC–MS [5], LC–MS [6], and HPTLC methods [7] have been reported.

The aim of this work was to compare the capabilities of two chro-matographic methods, HPTLC and HPLC, for identification and quantification of the four major boswellic acids in Boswellia ser-rata extracts.

Left to right: Prof. Alexander Shikov*, Dr. Olga Pozharitskaya, Dr. Svetlana Ivanova, Prof. Valery Makarov, Dr. Vera Kosman

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CBS 104 3

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Chromatogram layer and HPLC column• HPTLC plates silica gel 60 F254, 10 x 10 cm (Merck).

• HPLC column Luna C18 (150 x 4.6 mm, 5 µm, Phenomenex, USA) and a SecurityGuard 20-mm precolumn with the same sorbent

Standard solutionsMethanolic solutions (0.5 mg/mL) of BA, ABA, KBA, and AKBA were used.

Sample preparationCommercially available standardized Boswellia ser-rata extracts were a kind gift from New Ambadi Estates Pvt. Ltd. (Chennai, India). Sample solutions were prepared by dissolving of the Boswellia serrata extracts in methanol (10 mg/mL).

Sample application and HPLC injection• Bandwise with Linomat 5, band length 6 mm, dis-

tance from lower edge 10 mm, distance on both sides min. 10 mm, application volumes 1–20 µL

• Injection volume of 20 µL for HPLC analysis

Chromatography• In the Twin-Trough Chamber pre-saturated (for

15 min, using wetted filter paper) with n-hexane – ethyl acetate – glacial acetic acid 16:5:1 up to a migration distance of 7 cm (ca. 10 min)

• HPLC (Waters Inc., USA) consisting of two 510 series pumps, an automated gradient controller and a 484 model tunable absorbance detector. Separation was carried out at room temperature with a flow rate of 1 mL/min using a 20-min linear gradient from 75 % to 100 % acetonitrile (other phase: 0.03 % aqueous trifluoroacetic acid solu-tion), followed by a 15-min isocratic step.

Densitometry• Absorption measurement at 254 nm for KBA and

AKBA, and after derivatization at 560 nm for BA and ABA using TLC Scanner 3 and winCats soft-ware.

• HPLC-UV detection at 254 nm for KBA and AKBA and at 210 nm for BA and ABA.

Post-chromatographic derivatizationFor visualization of BA and ABA, the plate was manu-ally dipped in anisaldehyde sulfuric acid reagent (1 mL anisaldehyde and 2 mL conc. sulfuric acid in 100 mL glacial acetic acid) followed by heating at 110 °C for 5 min on the TLC plate heater.

Note (editor): Using automated immersion by the TLC Chroma-togram Immersion Device (immersion time 1 s, vertical speed 3.5 cm/s) will improve the precision.

HPTLC densitogram at 254 nm of BA (track 1), ABA (track 2), AKBA (track 3), KBA (track 4), and two B. serrata extracts (track 5 and 6)

Visualization by anisaldehyde sulfuric acid reagent: tracks 1 and 2 B. serrata extract at 5 and 10 µg/band, track 3 BA, and track 4 ABA

Results and discussionFor both methods, quantification of boswellic acids by external standard calibration was performed, and both methods were validated according to the ICH guidelines on the validation of analytical methods. Using a 20-µL volume for injection in HPLC, the limits of detection (LOD) for KBA and AKBA were

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4 CBS 104

The two methods treated as paired data were compared by the matched pair Student‘s t-test. The calculated t-values were between 2.16 and 2.45 for the different boswellic acids and below the t-table value of 2.57. Hence, it was concluded that both methods gave identical results for the analysis of boswellic acids in the extracts. There was no statisti-cally significant difference (P = 99 %) between the mean values for all extracts. Considering the fast analysis time, low solvent consumption and high sample throughput capacity, HPTLC is the method of choice for routine analysis.

Results of HPLC and HPTLC quantification of boswellic acids in Boswellia extracts

Compound Sample 1 (%, w/w)a Sample 2 (%, w/w)a

HPLC HPTLC HPLC HPTLC

BA 18.9 ± 1.2 19.0 ± 1.7 22.4 ± 0.7 23.4 ± 1.9

ABA 11.9 ± 1.2 12.4 ± 1.4 11.6 ± 0.3 12.3 ± 1.2

KBA 3.8 ± 0.6 3.4 ± 0.1 8.0 ± 0.1 7.7 ± 0.1

AKBA 3.9 ± 0.7 3.6 ± 0.1 5.1 ± 0.2 5.2 ± 0.1

Total 38.5 37.9 47.1 48.6

a ± standard deviation (n = 3) expressed on dry weight

Boswellic acids:

BA with R = a-OH KBA with R = a-OH

ABA with R = a-CH3COO AKBA with R = a-CH3COO

Further information is available on request from the authors.

[1] T. Syrovets et al. J. Immunol. 174 (2005) 498

[2] B.A. Shah et al. Nat. Prod. Rep. 26 (2009) 72

[3] R.K. Gupta et al. Indian Drugs 21 (1984) 523

[4] B. Buchele and T. Simmet J. Chromatography B 795 (2003) 355

[5] A. Kaunzinger et al. J. Pharm. Biomed. Anal. 28 (2002) 729

[6] K. Reising et al. Anal. Chem. 77 (2005) 6640

[7] O.N. Pozharitskaya et al. J. Sep. Sci. 29 (2006) 2245

* Prof. Dr. Alexander Shikov, Saint Petersburg Institute of Phar- macy, 47/5, Piskarevsky prospect, 195067, St. Petersburg, Russia, [email protected]

6–8 ng and for BA and ABA 60–80 ng. In HPTLC just a 2-µL volume was applied. LOD obtained were 150 ng for KBA and AKBA and 100 ng for BA and ABA. If required, LOD can be improved using a higher volume for application. Regarding precision, the relative standard deviations (%RSD) of boswellic acids varied from 6 to 18 % using HPLC. For HPTLC, %RSD of AKBA and KBA were ≤ 2 %, and after derivatization, for BA and ABA about 10 %, which could be improved by automated immersion.

Two differently marketed, dry Boswellia serrata extracts were analyzed in triplicate using both methods.

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CBS 104 5

CAMAG Laboratory: Method Development in Practice

Validated HPTLC method for skin lipids

Karin Rothenbühler

In cooperation with the University of Basel and under supervision of Prof. Matthias Hamburger, Ms. Karin Rothenbühler has worked on her master thesis [1] in Pharmaceutical Biology at the CAMAG laboratory.

IntroductionEven though numerous literature references indi-cate that TLC/HPTLC is the method of choice for skin lipid analysis, no validated quantitative HPTLC method was found. Following the recent publica-tion on the HPTLC analysis of phospholipids [2], Ms. Rothenbühler developed and validated a HPTLC method for the most important markers of non-polar lipid classes of the human stratum corneum: squalene, triolein, palmitic acid, 1,2-dipalmitoyl-sn-glycerol, stearyl palmitate, cholesteryl palmitate, and cholesterol.

In combination with appropriate sampling procedures the method was rapid, robust and reliable for use by the R&D laboratories of cosmetic industry. The advantages of HPTLC, in comparison to RP-HPLC, are its simple derivati-zation as a prerequisite for lipid detection and the separation based on functional groups.

Sample preparationSkin samples were obtained from the inner forearm of volunteers either by direct extraction with etha-nol, abrasion of a defined area with a razor blade or with Epiglu, a tissue adhesive for medicinal use.

Standard solutions2 mg each of squalene, triolein, palmitic acid, 1,2-dipalmitoyl-sn-glycerol, stearyl palmitate, cholesteryl palmitate, and cholesterol were dissolved in 10 mL of

chloroform – methanol 1:1. For quantification 1 mL of this solution was diluted with 4 mL of chloroform – methanol 1:1.

Chromatogram layerHPTLC plates LiChrospher silica gel 60 F254 (Merck), 20 × 10 cm, pre-washed by developing with metha-nol followed by drying in an oven at 120 °C for 20 min.

Sample applicationBandwise with ATS4, band length 8 mm, track dis-tance min. 10 mm, distance from lower edge 8 mm, distance from left edge min. 15 mm, application volumes 2–30 µL of samples and 2.5–10 µL of standard solutions.

ChromatographyIn the ADC2 with chamber saturation for 20 min first with toluene to a migration distance of 80 mm followed by drying for 5 min, then with n-hexane, t-butyl methyl ether, acetic acid 80:20:1 to 45 mm. Separation was affected by the plate activity, there-fore plates were conditioned prior to both develop-ments at 33 % relative humidity for 10 min using a saturated solution of magnesium chloride.

Post-chromatographic derivatizationCopper(II) sulfate reagent was prepared by dissolving 20 g Copper(II) sulfate pentahydrate in 200 mL of cooled methanol and then adding 8 mL of sulphuric acid 98 % and 8 mL of orthophosphoric acid 85 %. With the Immersion Device III the plate was dipped for 6 s into the reagent, then dried for 30 s with cold air and finally heated on a plate heater for 30 min at 140 °C.

DensitometryTLC Scanner 3 with winCATS software, absorption measurement at 350 nm.

Results and discussionSince there was no standardized methodology for sampling of human skin samples, various tech-niques were evaluated. Skin samples from the in-ner forearm of volunteers were obtained by use of various commercial tapes, medicinal tissue adhesive,

4

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6 CBS 104

The major challenge involved with the use of tapes and glues was to selectively extract the skin lipids from the carrier ma-terial, whereas the direct application of organic solvents was limited to ethanol to avoid skin irritations. Three sampling methods (direct extraction with ethanol, abrasion, Epiglu) were suitable for quantitative investigations, as neither skin nor glue matrix interfered with the lipid zones. However, standardization of the sampling procedure was still difficult because the depth of skin removed (number of stratum cor-neum layers) was unclear and the area of treated skin was difficult to define; further investigations are under way.

Sampling A) by direct abrasion and B) with Epiglu; track 1: lipid standard mix, 2–7: skin lipid samples, 8–9: Epiglu blanks

Standards (track 1: cholesterol, 2: triolein, 3: stearyl palmitate*, 4: ceramid VI, 5: squalene, 6: cholesteryl palmitate*, 7: palmitic acid, 8: 1,2 dipalmitoyl-sn-glycerol) and various extracts of skin lipids (track 9: using ethanol, 10: cyclohexane – ethanol 1:9, 11: cyclohexane – ethanol 1:4, 12: n-hexane – methanol 2:3)*encircled, other zones are impurities

abrasion with a razor blade, cold wax, aluminium foil, cling film or by direct application of organic solvents.

The method was validated regarding stability, robustness, pre-cision of RF values and standard determinations as well as linear range. All lipid standards were stable for at least 3 h in chloroform – methanol 1:1 and on the plate prior to development. Stand-ards as well as extracted skin samples were stable during chromatography. The derivatized chromatogram was stable for at least 2 h. The influence of relative humidity on the

Further information is available on request from the authors.

[1] K. Rothenbühler, Master thesis, Institute for Pharmaceutical Biology, University of Basel, 2009

[2] D. Handloser, V. Widmer, E. Reich, J. Liq. Chro-matogr. Rel. Technol. 31 (2008) 1857

separation was evaluated at 5 %, 33 %, 47 %, and 75 % using the ADC 2. For reproducible selectivity, the relative hu-midity must be maintained between 33 % and 47 %. The precision of the RF values of seven compounds was deter-mined between plates (3 plates devel-oped on the same day, followed by one plate each on two different days). Differ-ences of RF values were <0.03 and thus well below the acceptance criterion of <0.05. Precision of measurement (n = 9) was compared on various HPTLC silica gel 60 plates of different layer thickness (100 and 200 µm) and particle shapes (irregu-lar and spherical particles LiChrospher). The HPTLC LiChrospher Si 60 F254S plates with a thickness of 200 µm showed the lowest relative standard deviations (%RSD ≤ 5 %) for all investigated compounds. The linear range for all but two of the selected markers was between 100 and 350 ng/band (40–160 ng for cholesterol, 100–280 ng for 1,2 dipalmitoyl-sn-glyc- erol). Calibration curves showed correlation coefficients of r > 0.9975.

5 1 2 3 4 5 6 7 8 9 10 11 12

6 1 2 3 4 5 6 7 1 2 3 4 5 6 7 8 9

A B

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CBS 104 7

7

continuation on page 9

Planar Chromatography in Practice

Separation of common plant triterpenoids by HPTLC

Left to right: Dr. Irena Vovk*, Dr. Breda Simonovska and Mitja Martelanc

The Laboratory for Food Chemistry at the National Institute of Chemistry in Ljubljana (www.ki.si) is the leading research group in the field of planar chromatography in Slovenia, providing consulting for industry and other institutions. Research and development activities are primarily focused on the field of nutraceuticals and the development of analytical methods based on chromatographic techniques.

IntroductionTriterpenoids represent a large class of secondary metabolites commonly present in plants, especially in leaf and fruit epicuticular waxes. Some of them exhibit beneficial activities, such as anti-inflamma-tory ones. Therefore, they are of emerging impor-tance as constituents of food supplements and functional foods.

In general HPLC is used for determination of trit-erpenoids, but due to their lack of chromophores and numerous possible isomeric structures, the choice of detector and mobile phases has limita-tions. On the other hand, HPTLC is indispensible in the investigation of triterpenoids, because it provides unique separations with a wealth of potential mobile phases and with possibilities for in situ derivatization, which results in char-acteristic specific coloration and fluorescence of the separated bands [1, 2]. In the investigation of triterpenoids in plant extracts, the proposed HPTLC methods enable easy, fast and inexpen-sive screening. Depending on the sample char-acteristics, quantification is possible.

Standard solutionsStandard solutions and mixtures were prepared in n-propanol (0.1 mg/mL).

Sample preparationFresh tomato fruit and fresh leaves of cabbage, rosemary and sage were immersed into dichlo-romethane. Pulverized oak bark was extracted with the same solvent. After filtration and evaporation of the solvent, final test solutions were prepared in n-propanol with concentrations of 5 mg/mL (cab-bage and rosemary leaves), 30 mg/mL (sage leaves), 10 mg/mL (oak bark) and 2 mg/mL (tomato fruit) [2].

Chromatogram layerHPTLC plates silica gel 60 (Merck), 20 x 10 cm, pre-washed by developing in chloroform – methanol 1:1 and HPTLC plates RP18 (Merck), 20 x 10 cm, prewashed by developing in acetone, followed by drying on the TLC plate heater at 110 °C for 10 minutes.

Sample applicationBandwise with Linomat, band length 6 mm, dis-tance from lower plate edge 5 mm, from left edge 12 mm, track distance 10 mm, application volumes as follows: 6 µL (cabbage leaves), 7 µL (rosemary leaves), 5 µL (sage leaves), 4 µL (oak bark), and 6 µL (tomato), for standard solutions 2-8 µL.

ChromatographyIn the Horizontal Developing Chamber with n-hex-ane – ethyl acetate 5:1 on silica gel plate (develop-ing time 15 min), whereby the conditioning tray was covered with the developing solvent, and with ethyl acetate – acetonitrile 3:2 or acetone – acetonitrile 5:1 on RP18 plate (developing time 17 min), run-ning distance 8 cm

Post-chromatographic derivatizationDried plates were dipped for 2 s in anisaldehyde sul-furic acid reagent (16 mL sulfuric acid and 1 mL p-methoxybenzaldehyde were added to 20 mL acetic acid and 170 mL methanol during cooling with ice water) using the Chromatogram Immersion Device (vertical speed 3.5 cm/s), dried in a stream of warm air and heated at 110 °C with a TLC Plate Heater for

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8 CBS 104

Know CAMAG

Online Coupling of HPTLC-MS on the road to success

Success obliges!

CAMAG will offer the same type of seminars in 2010

• 16.04.2010 University of Oldenburg, Prof. Dr. Christoffers, 26111 Oldenburg, Germany

• 03.06.2010 University of Leiden, Prof. Dr. Overkleeft, 2333 CC Leiden, The Netherlands

• 04.06.2010 University of Gent, Prof. Dr. De Spiegeleer, 9000 Gent, Belgium

• 29.06.2010 Technical University of Munich, Prof. Dr. Schieberle, 85345 Munich, Germany

If you are interested please register by E-mail ([email protected]). You will receive detailed information. Attendance is free of charge.

The one-day seminars announced in CBS 102 met with great interest. Between 30 and 35 analysts attended each of the seminars held in 2009 at Langenau, Offenburg, Münster, Berlin, Basle and Vienna. The participants came from companies and institutes where TLC/HPTLC analysis is a part of the daily routine in foods, pharmaceuticals, water, organic synthesis and natural products’ research. The seminar’s aim was to keep the participants informed on the innovative technique of online coupling and its potential.

Competent speakers reported of their own experi-ence: Dr. H. Luftmann (University of Münster), who developed the interface, reported of the history and background and his experience with its application in organic synthesis. Dr. W. Schulz (Zweckverband Landeswasserversorgung in Langenau) presented the use of HPTLC-MS coupling for identification of organic trace substances in raw and drinking water, Prof. Dr. H.-R. Schmutz (University Northwest Switzerland in Muttenz) lectured on HPTLC-MS of drug compounds and plant ingredients and PD Dr. Gerda Morlock (University of Hohenheim in Stutt-gart) covered applications in the field of food and pharmaceutical analysis. A wide range of analytes of different structural groups was shown such as atrazine and its metabolites, metoprolol and its

degradation products, caffeine, paracetamol, ace-tylsalicyl acid, ginsenoides, isopropylthioxanthone, food dyes, ergotamine, pyridinol and harmane.

In the afternoon there were practical demonstra-tions of the interface with the MS systems available in the respective laboratories. Some participants brought sample chromatograms which were suc-cessfully processed. All participants were convinced of the great potential of the new coupling tech-nique with respect to time saving, cost effectiveness and convenience.

8

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Dear friends

The efficient solution of ana-lytical tasks by HPTLC is the focus of this issue. An abso-lute prerequisite is a sound knowledge of the state-of- the-art technique – a con-clusion drawn also by Pro-fessor Coran (p. 5).

HPTLC is now clearly es-tablished in the laboratory, 35 years after the introduc-tion of the high-performance layers. But in the field, industry as well as regulatory laboratories, we meet many customers still using classical TLC layers and old fashioned procedures. To a large extent this is due to the fact that standard ope-rating procedures are based on classical TLC lay-ers, and that substituting an established proce-dure with HPTLC requires a lot of bureaucracy. Nonetheless, even this appears much better than struggling along for years with inadequate proce-dures and more importantly, suboptimal results.

Outriders for teaching state-of–the-art know-ledge should be university institutes. But unfor-tunately, nowhere is it more apparent than at universities that TLC is just rudimentarily presen- ted to students, if at all! CAMAG strives to up- grade the knowledge of contemporary HPTLC at universities by offering seminars. If you, as a teaching person are interested in a CAMAG seminar at your institute, contact us via info@ camag.com.

An opportunity to see first hand the progress in HPTLC is the attendance of the International Sym-posium on High-Performance Thin-Layer Chroma- tography in Basle, July 6th – 8th, 2011 (last yellow page). Make a note!

Sincerely,

Gerda Morlock [email protected]

104

CAMAG LITERATURDIENSTCAMAG BIBLIOGRAPHY SERVICEPLANAR CHROMATOGRAPHY

Liebe Freunde

Das effiziente Lösen analytischer Fragestellungen mit der HPTLC ist Schwerpunkt dieser Ausgabe. Voraussetzung ist, dass das gesamte Instrumen-tarium optimal eingesetzt wird – eine Folgerung, die auch im Beitrag Coran (S. 5) gezogen wird.

Die HPTLC ist heute – 35 Jahre nach Einführung dieser Schichten – längst in der Praxis angekom-men. Unsere zahlreichen Kundenkontakte zeigen allerdings auch, dass ein großer Teil der Prüfvor-schriften in Industrie und Kontrollinstituten noch auf den klassischen DC-Schichten basiert. Dies liegt einerseits am mangelnden Kenntnisstand eines Teils der Anwender, andererseits am büro-kratischen Aufwand, der erforderlich ist, eine DC-Methode auf HPTLC umzustellen. Aber wäre es nicht besser, die noch vorhandenen DC-Metho-den Schritt für Schritt durch die HPTLC mit ihrem großen Potential zu ersetzen, als sich jahrelang im Routinebetrieb mit einer unzulänglichen Prüfvor-schrift abzufinden? Bürokratie darf kein Hemm-schuh für den analytischen Fortschritt sein!

Vorreiter sollten eigentlich die Universitäten sein. Doch gerade dort wird, wenn überhaupt, den Studierenden die Dünnschicht-Chromatographie oft nur in ihrem rudimentären Stand nahe ge-bracht. CAMAG ist bemüht, durch Seminare den Wissensstand zu aktualisieren. Wenn Sie als Lehr- person daran interessiert sind, melden Sie sich bitte unter [email protected]

Eine Gelegenheit, Fortschritte in der HPTLC zu er-fahren, ergibt sich beim International Symposium on High-Performance Thin-Layer Chromatography in Basel vom 6. – 8. Juli 2011 (letzte gelbe Seite). Bitte reservieren Sie sich diesen Termin.

Mit freundlichen Grüssen

Gerda Morlock [email protected]

MARCH

2010

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THE CBS CLASSIFICATION SYSTEM1. Reviews and books

a) Books on TLC b) Books containing one or several chapters on TLC c) Books containing frequent TLC information spread over several chapters of other information

2. Fundamentals, theory and general a) General b) Thermodynamics and theoretical relationship c) Relationship between structure and chrom. behaviour d) Measurement of physico-chemical and related values e) Optimization of solvent systems f) Validation of methods

3. General techniques (unless they are restricted to the application within one or two classification sections) a) New apparatus/techniques for sample preparation b) Separation material c) New apparatus for sample application/dosage d) New apparatus/techniques for chromatogram development e) New apparatus/techniques for pre- or post- chromatographic derivatization f) New apparatus/techniques for quantitative evaluation g) New apparatus/techniques for other TLC steps (distinguished from section 4)

4. Special techniques a) Automation of sample preparation/application b) Automation of complex chromatogram developing techniques c) Automation, computer application in quantitative chromatogram evaluation d) Combination of TLC with other chromatographic techniques e) Combination of TLC with other (non-chromatogra- phic) techniques...MS, IR...etc.

5. Hydrocarbons and halogen derivatives a) Aliphatic hydrocarbons b) Cyclic hydrocarbons c) Halogen derivatives d) Complex hydrocarbon mixtures

6. Alcohols

7. Phenols

8. Substances containing heterocyclic oxygen a) Flavonoids b) Other compounds with heterocyclic oxygen

9. Oxo compounds, ethers and epoxides

10. Carbohydrates a) Mono- and oligosaccharides, structural studies b) Polysaccharides, mucopolysaccharides, lipopolysaccharides

11. Organic acids and lipids a) Organic acids and simple esters b) Prostaglandins c) Lipids and their constituents d) Lipoproteins and their constituents e) Glycosphingolipids (gangliosides, sulfatides, neutral glycosphingolipids)

12. Organic peroxides

13. Steroids a) Pregnane and androstane derivatives b) Estrogens c) Sterols d) Bile acids and alcohols e) Ecdysones and other insect steroid hormones

14. Steroid glycosides, saponins and other terpenoid glycosides

15. Terpenes and other volatile plant ingredients a) Terpenes b) Essential oils

16. Nitro and nitroso compounds

17. Amines, amides and related nitrogen compounds a) Amines and polyamines b) Catecholamines and their metabolites c) Amino derivatives and amides (excluding peptides)

18. Amino acids and peptides, chemical structure of proteins a) Amino acids and their derivatives b) Peptides and peptidic proteinous hormones

19. Proteins

20. Enzymes

21. Purines, pyrimidines, nucleic acids and their constituents a) Purines, pyrimidines, nucleosides, nucleotides b) Nucleic acids, RNA, DNA

22. Alkaloids

23. Other substances containing heterocyclic nitrogen a) Porphyrins and other pyrroles b) Bile pigments c) Indole derivatives d) Pyridine derivatives e) other N-heterocyclic compounds

24. Organic sulfur compounds

25. Organic phosphorus compounds (other than phospholipids)

26. Organometallic and related compounds a) Organometallic compounds b) Boranes, silanes and related non-metallic compounds c) Coordination compounds

27. Vitamins and various growth regulators (non-peptidic)

28. Antibiotics, Mycotoxins a) Antibiotics b) Aflatoxins and other mycotoxins

29. Pesticides and other agrochemicals a) Chlorinated insecticides b) Phosphorus insecticides c) Carbamates d) Herbicides e) Fungicides f) Other types of pesticides and various agrochemicals

30. Synthetic and natural dyes a) Synthetic dyes b) Chloroplasts and other natural pigments

31. Plastics and their intermediates

32. Pharmaceutical and biomedical applications a) Synthetic drugs b) Pharmacokinetic studies c) Drug monitoring d) Toxicological applications e) Plant extracts, herbal and traditional medicines f) Clinico-chemical applications and profiling body fluids

33. Inorganic substances a) Cations b) Anions

34. Radioactive and other isotopic compounds

35. Other technical products and complex mixtures a) Surfactants b) Antioxidants and preservatives c) Various specific technical products d) Complex mixtures and non-identified compounds

36. Thin-layer electrophoresis

37. Environmental analysis a) General papers b) Air pollution c) Water pollution d) Soil pollution

38. Chiral separations

XX. (abstract number underlined) refers to HPTLC related publication or application using HPTLC materials

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1. Reviewsandbooks104001 TaraMCGLINCHEY*,P.A.RAFTER,FionaREGAN,D.GILLIAN,P.MCMAHON(*Depart-

mentofAgriculture,Fisheries&Food,CentralMeatControl,BackwestonLaboratoryComplex,YoungsCross,Celbridge,Co.,Kildare, Ireland):Areviewofanalyticalmethodsfor thedeter-minationofaminoglycosideandmacrolideresiduesinfoodmatrices.Anal.Chim.Acta624(1),1-15(2008).Aminoglycosidesandmacrolidesareimportantantibioticsforveterinarymedicineandarewidelyusedinthetreatmentofbacterialdisease,andasfeedadditivesforgrowthpromo-tion.AsaresulttheEuropeancommissionsetstrictcriteriaformonitoringresiduesandrequirestestingforlowlevelsofaminoglycosidesandmacrolidesinfoods.Thereforethedevelopmentoffast,reliable,andsensitivemethodsfortheextractionandsubsequentanalysisoftheseantibioticsisofgreatinterest.Thereviewdiscussesanalyticalmethodsforbothextractionanddeterminationofantibioticsinvariousfoodmatricesfocusingonthelast10years.Extractionandclean-upme-thodssuchasdeproteinizationandsolid-phaseextractionaredescribed,andvariousscreeningme-thodsincludingTLC,EI,CE,microbiologicalassays,andLCcombinedwithMSarereviewed.agricultural,food,analysis,HPTLC,

review 1,28

2. Fundamentals,theoryandgeneral104002 TatjanaDJAKOVIC-SEKULIC*,NadaPERISIC-JANJIC,EvgenijaDJURENDI(*Department

ofChemistry,FacultyofSciences,UniversityofNoviSad,TrgDositejaObradovia�,21000NoviSad,Serbia):Retentiondatafromreverse-phasehigh-performancethin-layerchromato-graphyincharacterizationofsomebis-salicylicacidderivatives.Biomed.Chromatogr.2�(8),881-887(2009).HPTLCinvestigationofsalicylicacidderivativesonRP-phasewithvariousmethanol-wateranddioxane-waterbinarymixturesinordertoestablishrelationshipsbetweenchromatographicdataandselectedphysico-chemicalparametersthatarerelatedtoADME(absorption,distribution,metabolismandelimination).AlinearcorrelationbetweenRMvaluesandthevolumefractionofmobilephasemodifierwasobserved.TheobtainedRM0valueswerecorrelatedwithlipophilicity,solubility,humanintestinalabsorption,plasma-proteinbinding,andblood-brainbarrierdata.

HPTLC,QSRR,lipophilicity 2

10400� L.KOMSTA*,K.SZTANKE,P.MACZKA,M.UCHEREK,R.SKIBINSKI,A.GUMIENIC-ZEK(*DepartmentofMedicinalChemistry,FacultyofPharmacy,MedicalUniversityofLublin,Jaczewskiego4,20-090Lublin,Poland;[email protected]):Determinationofthelipo-philicityoftwenty-sevenimidazo[2,1-c][1,2,4]triazinederivativeswithstrongbiologicalactivitybyreversed-phaseTLC.ComparisonwithresultsobtainedbyuseofcomputationalalgorithmsJ.PlanarChromatogr.22,�27-��1 (2009)TLCof27novel imidazo[2,1-c][1,2,4]triazinederi-vativestogetherwith12compoundswithknownliteraturelogPvalues(asreferencecalibrationdata) on RP-18 with methanol - water binary mobile phases containing different proportionsofmethanol inhorizontalchamberswithoutchambersaturation.DetectionunderUV254nm.Usingprincipal-componentanalysistheobtainedresultswerecomparedwithresultsfromninecomputationalmethods.

pharmaceuticalresearch,qualitativeidentification 2c

104004 T.SAMUEL*,A.MANIKANDAN,A.SINGH(*CGPSGCollegeofPharmacy,Peelamedu,Coimbatore,India):Standardisationofherbalmedicinebyhigh-performancethin-layerchro-matography.AbstractNo.992�,IHCB(2009).HPTLCofseveralherbalformulations(tabletsextractedwithmethanol)onsilicagelwithtoluene-ethylacetate19:1.Thefingerprintmethodwassuitableforcorrectidentificationandforroutinequalitycontroloftheherbalextracts.

pharmaceuticalresearchqualitycontrol,herbal,HPTLC 2a

104005 M. WAKSMUNDZKA-HAJNOS, D. MATOSIUK, A. PETRUCZYNIK, U. KIJKOWSKA-MURAK*(*MedicalUniversityofLublinDepartmentof InorganicChemistry20-081LublinPoland):DeterminationofthelipophilicityofselectedisoquinolinealkaloidsbyRP-TLC.ActaChromatographica 24 (4), 56�-57� (2008).TLC of nine alkaloids on RP-18 with mixtures of

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aqueousacetoneoraqueousdioxanewithvariousmobilephaseadditives (ammonia,diethyla-mine,or tetrabutylammoniumchloride) inorder tosuppress ionizationof thealkaloidsand/orreduceionicinteractionswithsurfacesilanolgroups.Ion-pairTLConRP-18withaqueousace-tonemixturesandvariousmobilephaseadditives(pentanesulfonicacid,octanesulfonicacid,ordi-(2-ethylhexyl)orthophosphoric acid). Investigation of relationships between RM values andmodifierconcentrationusinga linearsemilogarithmicequationforexperimentaldata tocalcu-latelipophilicityvaluesRMW(RMforpurewater),theslope,andtheinterceptwiththex-axis.Comparisonwithretentiondataofstandardswithknownlipophilicity(logP).

doping 2d,22

3. Generaltechniques104006 V.G.BEREZKIN*,N.Y.KULAKOVA,S.S.KHREBTOVA(*A.V.TopchievInstituteofPetro-

chemicalSynthesis,RussianAcademyofSciences,Leninskypr.29,Moscow,119991,Russia,[email protected]): Three-dimensional thin-layer chromatography on plates with open andclosedadsorption layers.J.PlanarChromatogr.22,�1�-�19(2009).Presentationof twodiffe-rentmethodsof three-dimensionalTLCusingplateswithopenandsealed(closed)adsorptionlayers.Inthesuggestedmethodthecomponentsofthetestdyemixtureinitiallymigrateinthefirst direction, then in the seconddirection (different from thefirst) and in the thirddirection(differentfromfirstandsecond).TLCofdyemixture1(crystalviolet,xylencyanol,neutralblue,bromothymoldarkblue,methanylyellow,acridineorange,indophenol,ariabelred,SudanblueII,SudanIV,dimethylaminoazobenzene)withethanol-aceticacid10:1(1D),acetone(2D),andto-luene(�D)andofmixture2(darkviolet,brightorange,yellow,darkred,violet)onsilicagelwithtetrahydrofurane-benzene9:1(1D),dichloromethane-benzene�:1(2D),andtoluene(�D).

comparisonofmethods �d

104007 X.LIU*,T.KUBO,H.DIAO,J.BENJAMAS,T.YONEMICHI,N.NISHI(*CollegeofMateri-alsandTextiles,KeyLaboratoryofAdvancedTextileMaterialsandManufacturingTechnology,MinistryofEducation,ZhejiangSci-TechUniversity,XiashaHigherEducationZone,Hangzhou�10018,China):DNA/polyvinyl alcohol interpenetratingpolymernetworkas stationaryphaseforthin-layerchromatography.Anal.Biochem.�9�(1),67-72(2009).ADNA/polyvinylalcoholinterpenetratingpolymernetworkwasproducedbycross-linkingpolyvinylalcoholwithglutar-aldehydeandsubsequentcross-linkingofDNAbyUVirradiation.ThepolymerwasthenusedtocoatthesurfaceofporoussilicaparticlesforTLC.ThreetypicalDNA-bindingcompoundsandeightaminoacidenantiomerswereusedasmodelchemicalstoinvestigatethechromatographicbehaviorofthemodifiedTLCphase.Bothclassesofchemicalsprovidedhighseparationeffici-ency.DNA-modifiedTLCphasescouldbeusedforvariousapplicationfields,includingefficacyevaluationofamedicine,toxicityassessmentofapollutantatthemolecularlevel,aswellasse-parationofenantiomersofdyes,aminoacids,peptides,proteins,nucleotides,anddrugs.

stationaryphase �b

104008 S. WANGTHONG*, I.TONSIRIPAKDEE, T. MONHAPHOL, R. NONTHABENJAWAN, S.PATTANAARGSONWANICHWECHARUNGRUANG(*DepartmentofChemistry,FacultyofScience, Chulalongkorn University, Payatai, Bangkok 10��0,Thailand): PostTLC developingtechniquefortyrosinaseinhibitordetection.Bio.Chromatogr.21(1),94-100(2008).ThemethodfordetectionoftyrosinaseinhibitingsubstancesinvolvessprayingoftheTLClayerwithtyrosi-naseandl-tyrosinesolutionssuccessively.Positiveresultsaredetectedaswhitespotsagainstabrownish-purplebackground.Themethodissuitableeitherasaquickscreeningmethodfortyro-sinaseinhibitordetectionorasaguidingprocedureforanisolationoftyrosinaseinhibitorsfrommixturesornaturalproductextracts.Thetechniqueissensitiveenoughforresultsinthepresenceof6ng/zoneglabridin.

review,postchromatographicderivatization �d

4. Specialtechniques104009 P.ABU-RABIE*,N.SPOONER(*PreClinicalDevelopmentDrugMetabolismandPharmaco-

kinetics,GlaxoSmithKlineResearchandDevelopment,ParkRoad,Ware,Hertfordshire,SG12

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ODP,UnitedKingdom;[email protected]):Directquantitativebioanalysisofdrugsindriedbloodspotsamplesusingathin-layerchromatographymassspectrometerinterface.Anal.Chem.81,10275-10284(2009).DirectquantitativebioanalysisofdrugsfromdriedbloodspotsamplesusingaTLC-MSinterfacewithorwithoutHPLCseparation.Themethodgaveacceptab-lesensitivity,linearity,accuracy,andprecisiondataforbioanalyticalvalidations.Thedirecteluti-ontechniquewasshowntoincreaseassaysensitivityforarangeofanalytes.Investigationswereperformed to optimize extraction time, minimize sample-to-sample carry-over, and comparechromatographicperformance.Onthebasisofthispreliminaryassessment,ithasbeendemons-tratedthatthisTLC-MSinterfacehasthepotentialtobeaneffectivetoolforthedirectanalysisofdrugsindriedbloodsamplesatphysiologicallyrelevantconcentrations.

clinicalchemistryresearch 4e

104010 S.-C.CHENG(ChengSy-Chyi),M.Z.HUANG(HuangMin-Zong),J.SHIEA*(ShieaJentaie)(*NationalSunYat-SenUniversity-KaohsiungMedicalUniversityJointResearchCenter,Kaohsi-ung,804,Taiwan;[email protected]):Thin-layerchromatography/laser-inducedacousticdesorption/electrosprayionizationmassspectrometry.Anal.Chem.81,9274-9281(2009).TLCofdyestandards(FD&CGreenNo.�,FD&CRedNo.�,eriochromcyaninR),drugstandards(�,4-methylene-dioxy-N-methamphetamine, lysergicaciddiethylamide,flunitrazepam),andro-semaryessentialoilon1)RP-18with65%acetonecontaining1.5%formicacidand2)onsilicagelwithchloroform-methanol9:1.Rosemaryessentialoilwasalsoseparatedonsilicagelwithtoluene-ethylacetate9:1.DetectionunderUV254nmandindaylight.Thecombinationofla-ser-inducedacousticdesorptionandelectrosprayionizationmassspectrometry(LIAD/ESI/MS)canbeusedtorapidlycharacterizechemicalcompoundsseparatedonaTLCplate.

qualitativeidentification 4e

104011 N.GOTO-INOUE*,T.HAYASAKA,T.TAKI,TaniaVALDESGONZALEZ,M.SETOU(*De-partmentofMolecularAnatomy,HamamatsuUniversitySchoolofMedicine,Hamamatsu,Shi-zuoka4�1-�192,Japan):Anewlipidomicsapproachbythin-layerchromatography-blot-matrix-assistedlaserdesorption/ionizationimagingmassspectrometryforanalyzingdetailedpatternsofphospholipidmolecularspecies.J.Chromatogr.A1216(42),7096-7101(2009).PresentationofaTLC-blot-MALDI-IMSmethodwhichcombinesTLCandIMS(imagingmassspectrometry)foruseinlipidomics.Incomparisonwithcommonstainingmethodsthemethodallowshighlysensitivedetecionofwholelipidsandindividualmolecularspecies.Linearityforalllipidsrangedapproximatelyoveroneorderofmagnitude.Precision(%RSD)was<16%.TheTLCstepallowspreciseseparationofcomplexlipidmixturesintoindividuallipidclassesbeforeMSanalysisisperformed.

qualitativeidentification 4e

104012 E.HARRY,J.REYNOLDS,A.BRISTOW,I.WILSON,C.CREASER*(*CentreforAnalyticalScience,DepartmentofChemistry,LoughboroughUniversity,LoughboroughLE11�TU,UK,[email protected]):Directanalysisofpharmaceutical formulations fromnon-bonded re-verse-phasethin-layerchromatographyplatesbydesorptionelectrosprayionisationionmobilitymassspectrometry.RapidCommun.MassSpectrom.2�,2597-2604(2009).RP-TLCofpharma-ceuticalformulationscontainingparacetamol,ephedrine,codeine,andcaffeineonhydrocarbon-impregnated silicawithmethanol -water1:1.Detectionbydesorptionelectrospray ionization(DESI)combinedwithionmobilitymassspectrometry(IM-MS).Thelimitofdetectionwas9,16,�4,2�9and225µg/cm2forcodeine,caffeine,ephedrineandparacetamol,respectively.

pharmaceuticalresearch,qualitycontrol,qualitativeidentification 4e

10401� L.KOMSTA(DepartmentofMedicinalChemistry,MedicalUniversityofLublin,Jaczewskiego4,20-090Lublin,Poland):Acomparativestudyonseveralalgorithmsfordenoisingofthin-layerdensitograms.Anal.Chim.Acta641(1-2),52-58(2009).Comparisonofclassicalfilteringtech-niques(Savitzky-Golay,AdaptiveDegreePolynomialFilter,Fourierdenoising,ButterworthandChebyshevIIRfilters)andwaveletshrinkage(�1motherwavelets,�thresholdingtechniquesand

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CAMAGBIBLIOGRAPHYSERVICE No.1046

11decompositionlevels)withtheoriginalnoisysignalandareferencesignalwhichwasdenoi-sed experimentallyby averaging64measurements.Thebest similarity to the reference signalwasobtainedwithfilters,howeverthesignalwasslightlyoversmoothed.Thewaveletshrinkagemethodgave lessdenoisedsignals.Therewasasignificant influenceof the thresholding tech-niqueanddecompositionlevel,andbestconditionswereatlevel2or�andsoftthresholding),whereaschangingofthemotherwaveletalmostdidnotchangetheresult.Thepresentedresultscanbeusedasgeneralrecommendationsfordenoisingdensitometricfingerprintsbeforeapply-ingfurtherchemometricalgorithms.Thebestchoiceswere:Savitzky-Golayfilterofappropriatewindowwidth(optimizedagainstautocorrelation)orwaveletshrinkagewithHaarwavelet,softthresholdingandhighdecompositionlevel.

HPTLC,quantitativeanalysis,qualitativeidentification,densitometry 4c

104014 F.SCHULTE, J.MAEDER,L.W.KROH,U.PANNE, JaninaKNEIPP* (*ChemistryDepart-ment,HumboldtUniversitätzuBerlin,Brook-Taylor-Strasse2,12489Berlin,Germany;[email protected]):Characterizationofpollencarotenoidswithinsituandhigh-per-formancethin-layerchromatographysupportedresonantRamanspectroscopy.Anal.Chem.81,8426-84�� (2009). HPTLC of zeaxanthin, cryptoxanthin, beta-carotene, lutein and pollen ex-tractsonsilicagelwithtetrahydofuran-methylenechloride-n-hexanebyautomatedmultipledevelopment.Quantitativedeterminationbyabsorbancemeasurementat425nm,whichhastobeaccomplishedwithin5minafterdevelopmentduetothefastbleachingofthecarotenoidcolor.TheanalysisofcarotenoidsinpollenextractswasconfirmedbyresonanceRamandatameasureddirectlyontheHPTLCplates.

HPTLC,AMD,densitometry,quantitativeanalysis,biochemicalresearch4e,�0b

104015 M.SHARIATGORJI,Z.SPACIL,G.MADDALO,L.CARDENAS,L.ILAG*(*DepartmentofAnalyticalChemistry,StockholmUniversity,10691Stockholm,Sweden,[email protected]):Matrix-freethinlayerchromatography/laserdesorptionionizationmassspectrometryforfacileseparationandidentificationofmedicinalalkaloids.RapidCommun.MassSpectrom.2�,�655-�660(2009).TLCofberberineandpalmatineinrootsofBerberisbarandanaonsilicagelwithbutanol-aceticacid-water14:�:4.DetectionunderUV�66nm.Bandswerecutoutforfurtheranalysisbylaserdesorptionionizationmassspectrometry.ThehRFvalueofberberineandpalmatinewas56and46,respectively.

herbal,qualitativeidentification 4e

104016 C.SIMOES-PIRES,B.HMICHA,A.MARSTON,K.HOSTETTMANN*(*LaboratoryofPhar-macognosyandPhytochemistry,UniversityofGeneva,1211Geneva4,Switzerland,[email protected]):ATLCbioautographicmethodforthedetectionofalpha-andbeta-glucosidaseinhibitors inplant extracts.Phytochem.Anal. 20,511-515 (2009).Bioautographyof alpha-D-glucosidase (1) and beta-D-glucosidase (2) in buffer solution (sodium acetate 4.1 % in waterpH=7.5)sprayedontoasilicagelplate.Incubationatroomtemperaturefor60minfor(1)andat�7°Cfor20minfor(2).Fordetectionoftheactiveenzyme,solutionsof2-naphthyl-alpha-D-glucopyranosideor2-naphthyl-beta-D-glucopyranosideandFastBluesaltweremixedataratioof1:1for(1)or1:4for(2),andsprayedontotheplatetogiveapurplebackgroundcolorationafter2-5min.MethanolextractsoftheaerialpartsofTussilagofarfaraandUrticadioicaweretestedasenzymeinhibitorsandvisualizedaswhitespotsontheTLCplates.

pharmaceuticalresearch,herbal,qualitativeidentification,AMD,bioautography 4e

104017 G.STUBIGER,E.PITTENAUER,O.BELGACEM,P.REHULKA,K.WIDHALM,G.ALL-MAIER* (*InstituteofChemicalTechnologies andAnalytics,ViennaUniversityofTechnolo-gy,1060Vienna,Austria,[email protected]):Analysisofhumanplasmalipidsandsoybeanlecithinbymeansofhigh-performancethin-layerchromatographyandmatrix-assistedlaserdesorption/ionizationmassspectrometry.RapidCommun.MassSpectrom.2�,2711-272�(2009).HPTLC in combinationwithmatrix-assisted laserdesorption/ionizationmass spectro-metry(MALDI-MS)wasusedfortheanalysisofcomplexlipidmixtures.Fortheseparationof

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lipidsone-dimensionalHPTLConsilicagelaluminumfoilwasusedwithatwo-phasemobilephase.ThecombinationwithMALDI-MSallowedtheidentificationof70distinctlipidspeciesandtheanalysisofevenminorlipidclassesfromonlyverysmallvolumesofhumanplasma(50µL).

pharmaceuticalresearch,clinicalchemistryresearch,foodanalysis,HPTLC,quantitativeanalysis 4e

5. Hydrocarbonsandhalogenderivatives104018 I.BELAI*,G.OROS,B.BORDAS(*PlantProtectionInstitute,HungarianAcademyofSciences,

1525Budapest,P.O.Box102,Hungary;[email protected]):Quantitativestructure-retentionrelation-shipand�Dmolecularmodelingstudiesintheunusualchromatographicbehavioroftriphenyl-methanederivativesinRPTLCsystems.J.PlanarChromatogr.22,255-26�(2009).TLCof25triphenylmethanederivativesusingparaffinoil-coatedsilicagelandacetone-watermixtures,inwhichtheacetonecontentvariedbetween40and70%inincrementsof10%.DualretentionbehaviorisobservedfortriphenylmethanederivativesinreversedphaseHPTLCwhenthecom-positionofacetone-watermobilephaseisvaried.Thephysicochemicalandmolecularpropertiesoftriphenylmethanederivativesleadtoanunusualretentionbehavior,whichwasinvestigatdbytraditionalquantitativestructure-retentionrelationshipmodelingandby�Dmolecularmodeling.Lipophilicitywasfoundtobethemostimportantmolecularpropertygoverningtheretentionoftriphenylmethanederivatives.

qualitativeidentification 5b

8. Substancescontainingheterocyclicoxygen104019 H.M.KURTBAY,I.KAYNAK,S.S.BOZKURT,M.MERDIVAN*(*DepartmentofChemistry,

DokuzEylulUniversity,FacultyofScienceandArts,�5160 Izmir,Turkey;[email protected]):DensitometricHPTLCanalysisof the5-hydroxymethylfurfural contentofTurkishfruitwinesandvinegars.J.PlanarChromatogr.22,�6�-�66(2009).HPTLCof5-hydroxymethyl-furfuralinsevenTurkishfruitwinesandthreeTurkishvinegarsonsilcagelwithtoluene-ethylacetate-90%formicacid6:�:1inatwintroughchambersaturatedfor20min.Quantitativede-terminationbyabsorbancemeasurementat286nm.Thelimitofdetectionandquantificationwas0.05and0.1�ng/mL,respectively.

foodanalysis,toxicology,HPTLC,densitometry,quantitativeanalysis 8b

9. Oxocompounds,ethersandepoxides104020 PetraJAZBEC*,A.SMIDOVNIK,M.PUKLAVEC,M.KRIZMAN,J.SRIBAR,L.MILIVOJE-

VIC,M.PROSEK(*DepartmentofFoodChemistry,NationalIntituteofChemistry,Ljubljana,Slovenia;[email protected]):HPTLCandHPLC-MSquantificationofcoenzymeQ10andcho-lesterolinfractionatedchicken-breasttissue.J.PlanarChromatogr.22,�95-�98(2009).HPTLCofcoenzymeQ10,cholesterolandbiologicalextractsonsilicagelwithpetroleumether-diethylether-aceticacid85:15:1.Detectionbydippinginto5%phosphomolybdicacidinethanolfor10sfollowedbyheatingfor10minat110°C.Quantitativeevaluationinvisiblelight.

foodanalysis,HPTLC,quantitativeanalysis,densitometry,biochemicalresearch 9,20

10. Carbohydrates104021 T.BERNARDI,ElenaTAMBURINI*(*DepartmentofChemistry,UniversityofFerrara,ViaL.

Borsari46,44100Ferrara,Italy;[email protected]):AnHPTLC-AMDmethodforunderstandingthemetabolic behavior of microorganisms in the presence of mixed carbon sources.The case ofBifidobacterium adolescentis MB 2�9. J. Planar Chromatogr. 22, �21-�25 (2009). HPTLC ofglucose,fructose,galactose,lactose,raffinose,1-kestose,nystose,andfructosyl-nystoseondiolphasebyautomatedmultipledevelopmentwithacetonitrile-acetone-waterandacetonitrile-water.Preliminaryisocraticdevelopmentswereperformedat22-25°Cat65-75%relativehumi-dityinatwintroughchamber.Detectionbyvaporizationwith�7%hydochloricacidvaporfor�0minfollowedbydippingin4-aminobenzoicacid.Quantitativedeterminationbyfluorescencemeasurementat�1�nm.

HPTLC,densitometry,quantitativeanalysis,AMD,biochemicalresearch 10a

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104022 J. STROKA*, I. DONCHEVA, B. SPANGENBERG (*European Commission Joint ResearchCentre,InstituteforReferenceMaterialsandMeasurements,FoodSafetyandQualityUnit,Re-tieseweg111,2440Geel,Belgium; [email protected]):Determinationofsucralose insoftdrinksbyhigh-performancethin-layerchromatography:Interlaboratorystudy.J.AOACInt.92,115�-1159 (2009).HPTLCofsucraloseonaminophasewithacetonitrile -water4:1 inahorizontalorstandarddevelopmentchamberwithoutchambersaturation.Fordetectiontheplatewasheatedat190°Cfor20min,eitherinadryingovenoronatemperature-controlledheatingplate.Quantitativedeterminationbyabsorbanceandfluorescencemeasurementat254nm.Theresultsoftheinterlaboratorycomparisonshowgoodprecisioncharacteristics.Thefluorescencemeasurementsofthesucralosederivativesindicatedbettermethodperformance,comparedwithabsorbancemeasurementsintheUV.

foodanalysis,qualitycontrol,HPTLC,quantitativeanalysis,densitometry 10a

11. Organicacidsandlipids10402� RituARORA*,B.SINGH,R.SINGH,C.KATIYAR(*GuruNanakDevUniversity,Amritsar,

Punjab,India):ValidatedHPTLCmethodforthedeterminationofcinnamicacidincrudeplantmaterials,herbalextractsandpharmaceuticaldosageformscontainingCinnamomumcassia.60thIndianPharmaceuticalCongressPA-214(2008).HPTLCofcinnamicacid(inplantrawmaterial,herbalextractsandpharmaceuticaldosageforms)onsilicagelwithchloroform-methanol4:1inasaturatedtwintroughchamberatroomtemperature(25°C).Quantitativedeterminationbyabsorbancemeasurementat277nm.ThehRFvalueforcinnamicacidwas50.Themethodwaslinearintherangeof700-1400ng/spot.

pharmaceuticalresearch,herbal,HPTLC,densitometry,quantitativeanalysis 11a

104024 F.HASAN*,R.KHAR,F.AHMAD,M.ALI,M.RAZA(*Dept.ofPharmaceutics,JamiaHam-dard, Hamdard Nagar, New Delhi, India): Development of novel high-performance thin-layerchromatographymethodforestimationoflipidineggoil.AbstractNo.F-282,61st(2009).HPT-LCoflipidsonsilicagelinasaturatedtwintroughchamberwithcarbontetrachloride-methanol-aceticacid270:�0:11atroomtemperature(25°C).Quantitativedeterminationbyfluorescencemeasurementat�66nm.ThehRFvalueofcholesterolwas�5.Thecalibrationcurveshowedgoodlinearrelationshipwithr2=0.999intherangeof100-600ng/spot(viapeakarea).

pharmaceuticalresearch,qualitycontrol,HPTLC,quantitativeanalysis 11c

104025 P.HAZAM*,D.SARKAR,B.DEY,S.DAS(*HimalayanPharmacy Institute,Dept.ofPhar-macognosy,Majhotar,Sikkim,India:Ahigh-performancethin-layerchromatographic(HPTLC)method for theestimationof rosmarinicacid fromSalviaofficinalis (sage).60th IndianPhar-maceuticalCongressPG-256(2008).HPTLCof rosmarinicacid inSalviaofficinalisonsilicagelwith toluene -ethylacetate - formicacid5:4:1.Quantitativedeterminationbyabsorbancemeasurementat�28nm.Linearitywas0.1-1.0ng/mL,recoverywas99.4%.ThemethodwasfoundsuitableforroutinequalitycontroloftheSalviaofficinalisrawmaterial.

herbal,environmental,densitometry,HPTLC,quantitativeanalysis 11a

104026 Y. KAWAI*, M. MIYOSHI, J. MOON, J. TERAO (*Department of Food Science, GraduateSchool of Nutrition and Biosciences,The University ofTokushima,Tokushima 770-850�, Ja-pan): Detection of cholesteryl ester hydroperoxide isomers using gas chromatography-massspectrometrycombinedwiththin-layerchromatographyblotting.Anal.Biochem.�60(1),1�0-1�7 (2007). Determination of cholesteryl ester hydroperoxides, especially cholesteryl linole-atehydroperoxideisomers,bycombinationofTLCblottingwithdiphenyl-1-pyrenylphosphinefluorescentdetection(DPPP-TLCblotting)andGC-electronionization-MS(GC-EI-MS).AfterDPPP-TLCblottingofcholesterylesterhydroperoxidesfluorescentzoneswereobtianedwhichwereextractedandderivatizedbyhydrogenation,transmethylation,andtrimethylsilylation.Theresultingmethylester/trimethylsilyletherderivativesofhydroxyoctadecenoicacidwerethenana-lyzedbyGC-EI-MSusingselectedionmonitoringofisomer-specificfragmentionsoriginatingfromthealpha-cleavageofthetrimethylsilyloxylgroup.

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CAMAGBIBLIOGRAPHYSERVICE No.1049

agricultural,clinicalroutineanalysis,postchromatographicderivatization,qualitativeidentification,quantitativeanalysis 11

104027 H.LI(LiHaixing)*,T.QIU(QiuTing),Y.CAO(CaoYusheng),J.YANG(YangJiyan),Z.HU-ANG(HuangZhibing)(*Sino-GermanJointResearchInstitute,NanchangUniversity,Nanchang��0047,China):Pre-stainingpaperchromatographymethodforquantificationofgamma-amino-butyricacid.J.Chromatogr.A1216(25),5057-5060(2009).Paperchromatographyofgamma-aminobutyric acid.The method consists of application, separation and detection and is clean,rapid,inexpensiveandreproduciblecomparedtotheroutinepaperchromatography.Thederiva-tizationprocedurewithninhydrinreagentwasoptimizedregardingreagentconcentration,deri-vatizationtemperatureandtimeandCu2+concentration.Quantificationofgamma-aminobutyricacidbycombinationofwithvisspectrophotometry.Thelimitofdetectionwas0.05mg/mLandthelinearrangewasfrom0.5to20.0mg/mL.Thedeterminationcoefficientwasr2=0.998.Themethodwasaccurate(%RSD<2.6%),andrecoverieswere102.7-10�.9%.

qualitycontrol,traditionalmedicine,pharmaceuticalresearch,quantitativeanalysis,qualitativeidentification,paperchromatography 11a

104028 N. MANJU*,A. BINDU, N.ALEYKUTTY, J. SAJAN (*Department of Pharmaceutical Sci-ences,CheruvandoorCampus,Ettumanoor,Kottayam,Kerala,India):DevelopmentofHPTLCmethod forquantificationofgallic acid from the fruitsofPhyllanthusemblicaL.60th IndianPharmaceuticalCongressPG-265(2008).HPTLCofgallicacidintheethylacetatefractionoffruitsofPhyllanthusemblicaonsilicagelwithtoluene-ethylacetate-formicacid-methanol�0:�0:8:2.Detectionandquantitativedeterminationofgallicacidbyabsorbancemeasurementat280nm.TheproposedHPTLCmethodprovidedagoodresolutionofgallicacidfromotherconstituentspresentintheethylacetatefractionoffruitsofPhyllanthusemblicaandcanbeusedforthequantificationofgallicacid.

herbal,HPTLC,densitometry,quantitativeanalysis 11a

104029 D.MUKHERJEE*,T.BARMAN,S.RAJA,P.MUKHERJEE(*SchoolofNaturalProductStu-dies,JadavpurUniversity,Kolkata7000�2,India):EstimationofbetulinicacidinNelumbonu-cifera(Nymphaceae)rhizomeandseedextractbyvalidatedHPTLCmethod.AbstractNo.9192,IHCB(2009).HPTLCofbetulinicacidinhydroalcoholicextractsofNelumbonuciferarhizomeandseed,onsilicagelwithchloroform-methanol-formicacid49:1:1.Detectionbysprayingwithanisaldehydereagent.Quantitativedeterminationbyabsorbancemeasurementat420nm.Themethodwaslinearintherangeof2-10ng/spot,recoverywas98.1-98.4%.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis,postchromatographicderivatization 11a

1040�0 B.NIMAVAT*,D.MOVALIA,S.MISHRA,H.TANK(*S.J.ThakkarPharmacyCollege,Sau-rashtraUniversity,Rajkot,Gujarat,India):DevelopmentofvalidatedHPTLCmethodforquan-titative estimation of oleanolic acid as marker in total methanolic extract of fruits of Randiadumetorumlam.60thIndianPharmaceuticalCongressPA-217(2008).HPTLCofoleanolicacidintotalmethanolicextractoffruitsofRandiadumetorumlam.onsilicagelwithtoluene-ethylacetate-glacialaceticacid70:�0:1inatwintroughchambersaturatedfor10min.Detectionbytreatmentwith10%sulphuricacidinmethanol,followedbyheatingat110°Candimmediatedensitometricevaluation.Quantitativedeterminationbyabsorbancemeasurementat540nm.Themethodwaslinearintherangeof50-500ng/spot.Recoverywasintherangeof99.4-100.8%.

pharmaceuticalresearch,traditionalmedicine,herbal,HPTLC,quantitativeanalysis 11a

1040�1 P.PATEL*,R.SHAH,S.PATEL,UnnatiSHAH(*PharmanzaHerbalPvt.Ltd.,PlotNo.214,Kania�884�5,Gujarat,India;andLachooMemorialCollegeofScience&Technology,Jodhpur,India):Methoddevelopmentandvalidationfortheestimationof(-)hydroxycitricacidinfruitsofGarciniagummiguttaD.byHPTLC.AbstractNo.9191,IHCB(2009).HPTLCof(-)hydroxy

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CAMAGBIBLIOGRAPHYSERVICE No.10410

citricacid(themainconstituentofGarciniagummiguttafruits)onsilicagelwithn-propanol-water - glacial acetic acid 50:50:1. Quantitative determination by absorbance measurement at210nm.ThehRFvaluewas46.Themethodwaslinearintherangeof100-1000ng/spot,recove-rywas99.8-100.9%.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis 11a

1040�2 B.RAJ*,SalmaKHANAM,L.JOSEPHINE(*Dept.ofPharmacognosy,DayanandSagarCollegeofPharmacy,Bangalore560078,India,[email protected]):HPTLCmethodforestimationofursolicacid inOcimumsanctumextract.AsianJ.ofChem.21(9),6999-7004(2009).HPTLCofursolicacidinmethanolicandaqueousextractsofOcimumsanctum(Tulsi)onsilicagelwithtoluene-ethylacetate-aceticacid55:45:2withchambersaturation.DetectionbytreatmentwithLiebermannBurchard‘sreagent.Quantitativedeterminationbyabsorbancemeasurementat550nm.Themethodwaslinearintherangeof100-400ng/band.Theamountofursolicacidinaque-ousandmethanolicextractswasintherangeof0.2and0.4%.Samplescollectedfromdifferentgeographicalregionswerecompared,samplesfromKeralacontainedthehighestlevelsofursolicacid.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis 11a

1040�� B.RAJ*,SalmaKHANAM,S.JOHN,J.JENITA,AyeshaSIDDIQUA(*Dept.ofPharmacogno-sy, Dayananda Sagar College of Pharmacy, Kumaraswamy Layout, Bangalore 560078, India):ComparativeHPTLCanalysisofoleanolicacidinOcimumsanctumcollectedfromdifferentge-ographicalsources.AbstractNo.9226,IHCB(2009).HPTLCofoleanolicacid(inextractsofOcimumsanctumcollectedfromdifferentgeographicalsources)onsilicagelwithtoluene-ethylacetate-glacialaceticacid55:45:2.DetectionbysprayingwithLiebermann-Burchard‘sreagent.Quantitativedeterminationbyabsorbancemeasurementat600nm.Linearitywas in the rangeof 1-4 µg, recovery was 100.4-102.1 %. Hydro alcoholic extracts of the plant contained highamountsofoleanolicacid,maximumcontentswerefoundinplantscollectedintheKeralaregion.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,HPTLC,quantitativeanalysis 11a

1040�4 M.SAJEWICZ,D.KRONENBACH,M.GONTARSKA,M.WRÓBEL,R.PIETKA,TeresaKO-WALSKA*(*InstituteofChemistry,SilesianUniversity,9SzkolnaStreet,40-006Katowice,Po-land;[email protected]):TLCinasearchforstructurallimitationsofspontaneousoscillatoryin-vitrochiralconversion.Alpha-hydroxybutyricandmandelicacids.J.PlanarChromatogr.22,241-248(2009).TLCofalpha-hydroxybutyricacidsandmandelicacidonsilicagel,prewashedwithmethanol-water9:1andimpregnatedbydippingfor2sin0.05g/Laqueouscopperace-tatesolution,withdioxane-water9:1at22+/-2°C.Quantitativedeterminationbyabsorbancemeasurementduring16daysat�26nm.Spontaneousoscillatoryin-vitrochiralconversionwasobservedforalpha-substitutedpropionicacidsaswellaschiralcarboxylicacidswith twoandfourcarbonatoms.

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13. Steroids1040�5 R.XIA(XiaRui)*,SH.DONG(DongShuying),B.CHE(CheBaoquan)(*BeijingMunicip.Inst.

DrugCont.,Beijing1000�5,China):(RapididentificationofglucocorticoidinChinesetraditi-onalmedicinalformulationsbythin-layerchromatography)(Chinese).ChineseJ.Pharm.Anal.28(�),470-471(2008).TLCofglucocorticoidinTCMformulationsextractedwithchloroform-methanol9:1onsilicagelwithdichloromethane-diethylether-methanol-water�85:60:15:2.Detectionby sprayingwith a solutionof tetrazoliumblue chloride.Successful separation andidentificationoffiveglucocorticoids.

doping,pharmaceuticalresearch,traditionalmedicine,qualitycontrol,quantitativeanalysis,qualitativeidentification 1�

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CAMAGBIBLIOGRAPHYSERVICE No.10411

1040�6 B.YUAN(YuanBaoqiang)*,L.Yang(YangLahu)(*FuzhouMunicip.Inst.DrugCont.,Fuzhou,Fujian�50001,China):(Analysisofdexamethasoneacetateandtherelatedcompoundsintheta-blets)(Chinese).ChineseJ.Pharm.Anal.27(�),412-41�(2007).TLCofdexamethasoneacetateonsilicagelwithdichloromethane-methanol9:1.DetectionunderUV254nm.

pharmaceuticalresearch,qualitycontrol,qualitativeidentification,quantitativeanalysis 1�

15. Terpenesandothervolatileplantingredients1040�7 B.CHENGAIAH*,B.PRATAP,M.ALAGUSUNDARAM,M.RUTHU,V.SAROVARREDDY

(*AnnamacharyaCollegeofPharmacy,Rajampet,Kadapa,A.P.,India):IdentificationofterpenesinstemofOcimumbasilicumLinnbyHPTLCtechnique.60thIndianPharmaceuticalCongressPA-221(2008).HPTLCof terpenesinstemofOcimumbasilicumonsilicagelwithtoluene-ethylacetate19:1.Evaluationof5spotsunderUV254nmandundervisiblelightaftertreatmentwithanisaldehydereagentfollowedbyheatingat100°Cfor5min:borneol(yellow,hRF24),menthol(red,hRF27),eugenol(blue,hRF50),thymol(violet,hRF57),safrole(blue,hRF9�).

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17. Amines,amidesandrelatednitrogencompounds1040�8 A.ALPMANN,GertrudMORLOCK*(*UniversityofHohenheim,InstituteofFoodChemeistry,

Garbenstrasse28,70599Stuttgart,Germany;[email protected]):Rapidandcost-ef-fectivedeterminationofacrylamideincoffeebyplanarchromatographyandfluorescencedetec-tionafterderivatizationwithdansulfinicacid.J.AOACInt.92,725-729(2009).HPTLCofacryl-amideextracted fromcoffeesamplesonsilicagelwithethylacetate - tert.butylmethylether4:1inatwintroughchamberorautomaticdevelopingchamber.Pre-chromatographicinsitude-rivatizationoftheextracts(appliedasarea)byoversprayingwithdansulfinicacidproducedthefluorescentdansylpropanamideband.Quantitativedeterminationbyfluorescencemeasurementat254/>400nm.Thelimitofquantificationwas48µg/kg.Thelinearityoverthewholeprocedureshoweddeterminationcoefficientsbetween0.9995and0.9825(n=6).Thewithin-runprecision(%RSD,n=6)ofthechromatographicmethodwas�%.Commercialcoffeesamplesanalyzedshowedacrylamidecontentsbetween52and191µg/kg,whichwasincorrelationwithamountsreportedinpublications.

foodanalysis,toxicology,qualitycontrol,HPTLC,quantitativeanalysis,densitometry 17c

18. Aminoacidsandpeptides,chemicalstructureofproteins1040�9 J.D.VASTA,M.CICCHI, J.SHERMA*,B.FRIED(*LafayetteCollege,DepartmentofChe-

mistry,EastonPA18042-1782USA):Evaluationofthin-layerchromatographysystemsforana-lysisofaminoacids incomplexmixtures.ActaChromatographica21 (1),29-�8 (2009).Eva-luationofdifferentTLCsystemsforanalysisof21aminoacidsinbiologicaltissuesandfluids.Detectionbyderivatizationwithninhydrinreagent,anddeterminationofRFvaluesbyslit-scan-ningdensitometry.Thefivemostsuitablesystemswerecelluloseandsilicagelplatesdevelopedwitheither2-butanol-pyridine-aceticacid-water�9:�4:10:26or2-butanol-pyridine-25%ammonia-water�9:�4:10:26,andionexchangeplatesdevelopedwithcitratebufferofpH�.�.Detection with ninhydrin allowed the identification of all amino acids except for leucine andisoleucineincomplexmixtures.Quantificationispossibleaswelliftheaminoacidofinterestiswellseparatedfromadjacentcomponentsofthemixture.ThemethodisillustratedwithexamplechromatogramsoncelluloseHPTLC layer showing the identificationand separationof aminoacidsinsnailtissuesamples.

clinicalchemistryresearch,HPTLC,quantitativeanalysis,qualitativeidentification,densitometry 18a

104040 M.VEGA*, M.ARANDA (*University of Concepcion, Faculty of Pharmacy, Department ofFoodScience,NutritionandDietetic,BarrioUniversitarios/nCasilla2�7,PO40�-0249Con-cepcion,Chile;[email protected]):Determinationofavailablelysinebyplanarchromatography:Ausefultoolforproteinqualityevaluationinfishfeed.J.AOACInt.92,699-702(2009).HPTLCof a dinitrophenyl-lysine derivative (produced by incubation with 1-fluoro-2,4-dinitrobenzeneandhydolyzationwithhydrochloricacid)onsilicagel (prewashedwithmethanol)withn-pro-

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CAMAGBIBLIOGRAPHYSERVICE No.10412

panol-25%ammonia7:�inatwintroughchamber.Quantitativedeterminationbyabsorbancemeasurementat�60nm.Themethodwaslinear(r2=0.9991)intherangefrom12.5to125.0ng/band.Repeatability(%RSD)andintermediateprecision(%RSD)inmatrixwere0.8%and�.6%,respectively.Recoveriesofspikedsamplesattwolevelsrangedfrom72to85%withRSDfrom�to8%.Thismethodisareliable,highthroughputandlowcostanalyticalmethodforthesalmonfeedindustry.

foodanalysis,qualitycontrol,HPTLC,densitometry,quantitativeanalysis 18a

20. Enzymes104020 PetraJAZBECetal.,seesection9

22. Alkaloids104041 K.DHALWAL*,V.SHINDE,K.MAHADIK(*Dept.ofPharmacognosyandPhytochemistry,

PoonaCollegeofPharmacy,BharathiVidyapeethUniversity,Erandwane,Pune4110�8,India):Effective and sensitivemethods for quantitative analysis of alkaloids in sida species byusingHPLCandHPTLC.AbstractNo.9402,IHCB(2009).HPLCandHPTLCmethodsweredevelo-pedforthesimultaneousestimationofvasicineandvasicinoneinSidacordifoliaandSidaacutaroots.HPTLCofvasicineandvasicinoneonsilicagelwithethylacetate-methanol-ammonia40:10:1.Quantitativedeterminationbyabsorbancemeasurementat�00nm.Linearitywas�20-960ng/spot (vasicine) and80-400ng/spot (vasicinone).LinearitybyHPLCwas4-20µg/mL.TheHPTLCmethodwasmoresuitablebecauseofhighthroughputandlowanalysistime.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,comparisonofmethods 22

104042 Danuta RAJ*, A. KOKOTKIEWICZ, M. LUCZKIEWICZ (*Department of Pharmacognosy,WroclawMedicalUniversity,pl.Nankiera1,50-140Wroclaw,Poland;[email protected]):Densi-tometricHPTLCanalysisofindolizidinealkaloidsintheherbandin-vitrocultureofSecurinegasuffruticosa. J. Planar Chromatogr. 22, �71-�76 (2009). HPTLC of indolizidine alkaloids andextractsonsilicagelandRP-18(bothprewashedwithchloroform-methanol1:1)with11mobilephasesinahorizontalchamberwithoutchambersaturation.Thebestresolutionwasachievedonsilicagelwithchloroform-methanol20:1.DetectionunderUV254nmandaftersprayingwithDragendorffreagent.Quantitativedeterminationofsecurinineandallosecurininebyabsorbancemeasurementat254nm.Thelimitofdetectionandquantificationwas11and�6ng/zoneforse-curinineand12and41ng/zoneforallosecurinine,respectively.

herbal,qualitycontrol,traditionalmedicine,HPTLC,densitometry,quantitativeanalysis 22

10404� H.WIEDENFELD*,G.HOESCH,E.ROEDER,TH.DINGERMANN(*PharmazeutischesIns-titutderUniversität,Ander Immenburg4,5�121Bonn,Germany;[email protected]):LycopsamineandcumambrinB fromEupatoriummaculatum.Pharmazie64,415-416 (2009).TLCofthepyrrolizidinealkaloidlycopsamineandtheguaianolidecumambrinBonsilicagelwithdichloromethane-methanol-25%ammonia85:14:1.DetectionseeA.R.Mattocks,Detec-tionofpyrrolizidinealkaloidsonthin-layerchromatograms,J.Chromatogr.27,505-508(1967).

pharmaceuticalresearch,herbal,qualitativeidentification 22

104005 M.WAKSMUNDZKA-HAJNOSetal.,seesection2

104044 L.ZHANG(ZhangLu)*,H.LI(LiHongyu),Y.WEI(WeiYuhui)(*StateKeyLabofMinist.Educ.ofDrought&GrassplotZoology,Coll.LifeSci.,LanzhouUniv.,Lanzhou7�0000,China):(Analysis of the alkaloids in the seedsofSophoramoorcroftiana (Benth.)Baker byTLCandHPLC)(Chinese).ChineseJ.Pharm.Anal.28(7),1071-1074(2008).TLCofthealkaloidsma-trine,oxymatrine,sophocarpine,sophoridine,cytosinetheinseedextractsofSophoramoorcrof-tianaonsilicagelwithchloroform-methanol-ammonia50:6:1.DetectionunderUV254nm.

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CAMAGBIBLIOGRAPHYSERVICE No.1041�

Comparisonwith reference standards showed that extracts containedmatrine, oxymatrine, so-phocarpine,sophoridine,andcytosine.

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27. Vitaminsandvariousgrowthregulators104045 A.MOHAMMAD*,A.ZEHRA(*AligarhMuslimUniversity,AnalyticalResearchLaboratory,

DepartmentofAppliedChemistry,FacultyofEngineeringandTechnology,Aligarh,India):Spe-cificseparationofthiaminefromhydrophilicvitaminswithaqueousdioxaneonprecoatedsilicaTLCplates.ActaChromatographica20(4),6�7-642(2008).TLCofthiaminehydrochloridefromriboflavin, nicotinic acid, calcium D-pantothenate, pyridoxine hydrochloride, cyanocobalamin,andascorbicacidonsilicagelwithdioxane-water1:1.DetectionunderUVlight.Examinationoftheeffectofimpurities(metalcationsandinorganicanions)onthechromatographyofthiaminehydrochloride.Thedetectionlimitforthiaminehydrochloridewas90ng/spotand%RSDofthia-minehydrochloridewas14.9%(n=5).

pharmaceuticalresearch,qualitycontrol,foodanalysis,quantitativeanalysis,qualitativeidentification 27

104046 A.MOHAMMAD*,A.ZEHRA(*AnalyticalResearchLaboratory,DepartmentofAppliedChe-mistry,FacultyofEngineeringandTechnology,AligarhMuslimUniversity,Aligarh202002,In-dia;[email protected]):Simultaneousseparationandidentificationofcyanoco-balamin,thiamine,andascorbicacidonpolyoxyethylenesorbitanmonooleate-impregnatedsilicalayerswithwaterasmobilephase.J.PlanarChromatogr.22,429-4��(2009).TLCofthewater-solublevitaminscyanocobalamine,thiamine,andascorbicacidonsilicagel(impregnatedwitha2%solutionofthenon-ionicsurfactantTween80)withdoubledistilledwateringlassjarssatu-ratedfor�0minat�0+/-2°C.Detectionofallsubstancesexceptfolicacidandcyanocobalaminbyexposuretoiodinevaporandevaluationindaylight.

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104047 M.SUE-CHU,S.KRISTENSEN,H.H.TONNESEN*(*UniversityofOslo,SchoolofPharma-cy,DepartmentofPharmaceutics,P.O.Box1068,Blindern,0�16Oslo,Norway;[email protected]):Photoinducedcolorchangesintwodifferentqualitiesofriboflavininthesolidstateandvarioustabletformulations.Photoreactivityofbiologicallyactivecompounds.Pharma-zie64,428-4�5(2009).TLCofriboflavinandlumichrome(7,8-dimethylbenzo[g]pteridine-2,4-(1H,�H)-dione)onsilicagelwithaceticacid-acetone-methanol-benzene1:1:4:14DetectionundervisiblelightandUV254and�66nm.

pharmaceuticalresearch,foodanalysis,qualitativeidentification 27

28. Antibiotics,Mycotoxins104242 R.BHUSHANetal.,seesection�8

104048 U.HUBICKA,J.KRZEK*,H.WOLTYNSKA,B.STACHAZ(*CollegiumMedicumofJagiel-lonianUniversity,DepartmentofInorganicandAnalyticalChemistry,Medyczna9,�0-688Kra-kow,Poland;[email protected]):Simultaneousidentificationandquantitativedetermi-nation of selected aminoglycoside antibiotics by thin-layer chromatography and densitometry.J.AOACInt.92,1068-1075(2009).TLCandHPTLCofsixantibiotics(amikacin,gentamicin,kanamycin,neomycin,netilmicin,andtobramycin)inpharmaceuticalpreparationsonsilicagelwithmethanol-25%ammonia-chloroform�:2:1.Detectionbyderivatizationwith0.2%etha-nolicninhydrinreagent.Quantitativedeterminationbyabsorbancemeasurementat500nm.Thelimitofdetectionandquantificationwas250and500ng/zoneforamikacin,500and1000ng/zoneforkanamycin,480and800ng/zoneforneomycin,�80and6�0ng/zonefornetilmycin,480and800ng/zonefortobramycinand1000and1650ng/zoneforgentamicin.Precisionwasgoodwith%RSDof0.�-0.6%.

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CAMAGBIBLIOGRAPHYSERVICE No.10414

104049 S.JOSHI*,A.SHARMA,M.S.M.RAWAT,C.DHIMAN(*DepartmentofChemistry,K.L.D.A.V.(P.G.)College,Roorkee-247667.India;[email protected]):Developmentofconditionsfor rapid thin-layerchromatographyofbeta-lactamantibiotics. J.PlanarChromatogr.22,4�5-4�7(2009).TLCofpenicillins(benzylpenicillin,ampicillin,andamoxicillin)andcephalosporins(cephalexin,cefoperazone,ceftriaxone,cefixime,andcefadroxil)inpowderextractsonsilicagel(impregnatedwith0.2%ammoniumchloride)withpropanol-aceticacid4:1andbutanol-ace-ticacid-water4:1:2.DetectionunderUVlightat�65nm.

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104001 TaraMCGLINCHEYetal.,seesection1

104050 P.N.RANJANE*,S.V.GANDHI,S.S.KADUKAR,K.G.BOTHARA,(*DepartmentofPharma-ceuticalAnalysis,A.I.S.S.M.S.CollegeofPharmacy,KennedyRoad,NearR.T.O.,Pune411001,India): HPTLC determination of cefuroxime axetil and ornidazole in combined tablet dosageform.J.Chromatogr.Sci.48(1),26-28(2010).HPTLCofcefuroximeaxetilandornidazoleincombinedtabletdosageformonsilicagelwithtoluene-n-butanol-triethylamine17:4:1.ThehRFvalueofornidazolewas51andofcefuroximeaxetil67.Quantificationbydensitometryat285nm.Linearitywasbetween100and500ng/bandforbothcefuroximeaxetilandornidazole.Themethodwasusedfortheassayofthecompoundsinpharmaceuticalformulations.Thecon-tentofcefuroximeaxetilwas102.4%andofornidazole101.0%.

pharmaceuticalresearch,qualitycontrol,HPTLC,autoradiography,densitometry,quantitativeanalysis,qualitativeidentification 28a

104051 A.R.ROTE*,S.P.PINGLE*(*DepartmentofPharmaceuticalChemistry,M.G.V.‘sPharmacyCollege,Panchavati (PuneUniversity)Mumbai,Agra Road,Nashik42200�,Maharashtra, In-dia):Reversephase-HPLCandHPTLCmethodsfordeterminationofgemifloxacinmesylateinhumanplasma.J.Chromatogr.B877(29),�719-�72�(2009).HPTLCofgemifloxacinmesylateinhumanplasma,extractedwithchloroform-aceticacid59:1,onsilicagelwithethylacetate-methanol-ammonia8:4:�.ThehRFvalueofgemifloxacinmesylatewas��.Quantificationbydensitometryat254nm.Thecalibrationcurvewasestablishedintherangeof50to600ng/spot.Recoveryofgemifloxacinmesylatewasbetween80.0and86.2%.Thestabilityofgemifloxacinmesylateinplasmawasconfirmedwithsamplessubmittedtothreecyclesoffreeze-thawingat<20°C,andwithsamplesstoredonthebenchfor12h.

clinicalchemistry,research,HPTLC,densitometry,quantitativeanalysis,qualitativeidentification,comparisonofmethods 28a

104052 D.H. SHEWIYO*, E. KAALE, P.G. RISHA, B. DEJAEGHER, J. SMEYERS-VERBEKE,Y.VANDERHEYDEN(*DirectorateofLaboratoryServices,TanzaniaFoodandDrugsAuthori-ty,P.O.Box77150,DaresSalaam,Tanzania):Developmentandvalidationofanormal-phasehigh-performancethinlayerchromatographicmethodfortheanalysisofsulfamethoxazoleandtrimethopriminco-trimoxazoletablets.J.Chromatogr.A1216(42),7102-7107(2009).HPTLCofco-trimoxazoletablets(combinationofsulfamethoxazoleandtrimethoprim)onsilicagelwithtoluene-ethylacetate-methanol100:57:4�.DetectionunderUV254nm.ThehRFvalueswere�0and61fortrimethoprimeandsulfamethoxazole,respectively.QuantificationbydensitometryatUV254nm.Cochran‘scriteriontestindicatedhomoscedasticityofvariancesforthecalibrati-ondata.TheF-testsforlack-of-fitindicatedthatstraightlineswereadequatetodescribetherela-tionshipbetweenspotareasandconcentrationsforeachcompound.Repeatabilityandprecision(%RSD)was1.0and0.8%forsulfamethoxazoleaswellas1.�%and1.6%fortrimethoprim,re-spectively.Recoverywas99.0%and99.7%forsulfamethoxazoleandtrimethoprim,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,qualitativeidentification,quantitativeanalysis,densitometry 28a

10405� U.VINCENT,G.GIZZI,C.VONHOLST*,J.DEJONG,J.MICHARD(*EuropeanCommissi-on,JointResearchCentre,InsitututeforReferenceMaterialsandMeasurements,FoodSafetyand

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CAMAGBIBLIOGRAPHYSERVICE No.10415

QualityUnit,Retieseweg,2440Geel,Belgium,[email protected]):Validationofananalyticalmethodforthedeterminationofspiramycin,virginiamycin,andtylosininfeeding-stuffsby thin-layer chromatographyandbio-autobiography.FoodAddit.Contam.24,�51-�59(2007). Inter-laboratoryvalidationof the analyticalmethod (published in theSIMBAG-FEEDreport4.6)basedonTLCcoupledtobio-autographyforthedetectionoftylosin,spiramycinandvirginiamycininfeeding-stuffsforpoultry,pig,cattleandcalf.Thedetectionlimitofspiramycinwas2mg/kgandthemethodhasatargetconcentrationof1mg/kgfortylosinandvirginiamycin.ThemethodshowedhighspecificityandoffersthepossibilityforscreeningbeforeLC/MSanalysis.

qualitycontrol,quantitativeanalysis 28a

104054 L.YANG (Yang Lihong)*, CH. HU (Hu Changqin), W. LIU (Liu Wenying) (*China Pharm.Univ., Nanjing 210009, China): (Determination of gentamycin and the related compounds bythin-layerchromatography)(Chinese).ChineseJ.Pharm.Anal.26(2),221-224(2006).HPTLCofgentamycinandrelatedcompoundsonsilicagelwithchloroform-methanol-25%ammonia5:7:6.Themaincompoundiswellseparatedfromtheimpurities.Quantificationbydensitometryat485nm.Linearitywasbetween4.0-40ng/spot(r2=0.99)andthelimitofdetectionwasatthelownglevel.

qualitycontrol,pharmaceuticalresearch,HPTLC,densitometry,quantitativeanalysis,qualitativeidentification 28a

29. Pesticidesandotheragrochemicals104055 V.R.CHANDEGAONKAR,D.B.SHINDE,D.V.MANE* (*DepartmentofChemistry,Chhat-

rapatiShivajiCollege,Omerga,(MS)41�606India;[email protected]):Thin-layerchromatographic detection and identificationof the insecticide imidacloprid in biologicalma-terials.J.PlanarChromatogr.22,459-460(2009).TLCof imidacloprid(1-[(6-chloro-�-pyridi-nylmethyl)]-4,5-dihydro-N-nitro-1H-imidazol-2-amine)andbiologicalextractsonsilicagelwithchloroform-acetone7:�orhexane-acetone-ethanol8:1:1withchambersaturation.Detectionbysprayingwith5%dimethylaminobenzaldehydeinhydrochloricacid,followedbyheatingat100°Cfor10min.Imidaclopridwasdetectedasapinkzoneundervisiblelight.

agricultural,qualitativeidentification,postchromatographicderivatization 29a

104056 V.R.CHANDEGAONKAR,J.N.SANGSHETTI,D.B.SHINDE,D.V.MANE*(*DepartmentofChemistry,ChhatrapatiShivajiCollege,Omerga(MS)4�1606,India;[email protected]):Anewchromogenic spray reagent fordetectionand identificationofmonocrotophos. J.PlanarChromatogr.22,457-458(2009).TLCofmonocrotophosandbiologicalextracts,dime-thoate,endosulfan,carbaryl,andcypermethrinonsilicagelwithchloroform-acetone7:�withchambersaturation.Detectionbysprayingwith5%sodiumhydroxidesolutionfollowedby5%benzilreagent(5gbenzilin100mLacetone)andheatingat100°Cfor10min.Monocrotophoswasdetectedasapinkzoneindaylight.

toxicology,agricultural,qualitativeidentification 29b

104057 W.SCHWACK*,T.ZEISLER,C.STIEFEL(*UniversityofHohenheim,InstituteofFoodChe-mistry,Garbenstrasse28,70599Stuttgart,Germany;[email protected]):Determi-nationofdialkylphosphates asbreakdownproductsoforganophosphorus insecticides in fruitjuicesbyHPTLCwithfluorescencedetection.J.AOACInt.92,691-697(2009).HPTLCofdi-alkylphosphatestandards(dimethylphosphate,diethylphosphate,dimethylthiophosphate,diet-hylthiophosphateanddibutylphosphateasinternalstandard)onaminophase,prewashedwithmethanol,withdichloromethane in a twin troughchamber.Quantitativedeterminationbyflu-orescencemeasurement at �66/>400nm.The limitofquantificationwasbetween0.8 and1.4ng/zone.Fluorescenceenhancementwasachievedbydippingtheplateintoa50%solutionofparaffinoilinn-hexane,increasingthesensitivityandresultinginanLOQof0.5-0.6ng/zone.

agricultural,toxicology,qualitycontrol,foodanalysis,HPTLC,densitometry,quantitativeanalysis 29b

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CAMAGBIBLIOGRAPHYSERVICE No.10416

104058 T.TOSTI,G.RAKIC,M.NATIC,D.MILOJKOVIC-OPSENICA,S.HUSINEC,V.SAVIC,Z.TESIC*(*FacultyofChemistry,UniversityofBelgrade,P.O.Box51,11158Belgrade,Serbia;[email protected]):TLCretentionbehaviorofbrodifacoum,bromadiolone,andcoumatetra-lylandtheirimpuritiesondifferentadsorbents.J.PlanarChromatogr.22,���-�4�(2009).TLCofbrodifacoum,bromadiolone,coumateralylandimpuritiesonsilicagel,alumina,cellulose,andRP-18with46differentmobilephasesinatwintroughchambersaturatedfor�0min.Themostselectivephasesonsilicagelwerechloroform-ethylacetate-n-hexaneinvariousratios,ethylmethylketone-toluene1:9,andchloroform-toluene7:�;onaluminathebestmobilephasewasdichloromethane-n-hexane�:2.DetectionunderUVlightat254nm.

toxicology,qualitativeidentification 29f

104059 T.TUZIMSKI(DepartmentofPhysicalChemistry,FacultyofPharmacy,MedicalUniversityofLublin, 4 Staszica Street, 20-081 Lublin, Poland, [email protected]):Application ofSPE-HPLC-DAD and SPE-HPTLC-DAD to the analysis of pesticides in lake water. J. PlanarChromatogr.22,2�5-240(2009).HPTLCofpesticides(clofentezine,neburon,chlorfenvinphos,lenacyl,trifluralin,thiram,procymidone,flufenoxuron,tralkoxydim,propaquizafop,dinoseb)andwatersamples(samplepreparationbysolidphaseextraction)onsilicagelwithethylacetate-n-heptane1:4and�:7inahorizontalchamber.Quantitativedeterminationbydiodearrayden-sitometryintherangeof200to600nm.Thelimitofdetectionwasbetween40and650ng/spotandthelimitofquantificationwasbetween120and1920ng/spot.

environmental,toxicology,HPTLC,quantitativeanalysis 29a

30. Syntheticandnaturaldyes104060 GertrudMORLOCK*,C.OELLIG(*UniversityofHohenheim,Garbenstrasse28,70599Stuttg-

art,Germany;[email protected]):Rapidplanarchromatographicanalysisof25wa-ter-solubledyesusedas foodadditives. J.AOACInt.92,745-756 (2009).HPTLCof25dyes(brilliantblackBN,tartrazine,ponceau6R,resorcinyellow,fastyellowAB,orcein,allurared,greenS,amaranth,quinolineyellow,acidblue,erythrosine,sunsetyellowFCF,indigocarmine,ponceau4R,azorubine,brilliantblueFCF,carmine,scarletGN,copperchlorophyll,enocyanine,chlorophyllintrisodiumcoppersalt,curcumin,riboflavin-5-phosphate,riboflavin)onsilicagelinahorizontaldevelopingchamberwithethylacetate-methanol-water-aceticacid65:2�:11:1for40samplesin12min.Relativehumiditywas21+/-�%atatemperatureof20+/-�°C.Al-ternatively,atwintroughchamberorautomaticdevelopingchambercanbeused.Quantitativedeterminationbyabsorbancemeasurementat11differentwavelengths.Repeatabilities(%RSD,n=4)nearthelimitofquantificationshowedprecisionsofmostly<2.7%,rangingbetween0.2and 5.2 %. Correlation coefficients (R >0.9987) and RSD values (<4.2 %) of the calibrationcurveswerehighlysatisfactoryusingclassicalquantification.However,digitalevaluationoftheplate imagewas alsoused forquantification,which resulted inRSDvaluesof the calibrationcurvesofmostly<�.0%,exceptfortwo<6.0%.Themethodwasappliedfortheanalysisofsomeenergydrinksandbakeryinkformulations,directlyappliedafterdilution.Byrecordingofabsor-bancespectrainthevisiblerange,theidentitiesofthedyesfoundinthesampleswereascertainedbycomparisonwiththerespectivestandardbands(correlationcoefficients>0.9996).Ifnecessaryforconfirmation,onlinemassspectrawererecordedwithinaminute.

foodanalysis,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �0a

104014 F.SCHULTEetal.,seesection4e

104061 ZH.WANG(WangZhiyong)*,B.WANG(WangBingquan),H.ZOU(ZouHong)(*Dep.Chem.,Capital.Norm.Univ.,Beijing100�7,China):(Identificationofthecategoryofblackgelpeninkbythin-layerchromatography)(Chinese).PhysicalTestingandChem.Anal.,PartB:Chem.Anal.45(1),14-18(2009).TLCofinkextractsonsilicagelwithn-butanone-ethanol-water-aceticacid14:4:6:1.DetectioninvisblelightandidentificationbycomparisonofspotcolorsandhRFvalues.Themethodwasusedfor the identificationof�7differentblack inksamples fromgelpensfromdifferentsources,whichcouldthenbeclassifiedinto1�categories.

qualitycontrol,qualitativeidentification �0a

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CAMAGBIBLIOGRAPHYSERVICE No.10417

32. Pharmaceuticalandbiomedicalapplications104062 S.AGARWAL*,A.AIL,Y.DU,S.ABUJA(*Dept.ofPharmaceutics,FacultyofPharmacy,Ja-

mieHamdardUniversity,NewDelhi110062,India,[email protected]):DeterminationofartemisinininbulkandpharmaceuticaldosageformsusingHPTLC.Ind.J.Pharma.Sci.71(1),98-100 (2009).HPTLCofartemisininonsilicagelwith toluene -ethylacetatewithchambersaturationfor�0min.Quantitativedeterminationbyabsorbancemeasurementat520nm.Theme-thodwaslinearovertherangeof100-600ng/band,recoverywasintherangeof98.8-100.5%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

10406� S.AHMAD*,M.SINGH,M.KAUR,A.AHMED(*JamiaHamdard,FacultyofPharmacy,NewDelhi,India):QuantitativeestimationofglycyrrhizicacidinthetabletsofYashtimadhubyHPT-LC.60thIndianPharmaceuticalCongressPG-260(2008).HPTLCofglycyrrhizicacidonsilicagelwithchloroform-glacialaceticacid-methanol-water15:8:�:2.Quantitativedeterminationbyabsorbancemeasurementat254nm.ThehRFvalueofglycyrrhizicacidwas28.Themethodwas linear in the rangeof50-500ng/spot.Thesampleanalyzedby theproposedmethodcon-tained87.8µgglycyrrhizicacidpertablet,equivalentto0.015%w/wofthetabletformulation.

qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104064 S. AHMAD*, A. KAMAL, R. PARVEEN, F. AHMAD, K. SALEEM (*JMI, Dept. of Bio-sciences,NewDelhi,India):DevelopmentandvalidationofnovelHPTLCmethodforquantitativeestimationofstrychnineandbrucineinseedsofStrychnosNuxVomica.60thIndianPharmaceuti-calcongressPA-2�5(2008).HPTLCofstrychnineandbrucine(inseedsofStrychnosNuxVomica)onsilicagelwithchloroform-methanol-ammonia�8:2:1.Quantitativedeterminationbyabsor-bancemeasurementat258nm(strychnine,hRFvalue29)and271nm(brucine,hRFvalue21).Themethodwaslinearintherangeof100-1000ng/spot(bothcompounds).Themethodwassuitableforstandardizationofseveralherbalformulationscontainingnuxvomicaasaningredient.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104065 S.AHMAD*, M. SINGH, R. PARVEEN,Y. KAMAL (*Jamia Hamdard, Faculty of Pharma-cy, New Delhi, India): Quantitative estimation of withaferin a in the tablets ofAshwagandhabyHPTLC.60th IndianPharmaceuticalCongressPG-262 (2008).HPTLCofwithaferinA inAshwagandhaonsilicagelaluminumlayerwithtoluene-ethylacetate-formicacid5:5:1.Quan-titativedeterminationbyabsorbancemeasurementat214nm.ThechromatogramsofthetabletformulationshowedazonecorrespondingtostandardwithaferinA(hRFvalue�7)indicatingthepresenceofthesameintheherbalformulation.Linearitywasintherange50to500ng/spot.TheconcentrationofwithaferinAwas8.07µg/tabletand0.001�4%w/winthetabletformulation.

qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104066 M.ALAVALA(KLEUniversity‘sCollegeofPharmacy,Belgaum,Karnataka,India):Newsta-bilityindicatinghigh-performanceliquidchromatographyandhigh-performancethin-layerchro-matographymethod for theestimationofolopatadinehydrochloride.AbstractNo.F-�09,61stIPC(2009).HPTLCofolopatadineHClonsilicagelwithmethanol-chloroform-25%ammo-nia80:20:1.ThehRFvaluewas46.Quantitativedeterminationbyabsorbancemeasurementat�01nm.Themethodwaslinearintherangeof100-900ng/band.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104067 B.ARUN*,A.SUGANTHI,A.FATHIMUNNISA,T.RAVI(*CollegeofPharmacy,SriRama-krishnaInstituteofParamedicalScience,Coimbatore,TamilNadu,India):Developmentofvali-datedHPTLCmethodfortheestimationofbuclizinehydrochlorideintabletdosageform.Abs-tractNo.F-276,61stIPC(2009).HPTLCofbuclizinehydrochlorideonsilicagelwithmethanol-chloroform-ammonia8:1:1%.Quantitativedeterminationbyabsorbancemeasurementat2�4nm.

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CAMAGBIBLIOGRAPHYSERVICE No.10418

Thecalibrationcurvewaslinearintherangeof100-700ng/spot.Thelimitofdetectionandlimitofquantificationwere20and100ng/spot,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104068 J.BAGYALAKSHMI*,S.VIJAYARAJ,SajnaJOHN,T.RAVI(*SriRamkrishnaInstiuteofPara-medicalScience,CollegeofPhamracy,Coimbatore,Tamilnadu,India):Developmentandvalida-tionofsimultaneousestimationofparacetamol,aceclofenacandrabeprazoleincombinedtabletdosage formulationbyHPTLCmethod.60th IndianPhamraceuticalCongressPA-222 (2008).HPTLCofparacetamol,aceclofenacandrabeprazoleonsilicagelwithethylacetate-methanol-glacialaceticacid90:10:1.Quantitativedeterminationbyabsorbancemeasurementat275nm.Linearitywasintherangeof100-500µg/mL,20-100µg/mLand2-10µg/mLforparacetamol,aceclofenacandrabeprazolerespectively.Recoverywasintherangeof98.9-100.1%forallthreecompounds.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104069 N.BAIRWA*,A.TRIVEDI,S.MISHRA(*TheM.S.UniversityofBaroda,PharmacyDept.,Va-dodara,Gujarat,India):Simultaneousestimationofmarkersinahaematinicherbomineralformu-lationusinghigh-performancethin-layerchromatography.60thIndianPharmaceuticalCongressPG-251(2008).HPTLCofglycyrrhetinicacidandpiperineinhaematinicherbomineralcapsuleformulationonsilicagelwithtoluene-ethylacetate-glacialaceticacid25:15:1.QuantitativedeterminationbyabsorbancemeasurementatUV254nm.Themethodwaslinearintherangeof0.8-2.4ng/spot(glycyrrhetinicacid)and10-50ng/spot(piperine).Recoverywas96.�-98.6%.traditionalmedicine

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104070 V.BALI*,M.ALI,J.ALI(*JamiaHamdard,FacultyofPharmacy,NewDelhi,India):AnovelandrapidHPTLCmethodfortheanalysisofrosuvastatincalcium.60thIndianPharmaceuticalCongressPA-219(2008).HPTLCofrosuvastatincalciumonsilicagelwithtoluene-ethylace-tate-formicacid9:7:1.Quantitativedeterminationbyabsorbancemeasurementat254nm.ThehRFvaluewas�2.Themethodwaslinearintherangeof100-100ng/spot,recoverywas99.7%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104071 V.BHAVNANI*,V.DIWALE,P.DESHMUKH,A.DHIWARE(*A.I.S.S.M.S.CollegeofPhar-macy, Pune, Maharashtra, India):Validated method development for estimation of famotidineanddomperidoneincombinedtabletdosageform.AbstractNo.F-��5,61stIPC(2009).HPTLCoffamotidineanddomperidoneonsilicagelwithtoluene-methanol-triethylamine12:6:1.ThehRFvaluewas2�and67forfamotidineanddomperidone,respectively.Quantitativedetermina-tionbyabsorbancemeasurementat290nm.Themethodwaslinearintherangeof100-500ng/band.Recoverywas98.6-98.9%forbothdrugs.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104072 D.BHAWSAR*,P.RATHI,M.PURANIK,P.YEOLE(*InstituteofPharmaceuticalEducationandResearch,Wardha,Maharashtra,India):DevelopmentandvalidationofHPTLCtechniqueforsimultaneousestimationofgatifloxacinandornidazoleinsoliddosageforms.AbstractNo.F-�47,61stIPC(2009).HPTLCofgatifloxacinandornidazoleonsilicagelwithdichloromethane-methanol-25%ammonia95:10:�.ThehRFvaluewas16and60forgatifloxacinandornidazole,respectively.Quantitativedeterminationbyabsorbancemeasurementat�02nm.Themethodwaslinearintherangeof20-200ng/bandforgatifloxacinand50-500ng/bandforornidazole.Reco-verywasbetween100.4and101.9forbothdrugs.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

10407� R.BIDAWAI*,N.RAUT,D.WANKHEDE,N.GAIKWAD(*UniversityDept.ofPharmaceuti-calScience,RTMNagpurUniversity,Nagpur,Maharashtra,India):Validatedstabilityindicating

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CAMAGBIBLIOGRAPHYSERVICE No.10419

HPTLCmethodfortheestimationofolmesartanmedoxomilinbulkandpharmaceuticaldosageform.60thIndianPharmaceuticalCongressPA-226(2008).HPTLCofolmesartanmedoxomil(anangiotensin-IIantagonist)onsilicagelwithtoluene-acetonitrile-methanol-ethylacetate-aceticacid(mobilephaserationotspecifiedbytheauthors).ThehRFvaluewas56.Quantitativedeterminationbyabsorbancemeasurementat262nm.The linearitywasbetween�00-800ng/spot.Themethodwassuitable forseparationofolmesartanmedoxomil fromdegradationpro-ductsobtainedbyforcedstressconditions(acid,alkali,peroxide,light,heat).

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104074 A.CHABUKSWAR*,S.JAGDALE,S.KUMBHAR,R.WAVHALE(*BombayCollegeofPhar-macy,Mumbai,Maharashtra,India):SimultaneousHPTLCestimationofcertainantihypertensivedrugs in tabletdosage form.60th IndianPharmaceuticalCongressPA-2�0 (2008).HPTLCofamlodipinebesylate(AB)andtelmisartan(TMS)onsilicagelwithethylacetate-1,4-dioxane-methanol-25%ammonia�0:�:6:�.ThehRFvaluewas16forTMSand��forAB.Quantitativedeterminationbyabsorbancemeasurement at �2�nm.Themethodwas linear in the rangeof100-500µg/mL(TMS)and200-1000µg/mL(AB),averagerecoverywas100.2-100.4%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104075 MrinaliniDAMLE*,K.BOTHARA,KirtiTOPAGI(*Dept. foChem.A.I.S.S.M.S.CollegeofPharma,KennedyRoad,R.T.O.Pune411044,India.,[email protected]):Stability-indi-catingHPTLCmethodfordeterminationofnebivololhydrochlorideandvalsartan.Ind.J.Phar-ma. Sci. 8(4), 198-201(2009). HPTLC of nebivolol hydrochloride and valsartan on silica gelwithethylacetate-methanol-aceticacid12:2:1inatwintroughchambersaturatedfor15min.Quantitativedeterminationbyabsorbancemeasurementat240nmforvalsartanand280nmfornebivololhydrochloride.Themethodwasfoundtobelinearintherangeof600-1400ng/bandfor valsartan 1200-2800 ng/band for nebivolol.The sample were subjected to different stressconditions (acid,alkali,oxidation,photolysis, thermal)andalldegradationproductswerewellseparatedfromthemaincompounds.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104076 R.S.DAREKAR,A.B.KHETRE,S.M.SINGH,M.C.DAMLE*(*DepartmentofPharmaceu-ticalChemistry,AISSMSCollegeofPharmacy,NearR.T.O.,KennedyRoad,Pune411001,India,[email protected]):HPTLCquantitationof2-hydroxy-4-methoxybenzaldehydeinHemidesmusindicusR.Br.rootpowderandextract.J.PlanarChromatogr.22,45�-456(2009).HPTLCof2-hydroxy-4-methoxybenzaldehydeandbiologicalextractsonsilicagelwithtoluene-ethylacetate-aceticacid7:2:1inatwintroughchambersaturatedfor20min.Quantitativedeter-minationbyabsorbancemeasurementat277nm.

herbal,traditionalmedicine,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104077 P. DESHPANDE*, G. SHRIDHARAN, L.ANANDI, D. JADHAV, M. DAMLE, S. GANDHI(*Dept.ofPharmaceuticalAnalysis,AISSMSCollegeofPharmacy,KennedyRoad,Pune, In-dia,[email protected]):Validatedmethoddevelopmentforestimationofatorvas-tatincalciumandfenofibrateinfixeddosecombinationbyHPTLC.ThePharmaReview7(�9),151-15�(2009).HPTLCofatorvastatincalciumandfenofibrateonsilicagel(pre-washedwithmethanol)withchloroform-methanol4:1over20mmwithchambersaturation.ThehRFvalueofatorvastatincalciumwas29andoffenofibrate77.Themethodwaslinearintherangeof200-1000ng/bandforatorvastatincalciumand�20-1600ng/bandforfenofibrate.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104078 S.R.DHANESHWAR*,V.K.BUSARI,M.V.MAHADIK(*BharatiVidyapeethUniversity,Poo-na College of Pharmacy, Department of Pharmaceutical Chemistry, Pune, Maharashtra, India4110�8; [email protected]): Application of a stability-indicating thin-layer chro-matographicmethod to thedeterminationof tenatoprazole inpharmaceuticaldosage forms. J.

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CAMAGBIBLIOGRAPHYSERVICE No.10420

AOACInt.92,�87-�9�(2009).TLCoftenatoprazole-beforeandafteracidandalkalihydroly-sis,oxidationandphotodegradation-onsilicagel,prewashedwithmethanolanddriedat110°Cfor5min,withtoluene-ethylacetate-methanol6:4:1inatwintroughchambersaturatedwiththemobilephasefor�0minat25°C.Quantitativedeterminationbyabsorbancemeasurementat�06nm.Thelimitofdetectionandlimitofquantitationwere50and100ng/spot,respectively.

qualitycontrol,pharmaceutical,research,densitometry,quantitativeanalysis �2a

104079 V.V.DIGHE,G.A.CHAREGAONKAR*(*S.P.Mandali‘sRamnarainRuiaCollege,Matunga,Mumbai 400 019, India; [email protected]): HPTLC analysis of myristicin andsafroleinseedpowderofMyristicafragransHoutt.J.PlanarChromatogr.22,445-448(2009).HPTLCofmyristicin,safroleandextractofseedsonsilicagel,prewashedwithmethanol,withtolueneinanautomaticdevelopingchambersaturatedfor20min.Quantitativedeterminationbyabsorbancemeasurementat210nmformyristicinandat290nmforsafrole.

pharmaceuticalresearch,qualitycontrol,herbal,traditionalmedicine,HPTLC,densitometry,quantitativeanalysis �2e

104080 AvaniDODIYA,ShwetaPAWAR,C.PATEL (*SchoolofPharmacyandTechnologyManage-ment,NMIMSUniversity,Mumbai,Maharashtra, India):Simultaneousdeterminationofnebi-vololhydrochlorideandhydrochlorothiazideintabletsbyhigh-performancethin-layerchromato-graphy.AbstractNo.F-280,61stIPC(2009).HPTLCofnebivololHClandhydrochlorothiazideonsilicagelwithtoluene-ethylacetate-methanol-25%ammonia�0:27:17:2.ThehRFvaluewas�8and68forhydrochlorothiazideandnebivolol,respectively.Quantitativedeterminationbyabsorbancemeasurementat281nm.Themethodwaslinearintherangeof500-�000ng/bandfornebivololand1000-6000ng/bandforhydrochlorothiazide.Recoverywas100%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104081 N.DUBEY*,N.DUBEY,R.MEHTA,A.K.SALUJA(*DeviAhilyaVishwaVidyalaya,SchoolofPharmacy, Indore, India;[email protected]) :DeterminationofpsoralenandplumbaginfromitspolyherbaloilformulationsbyanHPTLCdensitometricmethod.J.AOACInt.92,779-784(2009).HPTLCofpsoralenandplumbaginandextractsofayurvedicpolyherbaloilformulationsonsilicagelat22°Cand55%humiditywithtoluene-ethylacetate�:1inatwintroughchamberwithchambersaturation.UVspectrawererecordedfrom200to600nm;densitometricmeasurementswereperformedat�02nm(forpsoralen)and275nm(forplumbagin).

traditionalmedicine,herbal,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104082 N.DUBEY*,N.DUBEY,R.MEHTA,A.SALUJA(*DeviAhilyaVishwavidyalaya (DAVV),SchoolofPharmacy,Indore,MadhyaPradesh,India;[email protected]):Estima-tionofcatechininAyurvedicoilformulationscontainingAcaciacatechu.J.AOACInt.92,1021-1026 (2009). HPTLC of catechin and extracts from polyherbal oil formulations on silica gelusingchloroform-acetone-0.1%formicacid77:15:8%inatwintroughchambersaturatedfor20min.Quantitativedeterminationbyabsorbancemeasurementat296nm.Thelimitofdetec-tionandquantificationwas6and20ng/spot,respectively.

traditionalmedicine,herbal,qualitycontrol,HPTLC,quantitativeanalysis,densitometry �2e

10408� NidhiDUBEY*,N.DUBEY,R.MEHTA,A.SALUJA(*DeviAhilyaVishwavidyalaya,SchoolofPharmacy,Indore,M.P.,India):RapiddensitometricdeterminationofAlliumsativuminpo-lyherbaloilformulations.60thIndianPharmaceuticalCongressPA-202(2008).HPTLCofallyldisulphide(anactiveingredientofAlliumsativum,garlic)onsilicagelwithn-hexane.ThehRFvaluewas52.Quantitativedeterminationbyabsorbancemeasurementat298nm.Thelinearityrangewas200-1200ng/spot.Severalpolyherbal formulationscontaininggarlicwereanalyzedwiththeproposedmethodusingallyldisulphideasmarker.

traditionalmedicine,herbal,HPTLC,densitometry,quantitativeanalysis �2e

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CAMAGBIBLIOGRAPHYSERVICE No.10421

104085 R.R.DURÓN,L.CENICEROSALMAGUER,N.C.CAVAZOSROCHA,P.G.S.FLORES,No-emi WAKSMAN DETORRES* (*UniversidadAutónoma de Nueve León, Departamento deQuímicaAnalítica, Facultad de Medicina, PO Box 2�16, SucursalTecnológico, 64841, Mon-terreyNuevoLeón,Mexico;[email protected]):Comparisonofhigh-performanceliquidchromatographicand thin-layerchromatographicmethods fordeterminationofaloin inherbalproductscontainingAloevera.J.AOACInt.91,1265-1270(2008).TLCofaloinAandextractsof dried herbal products applied bandwise on silica gel with ethyl acetate - methanol - water100:17:10at25°Cwithchambersaturation.Detectionbysprayingwith1%methanolicdiphe-nylboricacid2-aminoethylester(naturalproductsreagent),followedby5%ethanolicpolyethyle-neglycol400andvisualizationunderUVlightat�65nm.ThehRFvalueofaloin(asamixtureofaloinAandBstereoisomers)was�8.Linearitywasbetween0.5and10mg/L.Precision(%RSD)ofthehRFvalueofthealoinbandwas0.88.Thelimitofdetectionwas1µg/band.Recovery(bystandardaddition)was87.6%foraloin.

qualitycontrol,herbal,pharmaceuticalresearch,qualitativeidentification �2e

104086 HalinaEKIERT*,A.SZEWCZYK,A.KUS(*JagiellonianUniversity,CollegiumMedicum,Fa-cultyofPharmacy,ChairandDepartmentofPharmaceuticalBotany,9MedycznaStreet,�0-688Kraków,Poland;[email protected]):FreephenolicacidsinRutagraveolensL.invitrocul-ture.Pharmazie64,694-696(2009).PreparativeTLCandHPTLCofprotocatechuicacid,vanil-licacid,syringicacid,andp-coumaricacidandmethanolicextractsonsilicagel.DetectionunderUVlightat254nm.

pharmaceuticalresearch,HPTLC,herbal,qualitative,identification,preparativeTLC �2e

104087 IzabellaFECKA(WroclawMedicalUniversity,DepartmentofPharmacognosy,Pl.Nankierea1,50-140Wroclaw,Poland; [email protected]):Developmentofchromatographicme-thodes fordeterminationofagrimoniinandrelatedpolyphenols inpharmaceuticalproducts. J.AOACInt.92,410-418(2009).HPTLCofagrimoniin,pedunculagin,ellagicacid,gallicacidandcatechinandplantextractsonsilicagel,RP-18andaminophaseinahorizontalchamber.Thebestresolutionandselectivitywereachievedwithdiisopropylether-acetone-formicacid-wa-ter4:�:2:1,tetrahydrofuran-acetonitrile-water�:1:6,andacetone-formicacid�:2.PolyphenolsweredetectedunderUVlightat254nmandinvisiblelightaftersprayingwith1%methanoliciron(III)chlorideorbis-diazotizedsulfanilamideandaftertreatmentwithavanillin-hydrochloricacidreagent.

herbal,pharmaceuticalresearch,qualitycontrol,HPTLC,qualitativeidentification �2e

104088 J.FISCHEDICK*,R.GLAS,A.HAZEKAMP,R.VERPOORTE(*DivisionofPharmacognosy,LeidenUniversity,GorlaeusLaboratories, 2���CCLeiden,TheNetherlands, [email protected]):AqualitativeandquantitativeHPTLCdensitometrymethodfortheanalysisofcannabinoi-dsinCannabissativa.Phytochem.Anal.20,421-426(2009).HPTLCofdelta-9-tetrahydrocanna-binolintheflowertopsofCannabissativaonsilicagelwithchloroformwithchambersaturationfor20min.Quantitativedeterminationbyabsorbancemeasurementat206nm.DerivatizationbydippinginFastBlueBsolutionfor5s.ThehRFvalueofdelta-9-tetrahydrocannabinolwas47andselectivityregardingmatrixwasgiven.Linearitywasgivenbetween50and500ng/zone.The limit of quantification and detection was 50 and 10 ng/zone, respectively.The intra- andinter-day repeatability (%RSD,n=9)werenot higher than5.0%.Recoverywas85.8% fordelta-9-tetrahydrocannabinolindecarboxylatedCannabissamples.Themethodwasshowntobecomparablewithinasmalldegreeoferror(0.5%)toresultsfromavalidatedHPLCmethod.toxicology,qualitycontrol,

herbal,HPTLC,densitometry,quantitativeanalysis,qualitativeidentification �2e

104089 M.GAME*,M.JADHAO,V.WANKHADE,G.GHENGE(*VidyabhartiCollegeofPharmacy,Amravati,Maharashtra,India):EstimationofandrographolideinherbalpowderandpolyherbalasavabyHPTLC.AbstractNo.F-299,61stIPC(2009).HPTLCofherbalpowderandpolyherbalformulationcontainingAndrographispaniculataonsilicagelwithbenzene-ethylacetate1:1.

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CAMAGBIBLIOGRAPHYSERVICE No.10422

Quantitativedeterminationbyabsorbancemeasurementat222nm.Thecalibrationcurveforan-drographolidewaslinearintherangeof�60-660ng/band.

qualitycontrol,herbal,HPTLC,densitometry �2e

104090 D. GANDHI*, N. PATEL, P. MEHTA (*Institue of Pharmacy, Nirma Univeristy,Ahmedabad,Gujarat,India):DevelopmentandvalidationofHPTLCmethodforsimultaneousdeterminationoflevodopaandcarbidopaintheircombineddosageform.AbstractNo.F-246,61stIPC(2009).HPTLCoflevodopaandcarbidopaonsilicagelwithacetone-chloroform-n-butanol-aceticacid-water50:45:42:�5:25.Quantitativedeterminationbyabsorbancemeasurementat28�nm.Themethodwaslinearintherangeof200-700ng/bandforbothcompounds,witharecoveryof98.7-99.9%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,comparisonofmethods �2a

104091 S.V.GANDHI*,S.I.KHAN,R.T.JADHAV,S.S.JADHAV,G.A.JADHAV(*AISSMSCollegeofPharmacy,DepartmentofPharmaceuticalAnalysis,Pune,India;[email protected]):High-performance thin-layerchromatographicdeterminationof rabeprazolesodiumanddomperidoneincombineddosageform.J.AOACInt.92,1064-1067(2009).HPTLCofrabepra-zolesodiumanddomperidoneintabletsonsilicagel(prewashedwithmethanolanddriedat110°Cfor5min)withtoluene-acetone-methanol9:9:1inatwintroughchambersaturatedwiththemobilephasefor5min.Quantitativedeterminationbyabsorbancemeasurementat285nm.ThehRFvalueofrapebrazolesodiumanddomperidonewas5�and�2,respectively.Linearitywasbetween50and800ng/bandforbothsubstances.

qualitycontrol,pharmaceutical,research,HPTLC,quantitativeanalysis,densitometry �2a

104092 M.GANESH*,S.SWANT,R. JAMBHALE,A.KASABE(*ArvindGawaliCollegeofPhar-macy, Satara, Maharashtra, India): Extraction and estimation of theobromine in marketed teabyHPTLCandUVmethod.AbstractNo.F-277,61st IPC(2009).HPTLCof theobromine indifferentextractsoftea(Cameliasinensis)onsilicagelwithethylacetate-methanol27:�.Quan-titativedeterminationbyabsorbancemeasurementat274nm.Themaximumcontentoftheobro-mineinteasampleswas2.�%.Linearitywasintherangeof�-15µg/zone.Thelimitofdetectionandquantificationwas�0and140ng/spot,respectively.

pharmaceuticalresearch,herbal,HPTLC,densitometry,quantitativeanalysis �2e

10409� A.GANTAIT*,K.MUKHERJEE,S.PONNUSANKAR,P.MUKHERJEE(*JadavpurUniver-sity,SchoolofNaturalProductStudies,Kolkata,India):Avalidatedmethodforstandardizationof Centella asiatica extract. 60th Indian Pharmaceutical Congress PG-244 (2008). HPTLC ofCentellaasiaticaextractwithasiaticosideasmarkeronsilicagelwithchloroform-glacialaceticacid-methanol-water15:8:�:2withchambersaturation.Detectionbysprayingwithanisalde-hydereagent, followedbyheatinginovenandimmediatequantitativedeterminationbyabsor-bancemeasurementat607nm.ThehRFvalueofasiaticosidewas81.Linearitywasintherangeof0.96-�.�6µg/spot.Hydroalcoholicextractscontainedapprox.�.2%ofasiaticoside.

herbal,HPTLC,densitometry,quantitativeanalysis,postchromatographicderivatization �2e

104094 AGANTAIT*,N.NEMA,A.SAHU,S.PANDIT,S.BHADRA,P.MUKHERJEE(*SchoolofNaturalProductStudies, JadavpurUniversity,Kolkata7000�2, India):Avalidatedmethod forquantificationofglycyrrhizininGlycyrrhizaglabraextractbyHPTLC.AbstractNo.9162,IHCB(2009).HPTLCofglycyrrhizininmethanolic(70%)extractsofGlycyrrhizaglabraonsilicagelwithchloroform-methanol-water1�0:72:15.Quantitativedeterminationbyabsorbancemeasure-mentat254nmandat420nmaftersprayingwithanisaldehydereagent.Themethodwaslinearintherangeof0.8-�.8µg/spot.Thelimitofdetectionandquantificationwas0.16and0.52µg/spot,respectively.Glycyrrhizinwasusedasbioactivemarkerforqualitycontrol.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,postchromatographicderivatization �2e

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CAMAGBIBLIOGRAPHYSERVICE No.1042�

104095 A.GANTAIT*,P.ROY,S.PANNUSANKAR,P.MUKHERJEE,B.SAHA(*SchoolofNaturalProductStudies,Jadavpur,Kolkata7000�2,India):StandardizationofTinosporacordifoliaex-tractthroughHPTLCdensitometry.AbstractNo.91��4,IHCB(2009).StandardizationofTinos-poracordifoliaextractbyHPTLCofsyringicacidonsilicagelwithchloroform-methanol8:1.ThehRFvalueofsyringicacidwas5�.Quantitativedeterminationbyabsorbancemeasurementat254nm.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104096 VidyaGAWANDE*,ManishaPURANIK,A.CHANDEWAR(*PataldhamalWadhwaniCollegeofPharmacy,Yavatmal,Maharashtra,India):DevelopmentofvalidatedHPTLCmethodforsi-multaneousestimationofdomperidoneincombinationwithesomeprazolemagnesiuminsoliddosageform.60thIndianPharmaceuticalCongressPA-220(2008).HPTLCofdomperidoneandesomeprazoleonsilicagelwithchloroform-methanol9:1withchambersaturationfor�0min.ThehRFvaluewas25fordomperidoneand46foresomeprazole.Quantitativedeterminationbyabsorbancemeasurementat295nm.Themethodwaslinearintherangeof60-�00ng/spotfordomperidoneand80-400ng/spotforesomeprazole.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104097 S. GHODKE*,A. RATHORE, L. SATHIYANARAYANAN, K. MAHADIK (*BharatiVidya-peethUniversity,PoonaCollegeofPharmacy,Pune,Maharashtra,India):ValidatedHPTLCme-thodforsimultaneousestimationofisotretinoinandrrythromycininbulkdrugandtopicalgelform.AbstractNo.F-24�,61stIPC(2009).HPTLCofisotretinoinanderythromycinonsilicagelwithtoluene-dimethylsulfoxide-methanol65:2:25.Quantitativedeterminationbyabsorbancemeasurementat�40nmbeforederivatization for isotretinoinandat410nmforerythromycinafterderivatizationwith10%sulfuricacidfollowedbyheatingat100°Cfor15min.ThehRFvalue was �8 and 55 for isotretinoin and erythromycin, respectively.The linearity was in therangeof�0-150ng/bandforisotretinoinand1200-6000ng/bandforerythromycin.Recoverywasbetween96.9and99.7forisotretinoinandbetween97.2and102.6%forerythromycin.Intra-dayandinter-dayrelativestandarddeviationsforbothcomponentswere<2.0%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104098 S.GOHIL*,S.PATEL,N.PATEL,D.PATEL (*ShreeS.K.PatelCollegeofPharmaceuticalEducationandResearch,GanapatUniversity,Mehsana, India):Estimationof atomoxetinehy-drochloride by HPTLC method in pharmaceutical formulations. 60th Indian PharmaceuticalCongressPA-212(2008).HPTLCofatomoxetineHClonsilicagelwithacetone-methanol -triethylamine�0:15:2.Quantitativedeterminationbyabsorbancemeasurementat275nm.Themethodwaslinearintherangeof�00-2100ng/spotandwassuitableforroutinequalitycontrolofpharmaceuticalformulations.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104099 P.HAMRAPURKAR*,N.LONE,K.KAMAT,T.SAMBARE(*PrincipalK.M.KundnaniCol-legeofPharmacy,Mumbai,Maharashtra,India):Quantitativedeterminationofaloe-emodininRheumemodiusingHPTLC.60thIndianPharmaceuticalCongressPA-224(2008).HPTLCofaloe-emodininextractofRheumEmodi(preparedbysupercriticalfluidextraction)onsilicagelwithtoluene-acetone-formicacid80:20:1.Quantitativedeterminationbyabsorbancemeasure-mentat254nm.Linearitywasintherangeof100-400ng/spot.Comparedwithotherextractiontechniquessupercriticalfluidextractionwasmoreeffcientandlesstimeconsuming.

herbal,HPTLC,quantitativeanalysis,qualitativeidentification �2e

104100 T.HONG,M.L.JEONG,M.ZAHN,B.A.FAY,K.LEE,H.HWANGBO,E.PARK,M.KIM,W.MA*(*UnigenInc.,QualityControl/QualityAssuranceDepartment,2660WillametteDr,NE,Lacey,WA 98516, USA;[email protected]): Detection of the potential adulterantTeuc-

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CAMAGBIBLIOGRAPHYSERVICE No.10424

riumchamaedrysinScutellariabaicalensisrawmaterialandextractbyhigh-performancethin-layer chromatography. J.AOAC Int. 92, 785-788 (2009). HPTLC of plant extracts and herbalpreparationsappliedbandwiseonsilicagelwithethylacetate-formicacid-aceticacid-water100:11:11:25afterpreconditioningfor5min.Detectionbyimmersioninnaturalproductsrea-gent(diphenylboricacid2-aminoethylester)followedbypolyethyleneglycol400reagentfor2s.Afterair-dryingtheplateswereevaluatedunderUV�66nm.

herbal,traditionalmedicine,qualitycontrol,HPTLC,qualitativeidentification �2e

104101 F.HOU(HouFeng)*,F.LIU(LiuFang),Q.MO(MoQiwu)(*GuangzhouMeichenPharm.Co.Ltd.,Guangzhou510075,China):(StudyofthequalitystandardforConghuangBushencapsules)(Chinese).J.ChineseTrad.&Herb.Drugs40(8),1249-1252(2009).TLCofextractsoftheTCMdrugonsilicagelwith1)methanol-aceticacid-water18:1:4;2)petroleumether(60-90°C)-ethyl acetate1:1;�) toluene - ethyl acetate -methanol5:5:�;4)petroleumether (60-90°C) -ethylacetate-formicacid15:5:1.Detection1)bysprayingwithpotassiumiodobismuthatereagent;2)underUV254nm;�)bysprayingwith5%AlCl�inethanolandevaluationunderUV�65nm.

qualitycontrol,pharmaceuticalresearch,traditionalmedicine,quantitativeanalysis,qualitativeidentification �2e

104102 X.HOU(HouXiaotao)*,L.MU(MuLiqun),L.HUANG(HuangLifen),J.ZHOU(ZhouJi-angyu) (*Guangxi Inst.TCM,Nanning,Guangxi 5�0001,China): (Studyon thequality stan-dardforYixueanPills)(Chinese).ChineseJ.Hospit.Pharm.29(8),686-688(2009).TLCoftheextractsofYixueanpillsonsilicagelwith1)chloroform-ethylacetate-acetone-formicacid60:25:25:4;2)n-hexane-chloroform-methanol15:5:2;�)ethylacetate-formicacid-aceticacid-water15:1:1:2.Detection1)underUV254nm;2)byexposuretoiodinevaporandunderUV254nm;�)bysprayingwith10%sulfuricacidinethanolfollowedbyheatingat105°CuntilcolorationevaluationundervisiblelightandUV254nm.

cosmetics,pharmaceuticalresearch,traditionalmedicine,qualitycontrol,qualitativeidentification,quantitativeanalysis,review,densitometry �2c

10410� J.HUANG(HuangJiefen)*,H.LI(LiHuixia),H.DENG(DengHuimin)(*GuangzhouZhongyiPharm. Co. Ltd., Guangzhou 5105�0, China): (Study of the quality standard for Xinyi Biyanpills)(Chinese).J.ChineseTrad.&Herb.Drugs40(8),245-247(2009).TLCoftheTCMdrugextractson silicagelwith1)petroleumether (90-120 °C) - toluene - formicacid20:40:1;2)chloroform-ethylacetate-methanol-water-formicacid�:10:2:2:2;�)ethylacetate-formicacid-water12:2:�.Detection1)bysprayingwith10%sulfuricacidinethanolfollowedbyhea-tingat105°C;2)byexposuretoiodinevapor;�)underUV254nm.

pharmaceuticalresearch,qualitycontrol,traditionalmedicine,herbal,qualitativeidentification,quantitativeanalysis �2e

104104 X.HUANG(HuangXiaoyu)*,N.HUANG(HuangNojia)(*WannianqingPharm.Co.,Guang-dongProv.,Shantou,Guangdong5150�1,China):(SimultaneousidentificationofFructusSchi-sandraesphenantherae,RhizomaAcoritatarinowii,RhizomaChuanxiongandvitaminEinNao-libaopillsbythin-layerchromatography)(Chinese).J.ChinesePharm.Standard10(4),284-286(2009).TLC of Naolibao pill extracts on silica with n-hexane - ethyl acetate 5:1. QualitativeidentificationbydetectionunderUV254nmand�65nm.Themethodissimple,rapid,reliable,andsuitableforthequalitycontroloftheTCMformulation.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,herbal,qualitativeidentification �2c

104105 Demiana I. NESSEEM*, C.G. MICHEL,A.A. SLEEM,T.S. EL-ALFY (*Pharmaceutics De-partment, National Organization for Drug Control & Research (NODCAR), 6 Abou HazemSt. PyramidsAve, Cairo, Egypt; [email protected]): Formulation and evaluation ofantihyperglycemic leafextractsofZizyphusspina-christi (L.)WILLD.Pharmazie64,104-109

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CAMAGBIBLIOGRAPHYSERVICE No.10425

(2009).TLCofchristinin-Aasmarkerandleafextractsonsilicagelwithchloroform-methanol-water1�:8:2andbutanol-aceticacid-water4:1:5(upperphase).Detectionbysprayingwithp-anisaldehydereagent.

pharmaceuticalresearch,herbal,qualitativeidentification �2e

104106 P.S.JAIN(R.C.PatelCollegeofPharmacy,KarwandNaka,ShirpurDist.Dhule425405(M.S.)India):Stability-indicatingHPTLCdeterminationofambroxolhydrochloride inbulkdrugandpharmaceuticaldosageform.J.Chromatogr.Sci.48(1),45-48(2010).HPTLCofambroxolhy-drochlorideonsilicagelwithmethanol-triethylamine2:�.ThehRFvalueofambroxolwas5�.Quantificationbyabsorbancemeasurementat254nm.Linearitywasgivenintherangeof100-1000ng/spotwithr2=0.9966(viapeakarea).Thelimitsofdetectionandquantitationwere10and�0ng/spot,respectively.Ambroxolhydrochloridewassusceptibletodegradationunderoxi-dationandthermalstressconditions.Themethodissuitableforpuritytestingofthedrugasitdetectstherelatedimpurities.

pharmaceuticalresearch,qualitycontrol,HPTLC,qualitativeidentification,quantitativeanalysis,densitometry �2c

104107 V.JAITAK*,A.GUPTA,V.KAUL,P.AHUJA(*NaturalPlantProductsDiv. InstituteofBio-resourceTechnology, Palampur 176061, H.P., India, [email protected]):Validated high-performance thin-layer chromatography method for steviol glycosides in Stevia rebaudiana. J.Pharm.Biomed.Anal.47,790-794(2008).HPTLCofthesteviolbioside,steviosideandrebau-diosideAinSteviarebaudiana leavesonsilicagelwithethylacetate-ethanol-water20:5:�.Detectionbysprayingwithaceticanyhdride-sulphuricacid-ethanol1:1:10reagent.Quantita-tivedeterminationbyabsorbancemeasurementat510nm.Linearitywasintherangeof160-960ng/spotforsteviolbioside,1-6µg/spotforsteviosideand0.5-�µg/spotforrebaudiosideAwithgoodcorrelationcoefficients(0.998-0.999).Themethodwasusedfortheassayofsteviolglyco-sidesinS.rebaudianaleavescollectedfromtendifferentlocations.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104108 P.JHA*,S.KHAN,R.PARVEEN,S.AHMAD(*JamiaHamdard,FacultyofPharmacy(Ham-dardUniversity),NewDelhi,India):DevelopmentandvalidationofnovelHPTLCmethodforquantitativeestimationofomeprazoleinpharmaceuticaldosageform.60thIndianPharmaceuti-calcongressPA-2�4(2008).HPTLCofomeprazoleonsilicagelwithchloroform-methanol9:1.ThehRFvaluewas�9.Quantitativedeterminationbyabsorbancemeasurementat�02nm.Themethodwaslinearintherangeof5-�000ng/spot,recoverywas99.5%.Themethodwassuitableforroutinequalitycontrolofformulations.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104109 MaithileeJOSHI*,A.NIKALJE,M.SHAHED,M.DEHGAN(*Y.B.ChavanCollegeofPhar-macy,Dr.RafiqZakariaCampus,RauzaBagh,Aurangabad4�1001,India,[email protected]):HPTLCmethod for the simultaneous estimation of emtricitabine and tenofovir in tablet dosage form.Ind. J. Pharma. Sci. 71(1), 95-97 (2009). HPTLC of emtricitabine and tenofovir on silica gelwithchloroform-methanol9:1.Quantitativedeterminationbyabsorbancemeasurementat265nm.Thecalibrationcurvewaslinearbetween200and1000ngwitharegressioncoefficientof0.9995.

pharmaceuticalresearch,densitometry,HPTLC,quantitativeanalysis �2a

104110 S.S.KADUKAR,S.V.GANDHI*,P.N.RANJANE,S.S.RANHER(*DepartmentofPharmaceu-ticalAnalysis,AISSMSCollegeofPharmacy,KennedyRoad,NearR.T.O.,Pune411001,Ma-harashtra, India; [email protected]):HPTLCanalysisofolmesartanmedoxomilandhydrochlorothiazideincombinationtabletdosageforms.J.PlanarChromatogr.22,425-428

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CAMAGBIBLIOGRAPHYSERVICE No.10426

(2009).HPTLCofolmesartanmedoxomilandhyrochlorothiazideonsilicagel,prewashedwithmethanol,withchloroform-methanol-toluene6:4:5inatwintroughchambersaturatedfor15min.Quantitativedeterminationbyabsorbancemeasurementat258nm.

pharmaceuticalresearch,qualitycontrol,HPTLC �2a

104111 R.KAKDE*,D.SATONE,N.BAWANE(*DepartmentofPharmaceuticalSciences,RTMNag-purUniversity,Nagpur-4400��,Maharashtra,India;[email protected]):HPTLCmethodforsimultaneous analysis of escitalopram oxalate and clonazepam in parmaceutical preparations.J.PlanarChromatogr.22,417-420(2009).HPTLCofescitalopramoxalateandclonazepamonsilicagel,prewashedwithmethanol,inatwintroughchambersaturatedfor20minat25°Cwithmethanol-toluene-triethylamine10:�5:1.Quantitativedeterminationbyabsorbancemeasure-mentat25�nm.

pharmaceuticalresearch,qualitycontrol,HPTLC,quantitativeanalysis,densitometry �2a

104112 P. KAKULTE*, M. DESHPANDE, S. CHAUDHRI,V. KASTURE (*Amrutvahini College ofPharmacy, Ahemadnagar, Maharashtra, India): High-performance thin-layer chromatographicdeterminationofambroxol inhumanplasmabyliquid-liquidextractionanditsuseinstabilitystudy.AbstractNo.F-286,61stIPC(2009).HPTLCofambroxol(extractedfromplasmawithdiethylether,aftercentrifugationtheorganiclayerwasevaporatedandtheresiduewastakenupin1mLofmethanol)onsilicagelwithacetonitrile-methanol-triethylamine41:5:4.Quantitativedeterminationbyabsorbancemeasurementat254nm.

pharmaceuticalresearch,clinicalroutineanalysis,HPTLC,quantitativeanalysis �2b

10411� R.KANT*,M.GUPTA(*DelhiInstituteofPharmaceuticalScienceandResearchNewDelhi,India):HPTLCmethoddevelopmentanditsvalidationfordeterminationofranolazineinphar-maceuticalformulations.AbstractNo.F-259,61stIPC(2009).HPTLCofranolazineonsilicagelwithmethanol-toluene9:11inatwintroughchamberwithchambersaturationfor�0min.ThehRFvaluewas64.Quantitativedeterminationbyabsorbancemeasurementat271nm.Themethodwaslinearintherangeof2-14µg/band.Recoverywas98.�-101.4%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104114 A. KAUR*,V. RAVICHANDRAN, P. JAIN, R.AGRAWAL (*Pharmaceutical Chemistry Re-searchLab.Dept.ofPharmaceuticalSciences,Dr.HariSinghGourUniv.Sagar,MP47000�,India, [email protected]): High-performance thin-layer chromatography method forestimationofconessineinherbalextractandpharmaceuticaldosageformulations.J.Pharm.Bi-omed.Anal.46,�91-�94(2008).TLCofconessineonsilicagelwith toluene-ethylacetate-diethylamine1�:5:2inatwintroughchambersaturatedat25°C.Detectionbytreatmentwithmo-difiedDragendorff‘sreagent.Quantitativedeterminationbyabsorbancemeasurementat520nm.ThehRFvalueofconessinewas82.Linearitywasintherangeof1-10µg/zonewithacorrelationcoefficientof0.9998viapeakarea.

pharmaceuticalresearch,herbal,densitometry,quantitativeanalysis �2e

104115 H.KHAN*,M.ALI,A.AHUJA,S.AHMAD, J.Ali (*JamiaHamdard,FacultyofPharmacy,NewDelhi,India):StabilityindicatingTLCmethodforsimultaneousestimationofaceclofenacandparacetamolinbulkdrugsandintheirfixeddosecombinations.60thIndianPharmaceuticalCongressPA-218(2008).TLCofaceclofenacandparacetamolonsilicagelwithtoluene-iso-propylalcohol - ammonia8:7:1.ThehRFvalueofaceclofenacwas24andofparacetamol68.Quantitativedeterminationbyabsorbancemeasurementat254nm.Linearitywasintherangeof25-2000ng/bandwithcorrelationcoefficientsof0.9998foraceclofenacand0.9996forparace-tamol.Thelimitsofdetectionandquantificationwere25and150ng/bandforaceclofenacand50and200ng/bandforparacetamol.Bothdrugsweresubjected toacidandalkalihydrolysis,oxidativedegradation,andphotodegradation.Thedegradationproductswerewellresolvedfromthepuredrug.

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CAMAGBIBLIOGRAPHYSERVICE No.10427

pharmaceuticalresearch,quality,control,densitometry,quantitativeanalysis �2a

104116 P.KHATWANI*,S.KULKARNI(*BombayCollegeofPharmacy,Mumbai,Maharashtra,India):Asensitivehigh-performancethin-layerchromatographymethodforestimationofwedelolactonefromEcliptaalbabydifferentmethodsofextraction.AbstractNo.F-272,61stIPC(2009).HPT-LCofwedelolactoneonsilicagelwithtoluene-ethylacetate9:1.Quantitativedeterminationbyfluorescencemeasurementat�66nm.Themethodwaslinearintherangeof500-8000ng/mL.Recoverywasintherangeof100.2-101.0%.Theplantmaterialwasextractedusingpercolation,maceration,hotsolventextraction,supercriticalfluidextraction,microwaveassistedextraction,ultra sonication,andanorbital shaker.Quantificationofwedelolactone in theextracts showedhighestlevelsforSoxhletextractionandlowestlevelsforsupercriticalfluidextraction.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2a

104117 A. KHODKE*, M. DAMLE, K. BOTHARA (*AISSMS College of Pharmacy, Pune, Maha-rashtra, India):A vlidated stability indicating HPTLC method for simultaneous estimation ofirbesartanandhydrochlorothiazide.AbstractNo.F-269,61stIPC(2009).HPTLCofhydrochlo-rothiazideandirbesartanonsilicagelwithacetonitrile-chloroform5:6.ThehRFvaluewas27and45forirbesartanandhydrochlorothiazide,respectively.Quantitativedeterminationbyabsor-bancemeasurementat270nm.Thesamplewasexposedtodifferentstressconditions(acid,al-kali,oxidative,photodegradation,thermal).Neitherofthecompoundsshoweddegradationunderthermalandphotodegradationconditions,butbothcompoundsshowedsignificantdegradationunderacid,alkaliandhydrolyticconditions.Degradedproductswerewellresolvedfromthepa-rentcompounds.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104118 E.KILINC*,F.AYDIN(*DepartmentofChemistry,FacultyofArtandScience,UniversityofDicle,Diyarbakir,21280,Turkey;[email protected]):Stability-indicatingHPTLCanalysisofflurbiprofeninpharmaceuticaldosageforms.J.PlanarChromatogr.22,�49-�54(2009).HPTLCofflurbiprofen(2-(�-fluoro-4-phenyl)phenylpropanoicacid)anddegradationproductsonsilicagel,prewashedwithmethanol,withchloroform-acetone-xylene5:2:1inatwintroughchambersaturatedfor20min.Quantitativedeterminationbyabsorbancemeasurement(theauthorsreportnowavelength).Linearitywasbetween50and600ng/band.Thelimitofdetectionandquantifi-cationwas10and�2ng/band,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104119 S.KOTHARI*,D.PATEL,N.SHAH,B.SUHAGIA(*ShriB.M.ShahCollegepfPharma.Ed-ucationandResearch,Modasa,Gujarat,India):HPTLCmethodforsimultaneousestimationoftelmisartanandhydrochlorothiazidefromtheircombinationdrugproduct.AbstractNo.F-�78,61stIPC(2009).HPTLCoftelmisartanandhydrochlorothiazideonsilicagelwithchloroform-toluene-methanol2:5:5.ThehRFvaluewas5�and75fortelmisartanandhydrochlorothiaziderespectively.Quantitativedeterminationbyabsorbancemeasurementat271nm.Themethodwaslinearintherangeof240-640ng/bandfortelmisartanand200-700ng/bandforhydrochlorothi-azide.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104120 MiroslawaKRAUZE-BARANOWSKA*,I.MALINOWSKA,D.GLOD,M.MAJDAN,A.WIL-CZANSKA (*Department of Pharmacognosy, Medical University of Gdansk, Gen. J. Hallera107, 80-416, Poland, [email protected]): UTLC of flavonols in Sambucus nigra flowers. J.PlanarChromatogr.22,�85-�87(2009).Ultrathin-layerchromatographyofquercetin,rutin,andquercetin-�-O-glucosideonmonolithicsilicagel(size�0mmx18mm)withbinaryandtertiarymobilephasesinacylindricalglasschamberpreviouslysaturatedfor1min.Themigrationdis-tancewas20mmanddevelopmenttimewas2min.Theinvestigatedmobilephaseswereethyl

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CAMAGBIBLIOGRAPHYSERVICE No.10428

acetate-n-hexane1:4and�:7,tetrahydrofurane-hexane2:�and�:2,tetrahydrofurane-metha-nol-hexane�:�:4,andhexane-acetone-methylethylketone�:�:4.Thebestseparationwasachievedwithacetone-methylethylketone-hexane�:4:�.Densitometricevaluationat�66nm.

herbal,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2e

104121 M.KRISHNA*,V.MURAGAN,P.MUSMADE,S.VENKATARAM(*DayanandaSagarCol-legeofPharmacy,Bangalore,Karnataka,India):Stabilityindicatinghigh-performancethin-layerchromatographymethodfordeterminationoftriamcinaloneacetonideinbulkdrugandpharma-ceuticaldosageforms.60thIndianPharmaceuticalCongressPA-211(2008).HPTLCoftriam-cinaloneacetonideonsilicagelaluminumfoilwithtoluene-ethylacetate-ammonia��:67:1%.ThehRFvalueoftriamcinaloneacetonidewas�8.Quantitativedeterminationbyabsorbancemeasurementat240nm.Themethodwaslinearintherangeof100-2000ng/spot;recoverywas99.5%.Thestabilityindicatingmethodhasbeensuccessfullyappliedtoforceddegradationstu-diesoftriamcinaloneacetonide(acid,alkali,hydrogenperoxide,photodegradationthermalandneut-ralhydrolysis)andresolveddegradationproductsandexcipientsfromtriamcinaloneacetonide.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104122 M.KUMAR*,B.SRINIVASAN(*DelhiInstituteofPharmaceuticalSciencesandResearch(DI-PASR), New Delhi, India): Stability indicatingHPTLCmethod for the determinationof cini-tapridehydrogentartrateinbulkdrugandpharmaceuticalformulations.AbstractNo.F-240,61stIPC(2009).HPTLCofcinitapridehydrogentartrateonsilicagelwithmethanol-toluene17:�.ThehRFvaluewas71.Quantitativedeterminationbyabsorbancemeasurementat265nm.Thelinearitywas in the rangeof90-450ng/band.Thecompoundwassubjected todifferent stressconditions(acid,alkali,oxidative,photodegradation,dryandwetheat)anddegradationproductswerewellseparatedfromthemaincomponent.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

10412� R.KUNDU*,S.DHOLE,M.CHARDE,A.KASTURE(*J.L.ChaturvediCollegeofPharmacy,Nagpur,Maharashtra,India):High-performancethin-layerchromatographicmethodforsimulta-neousestimationofbenzhexolhydrochlorideandtrifluperazinehydrochlorideinpharmaceuticalpreparations.AbstractNo.F-24861stIPC(2009).HPTLCofbenzhexolHClandtrifluperazineHClonsilicagelwithmethanol-acetone-toluene-25%ammonia10:10:70:1.ThehRFvaluewas�7and82fortrifluperazineandbenzhexolrespectively.Quantitativedeterminationbyabsor-bancemeasurementat210nm.Themethodwaslinearintherangeof40-800ng/bandforbenz-hexoland100-2000ng/bandfortrifluperazine.Recoverywas99.7-99.9%forbothcompounds.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104124 N. LADKAT*, M.ANRUTKAR, J. JAGADE,A. KALE, S. PAWAR,A. BHOSALE (*PoonaDist.EducationAsso.SethGovindRaghunathSableCollegeofPharmacy,Pune,Maharashtra,India):HPTLCestimationofcefiximeandcloxacillinintabletdosageform.AbstractNo.F-260,61st IPC (2009). HPTLCof cefixime and cloxacillin on silicagel, prewashedwithmethanol,withn-butanol-methanol-water-formicacid80:60:40:�.ThehRFvalueswere28and45forcefixime and cloxacillin, respectively. Quantitative determination by absorbance measurementat29�nmforcefiximeand�4�nmforcloxacillin.Thelinearityrangewas150-600ng/bandforbothcompounds.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

104125 Q.LI(LiQongya)*,J.WANG(WangJiaxin),Z.MA(MaZuo),SH.CHEN(ChenShuhe),Y.LIU(LiuYanwen),(*JointStateKeyLabofMinist.Educ.ofHubeiCollTCM&HeadOff.ofTCMCompound,Wuhan,Hubei4�0061,China):(QualitativeandquantitativestudyofAlternantheraphiloxeroides(Mart.)Griseb)(Chinese).ChineseJ.Pharm.Anal.28(5),7�2-7�4(2008).TLCofAlternantheraphiloxeroidesextractsonsilicagelwithchloroform-methanol40:1.ThemethodissuitableforthequalitycontroloftheTCMdruganditsformulations.

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CAMAGBIBLIOGRAPHYSERVICE No.10429

qualitycontrol,pharmaceuticalresearch,traditionalmedicine,herbal,densitometry,quantitativeanalysis,qualitativeidentification �2e

104126 H.LI*(LiHui),J.HU(HuJiangyu),H.OUYANG(OuyangHui),Y.LI(LiYanan),H.SHI(ShiHui), C. MA (Ma Chengjin),Y. ZHANG (ZhangYongkang) (*Jishou University, Hunan Pro-vincKeyLaboratoryofForestProductsandChemicalIndustryEngineering,HunanZhangjiajie,427000,People‘sRebublicofChina,andJishouUniversity,CollegeofChemistryandChemicalEngineering,HunanJishou416000,People‘sRepublicofChina; lihuijsdx@16�.com):Extrac-tion of aucubin from seeds of Eucomma ulmoides Oliv. using supercritical carbon dioxide. J.AOACInt.92,10�-110(2009).AnalyticalandpreparativeTLCofaucubinandherbalextractsafterextractonwithsupercriticalcarbondioxideonsilicagelwithmethanol-chloroform-petro-leumether-ethylacetate1:�:�:1.Visualizationbysprayingwith�0%sulfuricacid.

herbal,traditionalmedicine,pharmaceuticalresearch,qualitycontrol,qualitativeidentification,preparativeTLC �2e

104127 M.LIU(LiuMing)*,G.LI(LiGengsheng),H.WANG(WangHuisheng)(*HenanProvin.Acad.ChineseTrad.Med.&Pharm.,Zhengzhou,Henan450004,China):(StudyofthequalitystandardofRehmanniaglutinosa(Gdertn)Iibosch,aChinesetraditionalherbaldrug)(Chinese).ChineseJ.Phram.Anal.27(9),1�11-1�1�(2007).TLCofdrugextractsonsilicagelwithtrichlorometha-ne-methanol-water12:8:1.Detectionbysprayingwith5%vanillin-sulfuricacidreagentandevaluationindaylightandunderUVlight.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,herbal,quantitativeanalysis,qualitativeidentification �2c

104128 H.LU(LuHui)*,H.XIE(XieHongping),SH.YANG(YangShilin),B.GU(GuBing)(*Pharm.Coll.,SuzhouUniv.,Suzhou,Jiangsu21512�,China):(IdentificationofleafofVitexnegundoL.var.cannabifolia(Sieb.etZucc.)Hand.-Mazz.andOleumViticisNegundobythin-layerchro-matography)(Chinese).J.ChineseTrad.Med.&Pharm.(ShizhenGuoyiGuoyao)20(11),2799-2800(2009).TLCofTCMdrugextractsonsilicagelwithpetroleumether(60-90ºC)-ethylace-tate100:�.Detectionbysprayingwithasolutionof5%vanillin-10%sulfuricacidinethanol1:10followedbyheatingat105°Cuntilcoloration,evaluationinvisibleandUVlight.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,herbal,qualitativeidentification,quantitativeanalysis �2e

104129 K. LUNIYA*, R. MANTRI, S. DUBEY, S. BHARANI (*A.I.S.S.M.S. College of Pharmacy,PuneMaharashtra,India):Validatedmethoddevelopmentforestimationofnaproxensodiumasbulkdrugand in tabletdosage formbyHPTLC.AbstractNo.F-28�,61st (2009).HPTLCofnaproxensodiumonsilicagelwithtoluene-ethylacetate-aceticacid15:�:2.ThehRFvaluewas6�.Quantitativedeterminationbyabsorbancemeasurementat2�0nm.Themethodwaslinearintherangeof100-500ng/band.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

1041�0 ROSIDAH,M.YAM*,A.SADIKUN,M.AHMAD,G.AKYIREM,M.ZAINI(*DepartmentofHumanAnatomy,FacultyofMedicineandHealthSciences,UniversityPutraMalaysia,Serdang4�400, Selangor, Malaysia, [email protected]) :Toxicology evaluation of standardizedmethanolextractofGynuraprocumbens.J.Ethnopharmacol.12�,244-249(2009).HPTLCofkaempferol-�-O-rutinosideandastragalininleavesofGynuraprocumbensonsilicagelwithace-ticacid-methanol-dichloromethane1:�:7.Quantitativedeterminationbyabsorbancemeasure-mentat�66nm.ThehRFvaluesofkaempferol-�-O-rutinosideandastragalinwere4�and72,respectively, and selectivity regarding matrix was given. Linearity was given between 16 and1000µg/mLandthecorrelationcoefficientswere>0.987.

toxicology,herbal,HPTLC,quantitativeanalysis,densitometry �2e

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CAMAGBIBLIOGRAPHYSERVICE No.104�0

1041�1 A.MADAN*,B.PATEL(*K.B.InstituteofPharmaceuticalEducationandResearchGandhina-gar,Gujarat,India):HPTLCmethodforsimultaneousdeterminationofrabeprazoleanditoprideincapsulesanditsvalidation.AbstractNo.F-244,61stIPC(2009).HPTLCofrabeprazoleanditoprideonsilicagelwithethylacetate-methanol-benzene-chloroform2:4:�:1.ThehRFvaluewas42and61for rabeprazoleand itopride, respectively.Quantitativedeterminationbyabsor-bancemeasurementat276nm.Themethodwaslinearintherangeof200-�00ng/bandforrabe-prazoleand1500-2250ng/bandforitopride.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

1041�2 V. MADHAVAN*, S. YOGANARSIMHAN, R. TIJARE (*M. S. Ramaiah College ofPharmacy,Bangalore,India):PharmacognosticalandphytochemicalstudiesofrootstubersofAs-paragusgonocladosBaker.AbstractNo.9966,IHCB(2009).HPTLCofroot tuberextractsofAsparagusgonocladosBakeronsilicagelwithethylacetate-methanol-water15:�:2.Detectionbysprayingwithanisaldehydereagent.Quantitativedeterminationbyabsorbancemeasurementat425nm.ShatavarinIVwasusedasmarker.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis,postchromatographicderivatization �2e

1041�� U.MALLAVADHANI*,G.SAHU(*HerbalDrugsandBio-Remedies,InstituteofMineralsandMaterialTechnology (CSIR), Bhubaneswar-751 01�, Orissa, India; [email protected]):A rapidHPTLC method for standardizationofFicusbengalensisLinn. J. PlanarChromatogr.22,�77-�80(2009).HPTLCofstigmast-5-en-�beta-O-D-glucosideandbarkextractsonsilicagelwithchloroform-methanol-water��:7:4inasaturatedtwintroughchamber.Detectionbyderivatizationwithanisaldehydereagentfollowedbyheatingat105°Cfor5min.Quantitativedeterminationbyabsorbancemeasurementat515nm.

herbal,traditionalmedicine,qualitycontrol,HPTLC,quantitativeanalysis,densitometry �2e

1041�5 K.MANGUKIA*,T.VAJA,HasumatiRAJ,SadhanaRAJPUT(*N.R.VekariaInstituteofPhar-macy&ResearchCentreJunagadh,Gujarat,India):Developmentandvalidationofstability-indi-catingHPLCandHPTLCmethodsforanalysisofezetimibeinpureformandinpharmaceuticalformulation.AbstractNo.F-�20,62stIPC(2009).HPTLCofezetimibeonsilicagelwithethylacetate-toluene-methanol-formicacid10:10:1:1.Quantitativedeterminationbyabsorbancemeasurementat2�1nm.Themethodwaslinearintherangeof�01-�610ng/band.Recoverywas99.�-100.4%Thedrugwasexposedtodifferentstressconditions(acid,base,oxidative,thermal)andalldegradationproductswerewellresolvedfromthemaincompound.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,comparisonofmethods,quantitativeanalysis �2a

1041�6 T.MANI*,S.BADAMI,N.MAHADEVAN,S.MANIMARAN,B.SURESH(*BharathiCol-legeofPharmacy,BharathiNagara,Karnataka,India):DeterminationofharmalininPassifloraedulisleavesbyHPTLC.AbstractNo.9274,IHCB(2009).HPTLCofharmalinfromethanolicleafextractsofPassifloraedulisonsilicagelwithethylacetate-aceticacid-formicacid-water100:11:11:27.ThehRFvalueofharmalinwas�9.Themethodwaslinear in therangeof200-1600ng/spot,recoverywas98.4-99.2%.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,HPTLC,quantitativeanalysis �2e

1041�7 S.MANIMARAN*,M.CHAITANYA,T.PRAVEEN,S.DHANABAL(*JSSCollegeofPhar-macy,Ootacamund,TamilNadu,India):MethodvalidationandestimationofisovitexincontentinPassifloraincarnataLinnbyHPTLCtechnique.60thIndianPharmaceuticalCongressPG-258(2008).HPTLCofisovitexininPassifloraincarnatarawmaterialandextractonsilicagelwithethylacetate-formicacid-glacialaceticacid-water100:11:11:26.Theplantwasfoundtocon-tain0.087%w/wofisovitexin.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

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CAMAGBIBLIOGRAPHYSERVICE No.104�1

1041�8 R.MANTRI*,M.SENGAR,U.PATIL,S.GANDHI(*A.I.S.S.M.S.CollegeofPharmacy,Pune,Maharashtra,India):High-performancethin-layerchromatographicdeterminationofdiclofenacsodiumand thiocolchicoside infixeddosecombination.AbstractNo.F-284,61st IPC(2009).HPTLCofdiclofenacsodiumandthiocolchicosideonsilicagelwithtoluene-ethylacetate-me-thanol5:�:2.ThehRFvaluewas17and5�forthiocolchicosideanddiclofenacsodium,respec-tively.Quantitativedeterminationbyabsorbancemeasurementat285nm.Themethodwaslinearintherangeof50-�00ng/bandforbothdrugs.Recoverywas100.5-101.1%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

1041�9 A.MASLANKA. J.KRZEK*,M.STOLARCZYK(*Departmentof InorganicandAnalyticalChemistry, Jagiellonian University, Collegium Medicum, 9 Medyczna Street, �0-688 Cracow,Poland,[email protected]):Simultaneousanalysisofhydrochlorothiazide,triamterene,furosemide,andspironolactonebydensitometricTLC.J.PlanarChromatogr.22,405-410(2009).TLCofhydrochlorothiazide,triamterene,furosemide,andspironolactoneonsilicagelwithhe-xane-ethylacetate-methanol-water-aceticacid42:40:15:2:1withchambersaturation.Quan-titativedeterminationbyabsorbancemeasurementat264nm.Thelimitofdetectionforthediffe-rentcompoundswasbetween22and150ng/band,andthelimitofquantificationwasbetween68and450ng/band.

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis �2a

104140 AnnieMATHEW*,R.RAVINDRA(*C.U.ShahCollegeofPharmacy,S.N.D.T.Women‘sUni-versity,JuhuRoad,Santacruz(W)Mumbai,India):QuantitativeHPTLCanalysisofdiallydisul-fideingarlicoilmacerate.AbstractNo.9286,IHCB(2009).HPTLCofdiallydisulfideingarlicoilmacerateonsilicagelwithn-hexane-isopropylalcohol-formicacid196:4:�.Quantitativedeterminationbyabsorbancemeasurementat210nm.Themethodwaslinearintherangeof16-48µg/spot.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104141 S.MATHUR*,D.SHARMA,P.SAINI,R.SINGH(*R&DDiv.,IndianPharmacopoeiaCom-mission,MinistryofHealth&FamilyWelfare,Govt.ofIndia,Ghaziabad,U.P.,India):Simulta-neousestimationofdomperidoneandparacetamolinbulkanditstabletsdosageformsbyHPT-LCmethod.AbstractNo.F-�95,61stIPC(2009).HPTLCofdomperidoneandparacetamolonsilicagelwithacetone-toluene-methanol2:2:1withchambersaturationatroomtemperature.ThehRFvaluewas52and74fordomperidoneandparacetamol,respectively.Quantitativedeter-minationbyabsorbancemeasurementat248nm(paracetamol)and285nm(domperidone).Themethodwaslinearintherangeof16-48ng/band.Recoverywas99.5-101.2%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104142 DipaliMEHETRE*,A.CHABUKSWAR,B.KUCHEKAR,A.KATEGAONKAR(*MAEER‘sMaharashtraInstituteofPharmacy,Pune,Maharashtra,India):ValidationofHPTLCmethodforsimultaneousquantitationofolmesartanmedoximalandamlodipinebesylate inbulkdrugandformulation.AbstractNo.F-258,61stIPC(2009).HPTLCofolmesartanmedoximalandamlodi-pinebesylateonsilicagelwithchloroform-methanol-toluene-aceticacid80:10:1:1.Quantita-tivedeterminationbyabsorbancemeasurementat254nm.Thelinearityrangewas800-5000ng/bandforolmesartanand200-1400ng/bandforamlodipine.Recoverywasintherangeof98-102%forbothdrugs.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

10414� A.MISHRA*,R.BHOMIA,S.VASANTHARAJU,A.KARTHIK,S.SAYED,K.BHAT(*L.M.CollegeofPharmacy,Ahmedabad,Gujarat, India):Simultaneous estimationof salbutamolsilphateandguaiphenesinintheircombinedliquiddosageformbyHPTLCmethod.AbstractNo.F-2�8,61stIPC(2009).HPTLCofsalbutamolsilphateandguaiphenesin,usedaspharmaceutical

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CAMAGBIBLIOGRAPHYSERVICE No.104�2

syrupagainstcough,onsilicagelwithethylacetate-methanol-25%ammonia15:�:2.ThehRFvaluewas47and65forsalbutamolandguaiphenesin,respectively.Quantitativedeterminationbyabsorbancemeasurementat280nm.Themethodwaslinearintherangeof200-1000ng/bandforsalbutamoland10-15µg/bandforguaiphenesin.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104144 A.MISHRA*,R.BHOMIA,S.VASANTHARAJU,A.KARTHIK,S.SYED,K.BHAT(*Mani-palCollegeofPharmaceuticalSciences,ManipalUniveristy,Manipal,Karnataka,India):Stabili-ty-indicatingHPTLCmethodfortheestimationoftolterodineinbulkdrug.AbstractNo.F-2�7,61stIPC(2009).HPTLCoftolterodineonsilicagelwithtoluene-methanol-25%ammonia250:250:1.ThehRFvaluewas40.Quantitativedeterminationbyabsorbancemeasurementat284nm.Themethodwaslinearintherangeof200-1000ng/band.Thecompoundwassubjectedtodifferentstressconditions(acid,alkali,oxidation,thermal)anddegradationunderalkalinecondi-tionswasobserved.Thedegradationproductswerewellseparatedfromthemaincomponent.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

104145 S.MISHRA*,SunitaCHAUDHARY,K.GADHVI(*SaraswatiInstituteofPharmaceuticalSci-ences,Ahmedabad,Gujarat,India):EstimationofglycyrrhizicacidandwithanolideAinpoly-herbal formulationbyHPTLC.60th IndianPharmaceuticalCongressPA-2�� (2008).HPTLCofglycyrrhizicacidonsilicagelwithtoluene-ethylacetate-glacialaceticacid25:15:1.ThehRFvalueofglycyrrhizicacidwas52,linearitywasintherangeof500-1000ng/mLandreco-verywas99.2%.WithanolideAwasseparatedwithtoluene-ethylacetate-glacialaceticacid20:20.1.ThehRFvalueofwithanolideAwas44,linearitywasintherangeof400-1000ng/mLandrecoverywas99.4%.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104146 K.MODT*,N.PATEL,R.GOYAL(*Dept.ofPharmacology,ShriB.M.ShahCollegeofPhar-maceuticalEducation&Research,Modasa,Gujarat,India):AsensitiveHPTLCmethodfortheestimationofL-dopa fromMuccunapruriensLinnanda formulationcontainingM.pruriens.AbstractNo.9425,IHCB(2009).HPTLCofL-dopainMucunapruriensseedextractandfor-mulationsonsilicagelwithn-butanol-aceticacid-water4:1:1.Quantitativedeterminationbyabsorbancemeasurementat280nm.Themethodwas linear in the rangeof100-1200ng/spotwithanaveragerecoveryof100.�%.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,HPTLC,quantitativeanalysis �2e

104147 P. MUCAJI*, M. NAGY,T. LIPTAJ, N. PRÓNAYOVÁ, E. SVAJDLENKA (*Department ofPharmacognosy and Botany, Faculty of Pharmacy, Comenius University, Odbojárov 10, 8�2�2 Bratislava, Slovak Republic, [email protected]): Separation of a mixture of luteo-lin-7-rutinoside and luteolin-7-neohesperidoside isolated from Ligustrum vulgare L. J. PlanarChromatogr. 22, �01-�04 (2009).Analytical and preparativeTLC of luteolin-7-rutinoside andluteolin-7-neohesperidosideon silicagelwithethyl acetate - formicacid - acetic acid -water100:11:11:2�,oncellulosewith�0%aceticacid,andonpolyamidewithchloroform-methanol-2-butanone - acetyl acetone (=pentane-2,4-dione)9:4:�:1.Detectionby sprayingwithnaturalproductsreagentfollowedbytreatmentwithPEG4000,orbyanilinephthalate.

herbal,qualitycontrol,traditionalmedicine,preparativeTLC,qualitativeidentification �2e

104148 A.MUJTABA*,S.BABOOTA,J.ALI,K.KOHLI(*Dept.ofPharmaceutics,FacultyofPhar-macy, Hamdard University, New Delhi, India): Development and validation of novel HPTLCmethodforquantitativeestimationofondansetronHClinbulkandpharmaceuticaldosageform.AbstractNo.F-274,61stIPC(2009).HPTLCofondansetronHClonsilicagelwithchloroform-ethylacetate-methanol -25%ammonia90:50:40:1.ThehRFvaluewas52.Quantitativede-

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CAMAGBIBLIOGRAPHYSERVICE No.104��

terminationbyabsorbancemeasurementat254nm.Themethodwaslinearintherangeof100-1400ng/band.Recoverywas99.�%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104149 B.NARWATE*,P.GHULE,P.MOHITE,R.UGALE(*Dept.ofPharmaceuticalChem.,MESCollege of Pharma., Sonai,Tal.-Newasa, Dist.-Ahmednagar 414105 (M.S.) India., [email protected]):Ahigh-performancethin-layerchromatographicdeterminationofclopi-dogrelbisulphate in tablets. Ind.J.Pharma.Sci.8(4),211-212(2009).TLCofclopidogrelbi-sulphateonsilicagelwithcarbon tetrachloride -ethylacetate -ammonia50:�:2.Quantitativedeterminationbyabsorbancemeasurementat2�0nm.Linearitywasbetween�00and1500ng.Incomparisonwiththelabeledclaimtheamountofclopidogrelintabletswas99.2%.Thereco-verywas99.2%(viapeakarea).

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis �2a

104150 J.NIRMAL*,S.MAHESHWARI,H.RAJ,S.RAJPUT(*N.R.VekariaInstituteofPharmacy&ResearchCentre,Junagadh,Gujarat,India):Developmentandvalidationofstability-indicatingHPLCandHPTLCmethodsforanalysisofpravastatininpureformandapplicationoftheme-thodsforestimationofpharmaceuticalformulation.AbstractNo.F-�15,61stIPC(2009).HPT-LCforpravastatinonsilicagelwithethylacetate-toluene-acetonitrile-formicacid60:�5:5:2.Quantitativedeterminationbyabsorbancemeasurementat2�7nm.Themethodwaslinearintherangeof�18-�816ng/band.Recoverywas99.9-101.2%.Stabilitytestsshowedthatdegradationproductsresultingunderacidstressconditionswerewellresolvedfromthemaincomponent.

qualitycontrol,HPTLC,densitometry,comparisonofmethods,quantitativeanalysis �2a

104151 K.NISHAMOL*,A.BINDU,N.ALEYKUTTY,S.JOSE(*M.G.Univeristy,Dept.ofPharma-ceuticalSciences,Ettumanoor, Kottayam,Kerala, India):Development of a high-performancethin-layerchromatographymethodforthequantitativeestimationofrutininthefreshleavesofMoringapterygospermaGaertn.60thIndianPharmaceuticalCongressPG-26�(2008).HPTLCofrutininmethanolicextractsoffreshleavesofMoringapterygospermaonsilicagelwithethylacetate - formicacid -glacialaceticacid -water100:11:11:26.Quantitativedeterminationbyabsorbancemeasurementat254nm.Themethodprovidedgoodresolutionofrutinfromotherconstituentsoftheplant.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104152 D.N.OLENNIKOV(LaboratoryofMedicalandBiologicalResearch,DepartmentofBiologicallyActiveSubstances,InstituteofGeneralandExperimentalBiology,SiberianDivision,RussianAca-demyofSciences,Sakh‘yanovoySt6,670047,Ulan-Ude,Russia;[email protected]):Densi-tometricHPTLCanalysisofaloenininaloepharmaceuticals.J.PlanarChromatogr.22,�59-�62(2009).HPTLCofaloenininaloejuice,tablets,andliquidextractsonsilicagelwithethylacetate-95%ethanol-water20:�:1atroomtemperatureinasaturatedchamber.Detectionbyimmersionfor1sinfreshlyprepared5%sodiumhydroxidesolutionin95%ethanol,followedbyheatingat100°Cfor5min.Quantitativedeterminationbyabsorbancemeasurementat�65nm.

herbal,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

10415� A.OSMAN*,M.OSMAN(*NationalOrganizationforDrugControlandResearch,6AbuHa-zemStPyramids,POBox29,Cairo,Egypt;[email protected]):Specrofluorometry,thin-layerchromatography,andcolumnhigh-performanceliquidchromatographydeterminationofrabeprazolesodiuminthepresenceofitsacidicandoxidizeddegradationproducts.J.AOACInt.92,1�7�-1�81(2009).TLCofrabeprazolesodiumanditsdegradationproductsonsilicagelwithisopropanol-�0%ammonia40:1withchambersaturation.Quantitativedeterminationbyabsorbancemeasurementat284nm.

pharmaceuticalresearch,qualitycontrol,quantitativeanalysis,densitometry �2a

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CAMAGBIBLIOGRAPHYSERVICE No.104�4

104154 M.PAI*,RajashreeGUDE,SwatiKENY(*GoaCollegeofPharmacy,Panaji,Goa,India):De-velopmentandvalidationofanewsensitivemethod for thequantitativeanalysisof ranitidinehydrochlorideanddomperidoneinantiulcercombinationbyusingHPTLC.60thIndianPharma-ceuticalCongressPA-215(2008).HPTLCofranitidineHClanddomperidoneincombineddosageformonsilicagelwithethylacetate-methanol-ammonia100:10:1inatwintroughchambersa-turatedfor10min.Quantitativedeterminationbyabsorbancemeasurementat285nm.Themethodwaslinearintherangeof100-500ng/µLforbothcompoundswitharecoveryof102.5-100.8%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,comparisonofmethods,quantitativeanalysis �2a

104155 H.J. PANCHAL*, B.N. SUHAGIA, N.J. PATEL (*Patel College of Pharmaceutical EducationandResearch,GanpatVidyanagar,Kherva,Mehsana�82711,Gujarat,India;[email protected]):SimultaneousHPTLCanalysisofatorvastatincalcium,ramipril,andaspirininacapsuledosageform.J.PlanarChromatogr.22,265-271(2009).HPTLCofatorvastatincal-cium,ramipril,andaspirinandextractsofpharmaceuticalformulationsonsilicagel,prewashedwith methanol, with methanol - benzene - ethyl acetate - glacial acetic acid 9:140:100:1 in atwintroughchamber,saturatedwithmobilephasefor�0minatroomtemperature.Quantitativedeterminationbyabsorbancemeasurementat210nm.Thelimitofdetectionwas5ng/zoneforatorvastatincalcium,�ng/zoneforramipril,and19ng/zoneforaspirin.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104156 M.PANDE*,ShwetaGONDKAR,J.RAO,S.YADAV(*PoonaCollegeofPharmacy,BharatiVidyapeethUniversity,Pune,Maharashtra,India):SimultaneousdeterminationoftenofovirandemtricitabineinthebulkdrugandtabletdosageformbyHPTLCmethod.AbstractNo.F-25�,61stIPC(2009).HPTLCoftenofovirandemtricitabineonsilicagelwithtoluene-methanol-ethylacetate-aceticacid40:20:50:1.Quantitativedeterminationbyabsorbancemeasurementat27�nm.ThehRFvaluewas52fortenofovirand40foremtricitabine.Linearityoftenofovirandemtricitabinewasintherangeof120-600ng/spotand80-560ng/spot,respectively.Therecoverywas99.9and99.5%fortenofovirandemtricitabine,respectively.

qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104157 P.PARMAR*,AnkitaMEHTA(L.M.CollegeofPharmacy,Navrangpura,Gujarat�80009,In-dia,parul1�8�@gmail.com):DevelopmentandvalidationofHPTLCmethodfortheestimationofclotrimazoleinbulkdrugandtabletformulation.Ind.J.Pharma.Sci.71(4),451-454(2009).HPTLCofclotrimazoleinbulkdrugandtabletdosageformonsilicagelwithcyclohexane-to-luene-methanol-triethylamine80:20:5:2.Quantitativedeterminationbyabsorbancemeasure-mentat262nm.Thecalibrationcurvewaslinearbetween200to1000ng/spotforclotrimazole.Thelimitofdetectionandlimitofquantificationforclotrimazolewere50ng/spotand200ng/spot,respectively.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

104160 A.PATEL*,B.DHANYA,A.SEN,A.SETH(*Dept.ofPharma.,SumandeepVidyapeethUni-versity,Vadodara,Gujarat,India):DevelopmentandvalidationofaHPTLCmethodforestimati-onofdoxazosinmesylateintabletdosageform.AbstractNo.F-251,61stIPC(2009).HPTLCofdoxazosinmesylateonsilicagelwithacetone-toluene-25%ammonia60:40:1.ThehRFvaluewas65.Quantitativedeterminationbyabsorbancemeasurementat251nm.Linearitywasintherangeof20-100ng/band.Recoverywas10�.�%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104159 B.PATEL*,A.MODH,P.MEHTA,H.BHATT(*InstituteofPharmacy,NirmaUniversitySci-enceandTechnology,Ahmedabad,Gujarat, India):Developmentandvalidationofspectropho-tometricandHPTLCmethodforsimultaneousestimationoflevocetirizinedihydrochlorideand

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CAMAGBIBLIOGRAPHYSERVICE No.104�5

montelukastsodiumintheircombineddosageform.AbstractNo.F-�11,61stIPC(2009).HPTLCoflevocetirizinedihydrochlorideandmontelukastsodiumonsilicagelwithchloroform-metha-nol9�:7.ThehRFvaluewas21and65forlevocetrizineandmontelukast,respectively.Quantita-tivedeterminationbyabsorbancemeasurementat�45nm.Themethodwaslinearintherangeof100-�50ng/bandforlevocetrizineand600-1100ng/bandformontelukast.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,comparisonofmethods,quantitativeanalysis �2a

104161 C. PATEL*, B. PATEL, P. PATEL, C. PATEL (*Shri Sarvajanik Pharmacy College, Hem-chandracharyaNorthGujaratUniversity,Mehsana,Gujarat,India):Developmentandvalidationof a simultaneous HPTLC method for the estimation of atorvastatin calcium and amlodipinebesilateintabletdosageform.60thIndianPharmaceuticalCongressPA-21�(2008).HPTLCofatorvastatincalciumandamlodipinebesilateonsilicagelwithchloroform-toluene-methanol-water55:10:20:2.Quantitativedeterminationbyabsorbancemeasurementat242nm.Thecalib-rationcurvewasfoundtobelinearbetween400and1200ng/spotforbothatorvastatincalciumandamlodipinebesilate.Thelimitofdetectionandthelimitofquantificationforatorvastatincal-ciumwere100and400ng/spot,andforamlodipinebesilate200and400ng/spot,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

10417� D.PATEL*,S.HEMALATHA,SURESHB.,S.DHANABAL(*Dept.ofPharmacognosy.J.S.S.CollegeofPharmacy,Oacamund64�001,TamilNadu,India):PhytochemicalstandardizationandfingerprintinganalysisofBerberisaristataextractbyHPTLC.AbstractNo.9185,IHCB(2009).HPTLCofhydroalcoholicextractsofBerberisaristataonsilicagelwithbenzene-ethylacetate-diethylamine6:�:1.DetectionbysprayingwithAlCl�reagent(forestimationofflavonoids)orwithFolinCiocalteureagent(fortotalphenoliccontent).Thefingerprintprofilewasoptimizedusingtwodifferentmobilephases:n-butanol-aceticacid-water14:1:5andn-propanol-formicacid-water90:1:9.Theextractshowed6differentspotsandwasfoundtocontain1�.5%w/wofberberin.

pharmaceuticalresearch,qualitycontrol,herbal,densitometry,HPTLC,quantitativeanalysis,postchromatographicderivatization �2e

104162 D.PATEL*,B.SHAH,B.PATEL(*K.B.InstituteofPharmaceuticalEducationandResearchGandhinagar,Gujarat,India):Simultaneousestimationofatorvastatincalcium,ramiprilandas-pirinincapsuledosageformbyHPTLC.AbstractNo.F-245,61stIPC(2009).HPTLCofator-vastatin (AT)calcium, ramipril (RA)andaspirin (AS)on silicagelwithbenzene - ethyl ace-tate - toluene -methanol -aceticacid40:45:10:5:1.Quantitativedeterminationbyabsorbancemeasurementat220nm.ThehRFvalueswere45,28and72forAT,RAandAS,respectively.Thelinearityrangeswere0.5-2.5µg/band(r2=0.998)forAT,0.5-2.5µg/band(r2=0.9978)forRAand0.75-�.75µg/band(r2=0.9946)forASwithmeanrecoveriesof100.�,99.1and98.9forAT,RAandAS,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104164 F.PATEL*,J.DONGA,N.PATEL,V.GANDHI(*DharmajDegreePharmacyCollege,Dhar-maj, Gujarat, India): Determination of camylofin dihydrochloride in bulk and tablet by liquidchromatographyandHPTLC.AbstractNo.F-267,61stIPC(2009).HPTLCofcamylofindihy-drochlorideonsilicagelwithchloroform-ethylacetate-methanol-25%ammonia50:�0:20:1.Quantitativedeterminationbyabsorbancemeasurementat215nm.Linearitywasintherangeof1500-7500ng/band.Theproposedmethodissuitableforroutinequalitycontrolofbulkdrugandtablets.

pharmaceuticalresearch,HPTLC,densitometry,quantitativeanalysis �2a

104165 J.PATEL*,K.BHAT,F.SHAIKH,S.PANDYA(*BabariaInstituteofPharmacy,Varnama,Vado-dara,Gujarat,India):Simultaneousdeterminationofstrychnineandpiperineintheircombined

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CAMAGBIBLIOGRAPHYSERVICE No.104�6

herbaldosageformbyHPTLC.60thIndianPharmaceuticalCongressPA-192(2008).HPTLCof strychnineandpiperine inherbalextractsandherbal formulationsonsilicagelwith tolue-ne-ethylacetate-diethylamine7:2:1.Quantitativedeterminationbyabsorbancemeasurementat28�nm.Linearitywas400-2000ng/spot, recoverywas in the rangeof99.5-101.0both forstrychnineandpiperine.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104158 J.B. PATEL, S.K. LAHIRI, M.B. SHAH* (*Department of Pharmacognosy, L. M. College ofPharmacy,Navarangpura,Ahmedabad(Gujarat),�80009,India;mbshah2007@rediffmaol-com):DevelopmentofanewmethodforidentificationafWithaniasomniferaroot,andamethodforquantitativeanalysisofwithaferinAinyoungandoldroots.J.PlanarChromatogr.22,28�-286(2009).HPTLCofwithaferinandextractsofthepowderedrootonsilicagel,prewashedwithme-thanol,withtoluene-ethylacetate-acetone2:�:�inatwintroughchambersaturatedwithmo-bilephasefor�0min.Detectionbysprayingwithanisaldehydereagentfollowedbyheatingfor15minat105°C;characteristicorangefluorescencewasobservedforwhithaferin.Quantitativedeterminationbyabsorbancemeasurementat214nm.ThelimitofdetectionandquantificationforwithaferinAwas258and782ng/zone,respectively.

traditionalmedicine,herbal,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104170 M.PATEL*,P.MANDLEKAR,S.MULGUND,K.JAIN(*SinhgadCollegeofPharmacy,Pune,Maharashtra, India): Simultaneous HPTLC determination of ramipril hydrochlorothiazide andtelmisartanincombinedtablets.AbstractNo.F-2�9,61stIPC(2009).HPTLCofhydrochlorothi-azide, ramipril and telmisartanon silicagelwithethyl acetate - chloroform -methanol6:�:1.Quantitativedeterminationbyabsorbancemeasurementat215nm.Themethodwassuitableforroutinequalitycontrolofcombinedformulations.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

10416� N.PATEL*,G.PATEL,H.BHATT,C.SHASTRY(*ShreeDhanvantryPharmacyCollege,Surat,Gujarat, India):HPTLCmethod for simulteneousdeterminationof aspirin and atorvastatin inpharmaceuticalformulation.AbstractNo.F-29�,IPC(2009).HPTLCofaspirinandatorvastatinonsilicagelwithn-hexane-acetone-butylacetate-formicacid60:�0:12.Quantitativedetermi-nationbyabsorbancemeasurementat242nm.Forbothdrugs,themethodwaslinearintherangeof�-7µg/bandandtherecoverywasbetween99.�and101.0%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104171 P.PATEL*,R.MASHRU(*Babaria InstituteofPharmacy,Vadodara,Gujarat, India):Twodi-mensionalthinlayerchromatography(2D-TLC)forresolutionofisomersof(±)bupropionHCl.AbstractNo.F-254,61stIPC(2009).HPTLCofbupropionHClonsilicagelwithquininesul-phate-methanol-water1�:20:12in thefirstdirection.Quininesulphatewasusedasachiralselectorataconcentrationof�.5mM.ThetwoseparatedbandsweredetectedunderUV�66nm.ThehRFvaluesofI(-)andd(+)isomersofbupropionHClwere90and84,respectively.Afterthesecondrunintheseconddimensionwithmethanol-water80:1�theywerebetterresolvedwithhRFvaluesof88and76.

HPTLC,qualitativeidentification �2a

104172 P.PATEL*,R.MASHRU,T.PATEL(*BabariaInstituteofPharmacy,Varnama,Vadodara,Gu-jarat,India):DevelopmentandvalidationofadirectHPTLCmethodforseparationofisomersof (±)bupropionHClusingquininesulphateasachiralselector inmobilephase.60thIndianPharmaceuticalCongressPA-216(2008).HPTLCofisomersofbupropionHClonsilicagelwithquininesulphate-methanol-water1�:20:12(quininesulphateservedasachiralselector).Eva-luationunderUV�66nm.Linearitywasintherangeof10-100µg/spotford(+)-andl(-)-isomersofbupropion.Theisomerratiowas80%d(+)-bupropionand20%l(-)-bupropion.

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CAMAGBIBLIOGRAPHYSERVICE No.104�7

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104169 P.PATEL*,N.PATEL,R.GOYAL(*ShriB.M.ShahCollegeofPharmaceuticalEducation&Research,Modasa,Gujarat,India):Qualitycontrolofpolyherbalformulationsusedindiabetesmellitus.60thIndianPharmaceuticalCongressPG-246(2008).HPTLCofbiomarkerssuchascurcumin,charantin,andswertiamarininsomepolyherbalformulationsonsilicagelwithben-zene-methanol4:1(forcharantin),chloroform-methanol-formicacid74:4:1(forcurcumin),andethylacetate-methanol-water77:15:5(forswertiamarin).Quantitativedeterminationbyabsorbancemeasurementat5�6forcharantin(hRFvalue��),425nmforcurcumin(hRFvalue89),and2�8nmforswertiamarin(hRFvalue54).

traditionalmedicine,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104167 R.PATEL*,MrunaliPATEL,K.BHATT,B.PATEL (*A.R.CollegeofPharmacyandG.H.PatelInstituteofPharmacy,VallabhVidyanagar,Gujarat,India):DevelopmentandvalidationofHPTLCmethod: itsapplicationinqualificationofolanzapineinmucoadhesivemicroemulsionformulationsandinvitrostudy.AbstractNo.F-2�5,61stIPC(2009).HPTLCofolanzapineonsilicagelwithmethanol-ethylacetate4:1.ThehRFvaluewas�5.Quantitativedeterminationbyabsorbancemeasurementat285nm.Themethodwaslinearintherangeof100-600ng/band.Themethodwassuitableforanalysisofformulationsandin-housepreparedmucoadhesivemicroe-mulsions.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104166 R.B. PATEL*, M.R. PATEL, M.B. SHANKAR, K.K. BHATT (*Sardar Patel Univrsity,A. R.CollegeofPharmacy&G.H.PatelInstituteofPharmacy,VallabhVidyanagar�88120,Gujarat,India; [email protected]):Simultaneousdeterminationof alprazolamandfluoxetinehydro-chloride in tablet formulationshyhigh-performance column liquid chromatographyandhigh-performancethin-layerchromatography.J.AOACInt.92,1082-1087(2009).HPTLCofalpra-zolamandfluoxetinehydrochlorideinpurepowderandformulationsonsilicagelwithacetone-toluene-ammonia12:7:1inatwintroughchambersaturatedfor�0min.Quantitativedetermina-tionbyabsorbancemeasurementat2�0nm.Therewasnosignificantdifferenceinthedetermi-nedcontentofalprazolamandfluoxetinebyHPTLCandHPLCmethods(assayresultscomparedbyapplyingthepairedt-test).

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis,comparisonofmethods �2a

104168 S.PATEL*,N.PATEL(*ShreeS.K.PatelCollegeofPharmaceuticalEducationandResearch,GanapatUniversity,Mehsana,Gujarat,India):HPTLCestimationofamitriptylineHCl,trifluo-perazineHCl,risperidoneandalprazolaminpharmaceuticalproductsusingsinglemobilephase.60thIndianPhamraceuticalCongressPA-210(2008).HPTLCofamitriptylineHCl,trifluopera-zineHCl,risperidoneandalprazolamonsilicagelwithcarbontetrachloride-acetone-triethyl-amine80:20:�.Quantitativedeterminationbyabsorbancemeasurementat250nmintherangeof50-1200ng/spotforamitriptylineHCl,50-1200ng/spotfortrifluoperazineHCl,100-2400ng/spotforrisperidone,and25-600ng/spotforalprazolam.Thelimitofquantificationforamitripty-lineHClandtrifluoperazinHClwas50ng/spot,forrisperidone100ng/spot,andforalprazolam25ng/spot.

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis,HPTLC �2a

104174 P. PATIDAR *, S. MANIMARAN, N. SONI, S. DHANABAL (*J S S College of Pharmacy,Ooty,TamilNadu,India):SimultaneuosHPTLCestimationofquercetinandrutinfromTylopho-raindicaandTephrosiapurpurea.60thIndianPharmaceuticalCongressPG-261(2008).HPTLCofquercetinandrutininethanolicextractsofaerialpartsofTylophoraindicaandTephrosiapur-pureaonsilicagelwithethylacetate-formicacid-aceticacid-water100:11:11:26.Quantitativedeterminationbyfluorescencemeasurementat�66/>400nm.TheextractofTephrosiapurpurea

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CAMAGBIBLIOGRAPHYSERVICE No.104�8

contained1.56%ofquercetinand1.40%ofrutin,whereasTylophraindicacontained4.�0%ofquercetin.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104175 N.G.PATRE,L.SATHIYANARAYANAN,M.V.MAHADIK,S.R.DHANESHWAR*(*Depart-mentofPharmaceuticalChemistry,BharatiVidyapeethUniversity,PoonaCollegeofPharmacy,Center forAdvanced Pharmaceutical Research, Erandwane, Pune 4110�8, Maharashtra State,India;[email protected]):Avalidated,stability-indicatingHPTLCmethodforana-lysisofdoxofylline.J.PlanarChromatogr.22,245-�48(2009).HPTLCofdoxofylline(7-(1,�-dioxalan-2-ylmethyl)theophylline)inbulkdrugandinformulationsonsilicagel,prewashedwithmethanol,withtoluene-methanol4:1inatwintroughchambersaturatedfor20min.Quantita-tivedeterminationbyabsorbancemeasurementat275nm.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104176 M.PENG(PengMinjie)*,D.LI(LiDuowei),Y.WANG(WangYichao),SH.JIA(JiaShaoliang)(*Inst.LifeSci.,North-WestUniversity,Xi‘an710069,China):(Determinationofscalreolinitsformulations by thin-layer chromatography) (Chinese). Chinese J. Pharm.Anal. 28 (9), 1554-1556(2008).TLCofscalreolonsilicagelwithn-hexane-ethylacetate-formicacid�2:16:1.Detectionbysprayingwithvanillin-sulfuricacid-ethanol1:1:18.Quantificationbydensito-metryat520nm.Linearitywasbetween10and50µg/zonewithadeterminationcoefficientof0.9994.Recoverywas100.1%(n=6,RSD=0.9%).Repeatability(%RSD,n=6)was2.1%withinplateand2.�%plate-to-plate.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,densitometry,quantitativeanalysis,qualitativeidentification �2c

104177 CH. PIAO (Piao Chunmei)*, X. QU (Qu Xiangling), X. ZHOU (Zhou Xunrong) (*AffiliatedHosp. No.2, Guizhou Inst.TCM, Guiyang, Guizhou 55000�, China): (Identification procedu-re forTongmaitangYanming capsuls) (Chinese). Chinese J. Hosp. Pharm. 29 (4), 1246-1247(2009).TLCofTCMdrugextractsonsilicagelwith1)chloroform-methanol-acetone10:1:1;2)toluene-chloroform-acetone-methanol-formicacid4:6:8:1:4;�)chloroform-methanol4:1.Detection1)afterexposuretoammoniavaporunderUV254nm;2)underUV254nm;�)bysprayingwith10%sulfuricacidinethanolfollowedbyheatingat105°Cuntilcoloration.

pharmaceuticalresearch,qualitycontrol,traditionalmedicine,qualitativeidentification �2e

104178 L.POTALE*,M.DAMLE,K.BOTHARA(*AISSMSCollegeofPharmacy,KennedRaod,Pune,Maharashtra,India):AvalidatedstabilityindicatingHPTLCmethodforsimultaneousestimati-onoftelmisartanandrampril.AbstractNo.F-271,61stIPC(2009).HPTLCoftelmisartanandramprilonsilicagelwithmethanol-chloroform1:6.ThehRFvaluewas�8and68forramprilandtelmisartan,respectively.Quantitativedeterminationbyabsorbancemeasurementat210nm.Thesamplewasexposedtodifferentstressconditions(acid,alkali,oxidative,photodegradationandthermal).Bothdrugsdidnotdegradeunderacidicandphotolyticconditions,butshowedsig-nificantdegradationunderalkalineandthermalconditions.Bothcompoundswerewellseparatedfromdifferentdegradationproductsunderexperimentalconditions.

pharmaceuticalresearch,qualitycontrol,densitometry,HPTLC,quantitativeanalysis �2a

104179 KirtiPRABHU*,R.LOBO,RichaAGRAWAL,A.SHIRWAIKAR,A.SHIRWAIKAR,MamathaBALLAL(*Dept.ofPharmacognosy,ManipalCollegeofPharmaceuticalScience,ManipalUni-versity,Manipal,India):Applicationofastability-indicatingHPTLCmethodforthequantitativedeterminationofhesperidin inpharmaceuticaldosageform.AbstractNo.9�24, IHCB(2009).HPTLCofhesperidin inorangepeelextractandformulationonsilicagelwithethylacetate -methanol-water100:17:1�.Quantitativedeterminationbyabsorbancemeasurementat287nm.Themethodwaslinearintherangeof10-1000ng/spot.Hesperidinwassubjectedtodegradationstudies(acid,alkali,hydrolysis,oxidation,andthermalstress)andwasfoundsusceptibletodiffe-

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CAMAGBIBLIOGRAPHYSERVICE No.104�9

rentstresscondition.Themethodwassuitablefordeterminationofhesperidinanditsdegradati-onproductsinbulkdrugaswellasformulations.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104180 S.L. PRABU*,T. SINGH, C.D. KUMAR,A. JOSEPH, K.K. SRINAVASAN (*Manipal Col-lege of Pharmaceutical Sciences, Manipal 576104, India; [email protected]): High-per-formance thin-layer chromatographic method for analysis of racecadotril in the bulk drug. J.PlanarChromatogr.22,277-281(2009).HPTLCofracecadotril(2-{2(acetylsulfanylmethyl)-�-phenylpropanoyl}aminoaceticacidbenzylester)anditsdegradationproductsinthebulkdrugand in a pharmaceutical formulation on silica gelwith n-hexane - ethyl acetate 7:� in a twintroughchambersaturatedfor�0min.Quantitativedeterminationbyabsorbancemeasurementat2�0nm.Thelimitofdetectionandquantificationwas50and100ng/band,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104181 N.PRAJAPATI*,V.YADAV,S.PANCHOLI(*S.K.PatelCollegeofPharmaceuticalEducationandResearch,Mehsana,Gujarat,India):DevelopmentandvalidationofHPTLCmethodforde-terminationofrepaglinideandrosiglitazonemaleateincombineddosageform.AbstractNo.F-26�,61stIPC(2009).HPTLCofrepaglinide(REPA)androsiglitazone(ROSI)onsilicagelwithbenzene-methanol-acetone-aceticacid80:10:9:1.Quantitativedeterminationbyabsorbancemeasurementat266nm.Lienaritywasintherangeof800-2800ng/bandand400-2400ng/bandforREPAandROSI,respectively.Recoverywas101.7and99.5%forREPAandROSI,respec-tively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104182 P.PUSHPALATHA*,R.K.SARIN,M.A.RAO,T.R.R.BAGGI(*CentralForensicScienceLa-boratory,DirectorateofForensicScience,MinistryofHomeAffairs,GovernmentofIndia,Ra-manthapur,Hyderabad50001�,India;[email protected]):Anewthin-layerchromatographicmethodforanalysisofzolpidemandzoplicone.J.PlanarChromatogr.22,449-451(2009).TLCofzolpidemandzopliconeonsilicagelwithmethanol-triethylamine�9:1,acetonitrile-triethyl-amine�9:1,chloroform-methanol-triethylamine�8:2:1,andacetonitrile-methanol-triethyl-amine�4:4:1withchambersaturation.Detectionbysprayingwithchloranilicacidreagent(0.5chloranilicacidindioxane)andevaluationofcoloredzonesindaylight.

toxicology,qualitativeidentification �2a

10418� Y.QI(QiYanfei)*,Q.GONG(GongQing),M.LU(LuMin)(*ZhejiangProvin.Inst.Food&Med.,Hangzhou,Zhejiang�10004,China):(StudyofthequalitystandardforQingshenJianfeipills)(Chinese).J.ChineseTrad.&Herb.Med.�9(12),1818-1829(2008).TLCoftheextractsoftheTCMdrugonsilicagelwith1)chloroform-methanol-acetone-ammonia2:1:4:4;2)chloroform-methanol-acetone-formicacid�2:8:4:7;�)ethylacetate-butanone-formicacid-water10:1:1:1;4)chloroform-methanol-water1�:7:2.DetectionbyevaluationunderUV�65nmandaftersprayingwith1)potassiumiodobismuthatereagent;2)a1:1mixtureof1%potas-siumferricyanideand1%FeCl�;�)bysprayingwith10%sulfuricacidinethanolfollowedbyheatingat105°Cuntilcoloration.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,qualitativeidentification �2c

104184 T.QU(QuTingli),Y.DENG(DengYaning),L.HAU(HauLihong),ZH.ZHAO(ZhaoZheng-bao)* (*Pharm. Coll., Shanxi Univ. Med.,Taiyuan Shanxi 0�0001, China): (Identification ofShenlingbaizhupillsbythin-layerchromatography)(Chinese).J.ChineseTrad.PatentMed.�0(12),Supl.4-6(2008).TLCof theTCMdrugextractsonsilicagelwith1)dichloromethane-ethylacetate-methanol-water15:40:22:10;2)petroleumether(60-90°C)-diethylether�:2;�)petroleumether(60-90°C)-ethylacetate25:2;4)n-butanol-aceticacid-water4:1:2;5)chlo-roform-diethylether1:1.Detection1)bysprayingwith10%sulfuricacidinethanolfollowed

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byheatingat105°Cuntilcoloration;2)underUV�65nm;�)underUV254nm.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,qualitativeidentification �2c

104185 P.RAJA*,K.BHATT,V.JOSHI,K.AMIN(*A.R.CollegeofPharmacyandG.H.PatelIns-tituteofPharmacy,Anand,Gujarat,India):DevelopmentandvalidationofHPTLCmethodforsimultaneous estimation of olmesartan medoxomil and hydrochlorothiazide in their combinedtabletdosageform.60thIndianPharmaceuticalCongressPA-2�2(2008).HPTLCofolmesartanmedoxomilandhydrochlorothiazideonsilicagelwithmethanol-toluene-ethylacetate5:11:4withchambersaturationfor�0min.ThehRFvalueofolmesartanmedoxomilwas27andofhy-drochlorothiazide44.Themethodwaslinearintherangeof�00-1800ng/spotforbothdrugs.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104186 K.P.RANDAU,S.SPROLL,H.LERCHE,F.BRACHER*(*DepartmentPharmazie-Zentrumfür Pharmaforschung, Ludwig-Maximilians-Universität, Butenandtstr. 5-1�, 81�77 München,Germany;[email protected]):Pernambucone,anewtroponederivativefromCrotonargyroglossum.Pharmazie64,�50-�51(2009).PreparativeTLCofpernambucone(�,8-dimethyl-5-isopropyl-2,�-dihydro-1H-azulene-1,6-dione), orobanone and extracts of stem barkonsilicagelwithhexane-ethylacetate4:1anddichloromethane-methanol�9:1.Detectioninvisiblelight.

pharmaceuticalresearch,herbal,preparativeTLC �2e

104187 P.RAO*,R.KUMAR,G.REDDY,R.BABOO(*A.M.ReddyMemorialCollegeofPharmacy,Guntur,A.P., India):MethoddevelopmentandvalidationofHPTLCmethod forestimationofquetiapineinbulkdrugsandintabletdosageform.AbstractNo.F-261,61stIPC(2009).HPTLCofquetiapineonsilicagelwithmethanol-toluene4:�.ThehRFvaluewas41.Quantitativedeter-minationbyabsorbancemeasurementat2�5nm.Themethodwaslinearintherangeof100-500ng/band.Recoverywas98.9%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104188 J.RAO*,S.YADAV,M.APNDE,S.GONDKAR(*BharatiVidyapeethUniversity,PoonacollegeofPharmacy,Pune,Maharashtra,India):StabilityindicatingHPTLCmethodfortenofovirinthebulkdrugandtabletdosageform.AbstractNo.F-252,61stIPC(2009).HPTLCoftenofovironsilicagelwithn-butanol-aceticacid-water4:1:1.ThehRFvaluewas58.Quantitativedetermi-nationbyabsorbancemeasurementat260nm.Linearitywasintherangeof120-600ng/band.Thecompoundwassubjectedtodifferentstressconditions(acid,alkali,oxidation,photodegrada-tionandthermal)anddegradationsproductswerewellresolvedfromthemaincomponent.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104189 K. REMYA*,A. BINDU, N.ALEYKUTTY, J. SAJAN (*Department of Pharmaceutical Sci-ence,CheruvandoorCampus,Ettumanoor,Kottayam,Keral,India):High-performancethin-layerchromatographicmethodforquantitativedeterminationofquercetinintenderleavesofPsidiumguajava.60thIndianPharmaceuticalCongressPG-264(2008).HPTLCofquercetininacetoneextractsofPsidiumguajava leaveson silicagelwith toluene - acetone - formic acid�8:10:5.Quantitativedeterminationofquercetinbyabsorbancemeasurementat�64nm.Thecorrelationcoefficientwas0.9847.Therewasagoodcorrelationbetweenpeakareaandcorrespondingcon-centrationofquercetin.TheproposedHPTLCmethodprovidedagoodresolutionofquercetinfromotherconstituentspresentinacetoneextractoftenderleavesofPsidiumguajavaandcanbeusedforthequantificationofquercetin.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104190 A. REN (RenAinu)*,Y. LI (LiYun), M. JU (Ju Mingqiao) (*Jiangsu Provin.Acad. Med. &Pharm., Nanjing, 210028, China): (Study of the quality standard for Baozhi pills, a Chinese

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traditionalpatentmedicine) (Chinese).Chinese J.Pharm.Anal. 28 (1), 20-2� (2008).TLCofTCMdrugextractsonsilicagelwithtoluene-ethylacetate-methanol-isopropanol-ammonia12:6:�:�:1.DetectionunderUVlight.ThemethodissuitableforqualitycontrolofBaozhipills.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,herbal,quantitativeanalysis,qualitativeidentification �2c

104191 A.RICHA*,S.KIRTI,L.RICHARD,S.ANNIE(*Dept.ofPharmacognosy,ManipalCollegeofPharmaceuticalScience,Manipal,Karnataka576104,India):Pharmacognostical,phytochemicalandHPTLCfingerprintingevaluationofDendrophthoe falcata leaf.AbstractNo.9712, IHCB(2009).HPTLCofextracts fromleavesofDendrophthoefalcataonsilicagelwithmethanol-formicacid-water40:�:57.Quantitativedeterminationbyabsorbancemeasurementat280nmusingquercetinasmarker.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104192 K.K.ROUT*,O.P.ROUT,S.K.MISHRA(*PharmacognosyandPhytochemistryDivision,Uni-versity Department of Pharmaceutical Sciences, Utkal University, Vani Vihar, Bhubaneswar751004,Orissa, India;[email protected]):StandardizationofAyurvedic formulationscon-tainingAloeverabyquantificationofamarkercompound.J.PlanarChromatogr.22,�81-�84(2009).TLCofaloinincommercialAyurvedicpreparationsonsilicagel(prewashedwithmetha-nol)withethylacetate-methanol-water50:7:2inatwintroughchamberwithchambersatura-tionfor5-7minat�0+/-4°Candarelativehumidityof57+/-�%.Quantitativedeterminationbyabsorbancemeasurementat�60nm.Thelimitofdetectionandquantificationwas10and20ng/band,respectively.

traditionalmedicine,herbal,qualitycontrol,quantitativeanalysis,densitometry �2e

10419� P.SAINI*,C.JAIN,R.SINGH,S.MATHUR,G.SINGH,M.NASLAM(*Research&Develop-mentDiv.,IndianPharmacopoeiaCommission,Govt.ofIndia,MinistryofHealth&FamilyWel-fare,Sector-2�,Rajnagar,Ghaziabad201002, India, [email protected]):A simple and sensitiveHPTLCmethod for simultaneousdeterminationof abacavir sulphate and lamivudine in tabletdosageform.J.Pharma.Research8(4),187-191(2009).HPTLCofabacavirsulphateandlami-vudineonsilicagelwithmethanol-acetone-n-butylacetate1:1:2.Quantitativedeterminationbyabsorbancemeasurementat284nm.ThehRFvalueofabacavirsulphatewas58andoflami-vudine�5.Linearityofabacavirsulphateandlamivudinewasintherangeof240-1200ng/spotand120-600ng/spot,respectively.Thelimitofdetectionandquantificationofabacavirsulphatewas0.7and2ng/spot,respectively,andoflamivudine1and�ng/spot,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104194 A.SARASWATHY*,D.RAMASAMY,S.ARIMASAMY,D.NANDINI(*CSMDrugResearchInst.forAyurvedaandSiddha,AnnaHospitalCampus,Arumbakkam,Chennai600106,[email protected]):DevelopmentofHPTLCprofileandheavymetalanalysisofstembarkofthreeFicusspecies.IndianDrugs46(6),49�-496(2009).HPTLCofchloroformextractsofthebarkofFicusracemosa,F.bengalensis,andF.religiosaonsilicagelwithtoluene-ethylacetate-formicacid90:10:1.DetectionunderUV254nmandvisiblelightaftertreatmentwithvanillinsulfuricacidreagent,followedbyheatingat105°Cuntilcoloration.

herbal,HPTLC,qualitativeidentification �2e

104195 N.SARATHI*,M.GANDHIMATHI,R.SAKTHI,T.RAVI(*SriRamakrishnaInstituteofPara-medicalScience,Coimbatore,TamilNadu,India):ArapidHPTLCanalysisofoxcarbazepineinhumanplasma.60thIndianPharmaceuticalCongressPA-227(2008).HPTLCofoxcarbazepine(inacetonitrileextractsofhumanplasma)onsilicagelwithethylacetate- toluene-methanol7:2:1.ThehRFvaluesofoxcarbazepineandtheinternalstandardchlorzoxazonewere54and86,respectively.Thelinearityrangewas10-�00ng/mL,recoveryfromplasmawas75.2%.

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qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104196 S.SATHE*,S.BARI(*DepartmentofPharmaceuticalChemistry,R.C.PatelCollegeofPhar-macy,KarwandNaka,ShirpurDhule,Maharashtra425405,India,[email protected],[email protected]):Quantitativeanalysisoflosartanpotassiumandatenololbyhigh-per-formancethin-layerchromatography.IndianDrugs46(1),78-81(2009).HPTLCofatenololandlosartanpotassiumin tabletsonsilicagelwith toluene -methanol - triethylamine12:8:1withchambersaturationfor45min.Quantitativedeterminationbyabsorbancemeasurementat2�0nm.ThehRFvalueofatenololwas45andoflosartanpotassium67.Themethodwaslinearintherangeof1000-4000ng/spotforbothcompounds.Therecoverywas98.8-98.9%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104197 SunitaSEERAPU*,B.SRINIVASAN(*DelhiInstituteofPharmaceuticalSciencesandResearch(DIPSAR),NewDelhi,India):DevelopmentandvalidationofanalyticalmethodonHPTLCforthedeterminationofivabradinehydrochlorideasbulkdrugandinpharmaceuticalformulations.AbstractNo.F-275,61stIPC(2009).HPTLCofivabradineHClonsilicagelwithmethanol-chloroform1:1.ThehRFvaluewas59.Quantitativedeterminationbyabsorbancemeasurementat285nm.Linearitywasintherangeof100-800ng/spotwithr2=0.9989(viapeakarea).

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104198 M.SHAH*,A.PRAJAPATI,S.PATEL,N.PATEL(*ShreeS.K.PatelCollegeofPharmaceu-ticalEducationandResearch,GanpatUniversity,GanpatVidyanagar,Mehsana,Gujarat,India):EstimationofvoriconazoleinpowderbyHPTLCmethod.60thIndianPharmaceuticalCongressPA-2�1(2008).HPTLCofvoriconazoleonsilicagelwithtoluene-ethylacetate1:�.Quantita-tivedeterminationbyabsorbancemeasurementat255nm.Thelinearityrangewas10-1200ng/spot,recoverywas99.5%.Themethodwassuitableforroutinequalitycontrolofformulations.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104199 N.SHAH*,B.SUHAGIA,R.SHAH,N.PATEL(*ShriB.M.ShahCollegeofPharmaceuticalEducation & Research, Modasa �8��15): HPTLC method for the simultaneous estimation ofvalsartanandhydrochlorothiazideintabletdosageform.Ind.J.Pharma.Sci.71(1),72-74(2009).HPTLCofvalsartanandhydrochlorothiazideonsilicagelwithchloroform-methanol-toluene-aceticacid60:20:10:1.Quantitativedeterminationbyabsorbancemeasurementat260nm.Thecalibrationcurvewaslinearbetween�00to800ng/spotforvalsartanand100to600ng/spotforhydrochlorothiazide.Thelimitofdetectionandthelimitofquantificationforvalsartanwere100and�00ng/spot,respectively,andforhydrochlorothiazide�0and100ng/spot,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104200 R.SHAH*,H.BHATT,G.PATEL,C.SHARASTRY(*ShreeDhanvantaryPharmacyCollege,Surat, Maharashtra, India): Simultaneous estimation of mosapride citrate and pantoprazole insoliddosageformbyHPTLCmethod.AbstractNo.F-2�6,61stIPC(2009).HPTLCofpantopra-zoleandmosapridecitrateonsilicagel(pre-washedwithmethanol)withethylacetate-benzene-methanol-25%ammonia48:�5:15:2atroomtemperature.Quantitativedeterminationbyabsor-bancemeasurementat250nmor276nm.Themethodwaslinearintherangeof�-7µg/bandforbothdrugs.Recoverywasbetween99.0and10�.5%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104201 R.SHAH*,H.PANCHAL,B.SUHAGLA,N.PATEL(*S.K.PatelCollegeofPharma.Educa-tion&Research,Mehsana,Gujarat,India):Simultaneousdeterminationofatorvastatincalcium,ramiprilandaspirin incapsuledosageformbyHPTLC.60thIndianPhamraceuticalCongressPA-209(2008).HPTLCofatorvastatincalcium,ramiprilandaspirinonsilicagelwithmethanol-benzene -ethylacetate -glacialaceticacid9:140:100:1.Quantitativedeterminationbyabsor-

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CAMAGBIBLIOGRAPHYSERVICE No.1044�

bancemeasurementat210nm.ThehRFvalueoframiprilwas6,ofatorvastatin�8,andofaspirin86.Linearitywas100-600ng/band(atorvastatin),50-�00ng/band(ramipril)and500-�000ng/band(aspirin).Recoverywas99.9-100.0%forallthreecompounds.Salicylicacid,animpurityofaspirin,wasobservedincapsuledosageformwithanhRFvalueof72.Themethodwassuitab-leforanalysisofcombineddosageform.

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis,HPTLC �2a

104202 K. SHAH*, I. SOJITRA, R. SHAH, U.VACHHANI (*Rofel Shri G. M. Bilakhia College ofPharmacy,Vpi,Gujarat,India):DevelopmentandvalidationofHPTLCanalyticalmethodforde-terminationofL-dopainMucunaprurienspowderedextractandpolyherbalformulations.Abs-tractNo.F-262,61stIPC(2009).HPTLCofL-dopaonsilicagelwithn-butanol-water-acticacid4:1:1.ThehRFwas�7.Detectionbysprayingwith0.5%ethanolicninhydrinsolution,fol-lowedbyheatingat120°Cfor2min.Quantitativedeterminationbyabsorbancemeasurementat520nm.Themethodwaslinearintherangeof600-1400ng/band.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

10420� N. SHARMA, U. SHARMA,A. GUPTA, DEVLA,A. SINHA*, B. LAL, P.AHUJA (*Natu-ralPlantProductsDivision,InstituteofHimalayanBioresourceTechnology(CSIR),Palampur,HimachalPradesh,India,[email protected]):Simultaneousdensitometricdetermina-tionof shikonin,acetylshikonin,andbeta-acetoxyisovaleryl-shikonin inultrasonic-assistedex-tractsoffourArnebiaspeciesusingreversed-phase thin layerchromatography.J.Sep.Sci.�2,�2�9-�245(2009).HPTLCofshikonin(1),acetylshikonin(2),andbeta-acetoxyisovalerylshiko-nin(�)infourspeciesofArnebiaonRP-18withacetonitrile-methanol-5%formicacid20:1:4.Quantitativedeterminationbyabsorbancemeasurementat520nm.Linearitywasintherangeof100-600ng/zonefor(1)and(2)and100-1800ng/zonefor(�).Thelimitsofdetectionfor(1),(2)and(�)were18,15and12ng/zone,respectively,whilethelimitsofquantificationwere60,45and40ng/zone,respectively.

herbal,traditionalmedicine,HPTLC,quantitativeanalysis,densitometry �2e

104204 A.A. SHIRKHEDKAR*, P.M. BUGDANE, S. SURANA (*R.C. Patel College of Pharmacy,ShirpurDist:Dhule,(M.S.)425405India):Stability-indicatingTLC-densitometricdetermina-tionofnebivololhydrochlorideinbulkandpharmaceuticaldosageform.J.Chromatogr.Sci.48(2),109-11�(2010).HPTLCofnebivololhydrochlorideonsilicagelwithtoluene-methanol-triethylamine19:6:1.ThehRFvalueofnebivololhydrochloridewas��.Quantificationbydensi-tometryintheabsorbancemodeat281nm.Linearitywasbetween500and�000ng/spotwithr2=0.9994.Thelimitofdetectionandquantificationwas6�and191ng/spot,respectively.Nebivololhydrochloridewassubjected toacidandalkalihydrolysis,oxidation, thermaldegradation,andphotodegradation.Thedegradationproductswerewell-resolvedfromthemaincomponent.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis,qualitativeidentification �2c

104205 A.A.SHIRKHEDKAR*,S.J.SURANA(*DepartmentofPharmaceuticalChemistry,R.C.PatelInstituteofPharmaceuticalEducationandResearch,ShirpurDist:Dhule(M.S.)India425405;[email protected];[email protected]):SimultaneousdensitometricTLCana-lyisofatorvastatincalciumandfenofibrateinthebulkdrugandinpharmaceuticalformulations.J.PlanarChromatogr.22,�55-�58(2009).TLCofatorvastatincalciumandfenofibrateonsilicagel,prewashedwithmethanol,withtoluene-methanol-triethylamine�5:15:1inatwintroughchambersaturatedfor25minatroomtemperatureandrelativehumidityof60+/-5%.Quantita-tivedeterminationbyabsorbancemeasurementat258nm.Thelimitofdetectionandquantifica-tionforatorvastatincalciumwas25and77ng/zone,respectivelyandforfenofibrate292and886ng/zone,respectively.

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis �2a

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104206 A.R.SHRIVASTAVA,C.R.BARHATE,C.J.KAPADIA*(*DepartmentofPharmaceutics,Bom-bayCollegeofPharmacy,Kalina,Santacruz,Mumbai400098,India;[email protected]):Stress degradation studies in valsartam using validated stability-indicating high-performancethin-layer chromatography. J.PlanarChromatogr. 22, 411-416 (2009).HPTLCofvalsartan inbulkdrugandinformulationsonsilicagel(prewashedwithmethanol)withtoluene-ethylace-tate-methanol-formicacid60:20:20:1inatwintroughchambersaturatedfor20min.Quantita-tivedeterminationbyabsorbancemeasurementat250nm.Thelimitofdetectionandquantifica-tionwas25and150ng/band,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC �2a

104207 N.SINGH,S.KHATOON*,N.SRIVASTAVA,A.K.SINGHRAWAT,S.MEHROTA(*Pharma-cognosy and Ethnopharmacology Division, National Botanical Research Institute, Rana PratpMarg,Lucknow226001,India;[email protected],[email protected]):Qualita-tiveandquantitativestandardizationofMyricaesculentaBuch.-HamstembarkbyuseofHPT-LC. J. Planar Chromatogr. 22, 287-291 (2009). HPTLC of the biomarkers gallic acid, lupeol,oleanolic acid, and stigmasterol and plant extracts on silica gel with toluene - ethyl acetate -formicacid5:5:1forgallicacidandwithtoluene-ethylacetate4:1forlupeol,oleanolicacid,andstigmasterolinasaturatedtwintroughchamber.Quantitativedeterminationbyabsorbancemeasurementat272nm.Detectionofoleanolicacid,lupeol,andstigmasterolbydippinginanis-aldehydereagentfollowedbyheatingat110°Cfor5min.Densitometricevaluationat652nm.

traditionalmedicine,herbal,qualitycontrol,HPTLC,quantitativeanalysis,densitometry �2e

104209 B.SINGH*,S.ANANDJIWALA,M.NIVSARKAR(*NationalInstituteofPharmaceuticalEd-ucationandResearch,Ahmedabad,Gujarat,India):TLCdensitometricanalysisofglycyrrhizin,glycyrrhetinicacid,apigenin,kaempferolandquercetinfromGlycyrrhizaglabrausingHPTLC.60th Indian Pharmaceutical Congress PG-�2� (2008). HPTLC of glycyrrhizin, apigenin andkaempferol inmethanolicextractsandglycyrrhetinicacidandquercetin inhydrolizedextractsofGlycyrrhizaglabraonsilicagelwithethylacetate-methanol-aceticacid-water40:5:5:10(forglycyrrhizin),toluene-ethylacetate-methanol-formicacid�0:15:1:2(forkaempferolandquercetin),ethylactate-ethanol-water-ammonia65:20:4:1(forglycyrrhetinicacid).Quantita-tivedeterminationbyabsorbancemeasurementat254nm(glycyrrhetinicacidandapigenin),258nm(glycyrrhizin)and280nm(kaempferolandquercetin).Theplantwasfoundtocontain1.07%glycyrrhizin, 0.64 % glycyrrhetinic acid, 0.007 % apigenin, 0.0� % kaempferol and 0.24 %quercetin.

HPTLC,densitometry,quantitativeanalysis �2e

104208 K.SINGH*,S.AGRAWAL,M.GUPTA(*DelhiInstituteofPharmaceuticalSciencesandRe-search,NewDelhi,India):DevelopmentandvalidationofimprovedHPTLCmethodforsimul-taneousdeterminationofcurcumin,demethoxycurcuminandbis-demethoxycurcumin.60thIn-dian Pharmaceutical Congress PA-22� (2008). HPTLC of curcumin, demethoxycurcumin andbis-demethoxycurcuminonsilicagelwithchloroform-methanol19:1.ThehRFvalueswere25,�8,and61forbis-demethoxycurcumin,demethoxycurcumin,andcurcuminrespectively.Quanti-tativedeterminationbyabsorbancemeasurementat420nm.Themethodwaslinearintherangeof50-400ng/spot(curcumin),10-150ng/spot(demethoxycurcumin),and5-40ng/spot(bis-de-methoxycurcumin).Recoverywasintherangeof99.2-100.5%forallthreecompounds.

traditionalmedicine,qualitycontrol,herbal,HPTLC,densitometry,preparativeTLC,quantitativeanalysis �2e

104210 P.SINHA*,M.DAMLE,K.BOTHARA(*AISSMSCollegeofPharmacy,Pune,Maharashtra,India):Avalidatedstabilityindicatingmethodfordeterminationofaspirinandclopidogrelbisul-phate.60thIndianPharmaceuticalCongressPA-208(2008).TLCofaspirinandclopidogrelbi-sulphateonsilicagelwithcarbontetrachloride-acetone5:2.ThehRFvalueofaspirinwas15andofclopidogrelbisulphate80.Quantitativedeterminationbyabsorbancemeasurementat220nm.Themethodwaslinearintherangeof2-6µg/spotforaspirinand�-6µg/spotforclopidogrel.

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pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis �2a

104211 KrystynaSKALICKA-WOZNIAK*,M.L.HAJNOS,K.GLOWNIAK(*DepartmentofPhar-macognosywithMedicinalPlantLaboratory,MedicalUniversityofLublin,Chodzki1,20-09�Lublin,Poland; [email protected]):High-performance thin-layer chromatographycombinedwithdensitometryforquantitativeanalysisofchlorogenicacidinfruitsofPeucedanumalsaticumL.J.PlanarChromatogr.22,297-�00(2009).HPTLCofchlorogenicacidandofplantextractsonsilicagelwithethylacetate-formicacid-water10:2:�andethylacetate-formicacid-aceticacid-water100:11:11:21inasaturatedhorizontalchamber.Quantitativedeterminationbyabsorbancemeasurementat�20nm.Qualitativedetectionbyderivatizationwithnaturalproductsreagent(1%inmethanol)followedbytreatmentwith5%PEG400inethanol.

herbal,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104212 DanutaSOBOLEWSKA*,Z.JANECZKO,I.PODOLAK,A.SZERLOMSKA(*DepartmentofPharmacognosy,JagiellonianUniversity,CollegiumMedicum,Medyczna9,�0-688Cracow,Po-land;[email protected]):Densitometric analysisofdiosgenin inmethanolic extractsofAlliumursinumcollectedatdifferenttimesduringplantdevelopment.J.PlanarChromatogr.22,�05-�07(2009).TLCofdiosgenininmethanolicextractsoffreshleavesandbulbsonsilicagelwithn-hexane-acetone4:1.Detectionbysprayingwith25%sulfuricacidinmethanolandheatingat100°Cfor2min.Quantitativedeterminationbyabsorbancemeasurementat540nm.

herbal,qualitycontrol,traditionalmedicine,densitometry,quantitativeanalysis �2e

10421� P.SONAWANE*,M.DHOKA,V.GAWANDE,P.VAIDYA(*AllIndiaShriShivajiMemorialSociety‘sCollegeofPharmacy,Pune,Maharashtra,India):SimultaneousestimationofcefiximetrihydrateanderdosteineinpharmaceuticaldosageformbyHPTLCmethod.AbstractNo.F-256,61stIPC(2009).HPTLCofcefiximetrihydrateanderdosteineincombinedcapsuledosageformonsilicagelwithethylacetate-acetone-methanol-water15:5:5:�.Quantitativedeterminationbyabsorbancemeasurementat2�5nm.Thecalibrationcurvewaslinearbetween100and500ng/bandforcefiximeand150to750ng/bandforerdosteine.Thelimitofdetectionandquantifi-cationforcefiximewas0.�7µg/mLand1.14µg/mL,respectivelyandforerdosteine0.��µg/mLand1.04µg/mL,respectively.

qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104214 N. SONI*, S. MANIMARAN, N. MURUGANANTHAM, S. DHANABAL, K. ELANGO(*Dept.ofPhytopharmacy&Phytomedicine,JSSCollegeofPharmacy,Ootacamund,TheNil-giri,TamilNadu,India):ValidatedHPTLCmethodfortheanalysisofcolchicine.AbstractNo.99��,IHCB(2009).HPTLCofcolchicinesinGloriosasuperba(collectedfromdifferentpartsofIndia)onsilicagelwithethylacetate-methanol200:27.ThehRFvalueofcolchicinewas29.Quantitativedeterminationbyabsorbancemeasurementat�50nm.Themethodwaslinearintherangeof50-1000ng/spot.ThesamplecollectedfromKeralawasfoundtocontainhighestlevelofcolchicines(0.24%).

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104215 B. SPARZAK, Miroslawa KRAUZE-BARANOWSKA*, L. POBLOCKA-OLECH (*MedicalUniversityofGdansk,DepartmentofPharmacognosywith theMedicinalPlantsGarden,Hal-lera 107, 80-416 Gdansk, Poland; [email protected]): High-performance thin-layer chroma-tographydensitometricdeterminationofbeta-sitosterolinPhyllantusspecies.J.AOACInt.92,1�4�-1�48(2009).HPTLCofbeta-sitosterol,beta-amyrinandplantextractsonsilicagelwithchloroform-n-hexane-methanol1�:6:1.Detectionbysprayingwithvanillin-orthophosphoricacidreagent,5%phosphomolybdicacid,oranisaldehydereagent,followedbyheatingat110°Cfor5min.Vanillinreagentprovidedthebestresults.Quantitativedeterminationbyabsorbancemeasurementat525nm.

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herbal,qualitycontrol,densitometry,quantitativeanalysis,HPTLC �2e

104216 MalgorzataSTAREK*,M.REJDYCH(*JagiellonianUniversity,CollegiumMedicum,Depart-mentof InorganicandAnalyticalChemistry,Medyczna9,�0-688Kraków,Poland;[email protected]):Densitometricanalysisofcelecoxib,etoricoxibandvaldecoxibinpharmaceuticalpre-parations.J.PlanarChromatogr.22,�99-40�(2009).TLCofcelecoxib,etoricoxib,andvaldeco-xibonsilicagelwithchloroform-acetone-toluene12:5:2withchambersaturationfor15minatroomtemperature.Quantitativedeterminationbyabsorbancemeasurementat254and290nm.

pharmaceuticalresearch,qualitycontrol,densitometry,quantitativeanalysis �2a

104217 G.S.SUBRAMANIAN*,A.KARTHIK,A.BALIGA,P.MUSMADE,S.KINI(*DepartmentofPharmaceuticalQualityAssurance,ManipalCollegeofPharmaceuticalSciences,ManipalUni-versity,Manipal,Karnataka,India576104;[email protected]):High-performancethin-layerchromatographicanalysisofbicalutamideinbulkdrugandliposomes.J.PlanarChromatogr.22,27�-276(2009).HPTLCofbicalutamideandleflunomide(asinternalstandard)onsilicagelwithtoluene-ethylacetate4:5inatwintroughchambersaturatedfor�0minatroomtemperature.Quantitativedeterminationbyabsorbancemeasurementat27�nm.The limitofdetectionandquantificationwas50and200ng/band,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104218 P.SUBRAMANIAN*,A.RAJENDRAN,V.MADHURAM,R.PADMA(*DrugStandardisati-onUnitO.U.B.�2,Raod,No.4,Habsiguda,Hyderabad500007,India,[email protected]):HPTLCfingerprintingofsomeethnomedicinallyimportantCassiaspecies.IndianDrugs46(6),477-482(2009).HPTLCofextractsofCassiaauriculata,C.obtusifolia,andC.unifloraandofchrysophanolandemodinonsilicagelwithtoluene-ethylacetate-formicacid10:�:1.Detec-tionunderUV254nm.Basedonthefingerprintandbycomparisonwithchemicalmarkersiden-tificationofeachspecieswaspossible.

herbal,densitometry,HPTLC,qualitativeidentification �2e

104219 A.SUGANTHI*,A.FATHIMUNNISA,T.RAVI(*CollegeofPharmacy,SRIPMS,Coimbatore,TamilNadu,India):HPTLCmethodfor thesimultaneousestimationof itopridehydrochlorideandpantoprazoleinpharmaceuticaldosageform.AbstractNo.F-264,61stIPC(2009).HPTLCofpantoprazoleanditopridehydrochlorideonsilicagelwithn-butanol-chloroform-25%am-monia7:2:1.ThehRFvaluewas54and75forpantoprazoleanditopridehydrochloride,respec-tively.Quantitativedeterminationbyabsorbancemeasurementat291nm.The linearityof themethodwas80-240ng/bandforpantoprazoleand�00-900ng/bandforitopride.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104220 A.SUGANTHI*,M.SRIKANTH,A.GOP,T.RAVI(*CollegeofPharmacy,SriRamakrishnaInstituteofParamedicalSciences,Coimbatore,Tamilnadu,India):AvalidatedHPTLCmethodfortheestimationoffenoverineincapsuledosageform.AbstractNo.F-270,61stIPC(2009).HPTLCoffenoverineonsilicagelwithmethanol-butylacetate1:4.ThehRFvalueoffenoveri-newas67.Thelinearitywasintherangeof50to500ng/bandwithacorrelationcoefficientof0.9976.Thelimitofdetectionandquantificationwas�0ng/bandand100ng/band,respectively.Therecoverywas100.1%.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104221 B.SUHAGIA*,T.RATHOD,S.SINDHU(*L.M.CollegeofPharmacy,Ahmedabad,Gujarat,India):QuantitativedeterminationofSapindussaponins in thepericarpofSapindusmukoros-si.AbstractNo.F-287,61stIPC(2009).HPTLCofsaponins(amixtureofthesevendifferentsapindosidesA,B,C,D,E,F,andG)inthepericarpofSapindusmukorossionsilicagelwithchloroform-methanol-water50:14:1.Detectionbyderivatizationwithsulfuricacidreagentand

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CAMAGBIBLIOGRAPHYSERVICE No.10447

evaluationundervisiblelight.ThehRFvaluesofsapindosidesAtoGare19,26,41,48,59,67,and75.Quantitativedeterminationbyabsorbancemeasurementat550nmafterderivatization.ThelinearityrangesforsapinosidesAtoGwere0.9-4.�,0.7-5.4,�.�-15.2,1.2-9.7,2.7-12.5,0.2-1.�,0.�-1.5µg/band.Thepericarpcontained15.2%w/woftotalsapindosides.

herbal,HPTLC,densitometry,postchromatographicderivatization,quantitativeanalysis �2e

104222 DivyaSUKUMAR*,R.ARIMBOOR,C.ARUMUGHAN(*Agroprocessing&NaturalProductsDiv.,NationalInstituteforinterdisciplinaryScience&Technology,Thiruvananthapuram,Kerala695010, India,[email protected]):HPTLCfingerprintingandquantificationof lignansasmarkersinsesameoilanditspolyherbalformulations.J.Pharm.Biomed.Anal.47,795-801(2008).HPTLCofsesaminandsesamoline(themajorlignansinsesamumoilanditsherbalfor-mulations)onsilicagelwithbenzene-methanol50:1withchambersaturation.Quantitativede-terminationbyabsorbancemeasurementat290nm.TheidentityofsesaminandsesamolinewasconfirmedbyUV-VISspectra,NMRandMSofthecompoundsobtainedbyscrapingofffromtheplateandelution.Forfingerprintanalysisderivatizationwith5%methanolicsulphuricacidwasperformed,followedbyheatingat100°Cfor20minanddensitometryat450nm.

pharmaceuticalresearch,herbal,HPTLC,densitometry,quantitativeanalysis,comparisonofmethods,postchromatographicderivatization �2e

10422� KatarzynaSZEWCZYK*,L.KOMSTA,A.SKALSKA.KAMINSKA(*DepartmentofPharma-ceuticalBotany,FacultyofPharmacy,MedicalUniversityofLublin,Chodzki1,20-09�Lublin,Poland;[email protected]):DensitometricHPTLCmethodforanalysisoftriterpenoidsintheleavesofJovibarbasobolifera(Sims.)Opiz(Hennadchickenshouseleek).J.PlanarChro-matogr.22,�67-�69(2009).HPTLCoftriterpenoids(alpha-andbeta-amyrin,oleanolicacid)onsilicagelprewashedwithmethanolanddichloromethane,withdichloromethane-ethylacetate�7:�.inahorizontalchambersaturatedfor15min.Detectionbysprayingwith8%sulfuricacidinethanolandheatingat105°Cfor�min.EvaluationindaylightandunderUV�66nm.Quan-titativedeterminationbyabsorbancemeasurementat520nm.

herbal,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2e

104224 E.TOTH*,G.JANICSAK,I.MATHE,G.BLUNDEN(*InstituteofEcologyandBotanyoftheHungarianAcademyofSciences,Alkotmayu.2,216�Vacratot,Hungary;[email protected]):DeterminationofphenylpropanoidsinthreeBallotaspecies.J.PlanarChromatogr.22,29�-296(2009).TLCofverbascoside,forsythosideB,caffeoyl-malicacidandplant(Ballotanigra,B.hirsuta,andB.rupestris)extractsonsilicagelwithformicacid-aceticacid-water-ethylacetate15:15:�6:1�4.Quantitativedeterminationbyfluorescencemeasurementat�95nm.ItwasobservedthatamountsofphenylpropanoidsinBallotanigraleavesincreaseduringthemainandsecondaryfloweringperiodsinJune.

herbal,qualitycontrol,densitometry,quantitativeanalysis �2e

104225 J.VADHAVANA*,B.PATEL,R.PATEL(*K.B.InstituteofPharmaceuticalEducationandRe-search,Gandhinagar,Gujarat, India):Simultaneous estimationof nebivolol hydrochloride andS-amlodipinebesylatebyhigh-performancethin-layerchromatography.AbstractNo.F-247,62stIPC(2009).HPTLCofnebivololHClandS-amlodipinebesylateonsilicagel(prewashedwithmethanol)with chloroform - toluene -methanol - acetic acid50:20:1.ThehRFvaluewas��and48forS-amlodipineandnebivolol,respectively.Quantitativedeterminationbyabsorbancemeasurementat271nm.Themethodwaslinearintherangeof500-2500ng/bandfornebivololand250-1280ng/bandforS-amlodipine,respectively.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104226 D.VASA*,N.VASA,P.GIDE,V.VAGHELA(*A.R.CollegeofPharmacy&G.H.PatelInsti-tuteofPharmacy,Anand,Gujarat,India):HPTLCmethoddevelopmentforestimationofrivas-tigminehydrogentartrateinpharmaceuticaldosageform.AbstractNo.F-�65,61stIPC(2009).

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HPTLCofrivastigminehydrogentartrateonsilicagelwithmethanol-25%ammonia-aceticacid200:7:2.ThehRFvaluewas54.Quantitativedeterminationbyabsorbancemeasurementat215nm.Themethodwaslinearintherangeof1-10µg/band.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

104227 S.VASANTHARAJU*,A.KARTHIK,K.BHAT,C.PRASHANT,M.RAO,N.UDUPA(*Ma-nipalCollegeofPharmaceuticalScience,Manipal,Karnataka,India):HPTLCmethoddevelop-mentandvalidationofcapsaicininbulkdrug.AbstractNo.9452,IHCB(2009).HPTLCofcap-saicinonsilicagelwithtoluene-ethylacetate�:2.ThehRFvalueofcapsaicinwas�8.Quantita-tivedeterminationbyabsorbancemeasurementat280nm.Themethodwaslinearintherangeof100-1000ng/spot.Capsaicinwassubjectedtodifferentstressconditions(alkali,acid,oxidation,thermal).Themethodissuitableforseparationofcapsaicinfromitsdegradationproductsandcanbeusedtoindicatestability.

pharmaceuticalresearch,qualitycontrol,herbal,HPTLC,densitometry,quantitativeanalysis �2e

104228 R.VERMA*,H.MUKHTAR,R.SINGH,A.PASRIJA(*S.B.SCollegeofPharmacy,Patty,Pun-jab, India):ValidatedHPTLCmethod for thedeterminationof�H-4M-benzaldehyde in crudeplant material, extracts and dosage form of Hemidesmus indicus. 60th Indian PharmaceuticalCongressPG-�49(2008).HPTLCof�H-4M-benzaldehyde(incrudeplantmaterial,extractsanddosageformofHemidesmusindicus)onsilicagelwithtoluene-ethylacetate-methanol-aceticacid15:�:1:1.Quantitativedeterminationbyabsorbancemeasurementat2�0nm.

herbal,HPTLC,densitometry,quantitativeanalysis �2e

104229 S.WAKODE*,H.SINGH,V.SINGH(*DelhiInstituteofPharmaceuticalScience&Research,NewDelhi,India):DevelopmentandvalidationofHPTLCassaymethodforvoriconazoleinta-blets.60thIndianPharmaceuticalCongressPA-229(2008).HPTLCofvoriconazoleonsilicagelwithtoluene-methanol-glacialaceticacid78:20:1.Quantitativedeterminationbyabsorbancemeasurementat254nm.Themethodwas linear in therangeof50-400ng/spot, recoverywas99.9-100.7%.Themethodwassuitableforroutinequalitycontrolofthedosageform.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

1042�0 P.WAVHAL*,J.SANGSHETTI,A.SARKATE,P.WAKTE,D.SHINDE(*Dept.ofChemicalTechnology,Dr.BabasahebAmbedkarMarathwadaUniversity,Aurangabad,Maharashtra,India):Stability-indicatingHPTLCdeterminationof tadalafil inAPIandinitspharmaceuticaldosageform.AbstractNo.F-257,61st IPC (2009).HPTLCof tadalafilon silicagelwithn-hexane -ethylacetate-acetonitrile14:�:�.ThehRFvaluewas65.Quantitativedeterminationbyabsor-bancemeasurementat215nm.Themethodwaslinearintherangeof10-60ng/band.Thedrugwassubjected todifferentstressconditions (acid,alkali,oxidative,photodegradation, thermal)andshoweddegradationunderallstressconditions.Degradationproductsandexcipientsoftheformulationwerewellseparatedfromthemaincomponent.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,quantitativeanalysis �2a

1042�1 T.XONG(XongTing)(Pharm.Coll.,WuhanUniv.,Wuhan,Hubei4�0072,China):(Determina-tionofastragalosideinTianjiancapsule)(Chinese).ChineseJ.Hospit.Pharm.29(4),��6-��8(2009).TLCofastragalosideinTianjiancapsulesonsilicagelwithchloroform-methanol-wa-ter1�:6:2.Detectionbysprayingwith5%sulfuricacidinethanolfollowedbyheatingat105ºCuntilcoloration.Quantificationbydensitometryat515nm.Thelinearitywasbetween0.98and4.90µg/spot(r2=0.998),the%RSDwas2.4%(n=6)withinplateand2.�%(n=6)inter-plate,standardadditionrecoverywas99.2%withRSD=1.7%(n=6).

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,herbal,quantitativeanalysis,qualitativeidentification,densitometry �2e

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1042�2 L.XU(XuLi)*,Y.ZHAO(ZhaoYuan),Y.LUAN(LuanYuquan),Y.YANG(YangYongshou),CH.WANG(WangChengjun) (*BasicMed.Coll.,DaliAcad.,Dali,Yunnan671000,China):(StudyofthecontentofpuerarinindifferentpartsofRadixPuerariae)(Chinese).LearnedJ.DaliAcad.(GeneralIssue)8(10),�-6(2009).TLCofpuerarin(inextractsobtainedfromdifferentpartsofRadixPuerariae)onsilicagelwithtrichloromethane-methanol-water14:5:1.Detec-tionunderUV254nm.Themaximumamountofpuerarinwasfoundin thebineof thedrug,followedbythatintheroot,whereasnopuerarinwasfoundintheflowerandfruit.

pharmaceuticalresearch,traditionalmedicine,herbal,qualitycontrol,quantitativeanalysis,qualitativeidentification �2e

1042�� A.YADAV,R.M.SINGH*,S.C.MAHTUR,P.K.SAINI,G.N.SINGH(*IndianPharmacopoeiaCommission,Govt.ofIndia,MinistryofHealth&FamilyWelfare,Sect-2�,Rajnagar,Ghazia-bad(U.P),India201002;[email protected];[email protected]):Asimpleandsensi-tiveHPTLCmethodforsimultaneousanalysisofdomperidoneandparacetamolintabletdosageform.J.PlanarChromatogr.22,421-424(2009).TLCofdomperidoneandparacetamolonsilicagelwithacetone - toluene -methanol2:2:1 ina twin troughchamber saturated for�0minatroomtemperature.Quantitativedeterminationbyabsorbancemeasurementat285nmfordompe-ridoneandat248nmforparacetamol.

pharmaceuticalresearch,qualitycontrol,quantitativeanalysis,densitometry �2a

1042�4 A.YADAV*,N.TIWARI,P.SRIVASTAVA,S.SINGH,K.SHANKER,R.VERMA,M.GUP-TA(*AnalyticalChemistryDiv.Central InstituteofMedicinalandAromaticPlants,Lucknow226015, India,[email protected]): Iridoidglycoside-basedquantitativechromatogra-phicfingerprintanalysis:Arationalapproachforqualityassessmentof indianmedicinalplantGambhari (Gmelina arborea). J. Pharm. Biomed.Anal. 47, 841-846 (2008). HPTLC of irido-idglycosides in theaerialpartofGambhari (Gmelinaarborea)with iridoidgycoside6-0-(2“,�“-dibenzoyl)-o-L-rhamnopyranosylcatalpolasachemicalmarkerforthestandardizationofG.arboreaplantextractsonsilicagelwithchloroform-methanol4:1.Quantitativedeterminationbyabsorbancemeasurementat240nmandat4�0nmafterderivatizationwithvanillin-sulfuricacidreagent.Thelinearworkingrangewasbetween1000-5000ng/spotwithagoodcorrelationcoefficientof0.994.

pharmaceuticalresearch,qualitycontrol,HPTLC,densitometry,comparisonofmethods,quantitativeanalysis,postchromatographicderivatization �2e

1042�5 H.YAN(YanHua)*,Y.ZHANG(ZhangYumei),J.SONG(SongJincui),J.LU(LuJing)(*Nat.Inst.Cont.Pharm.&Biolog.Prod.,Beijing100050,China):(AnalysisofadenosineandadenineinLingzhicapsulesbyTLCandHPLC)(Chinese).ChineseJ.Pharm.Anal.28(11),1800-180�(2008).TLCofadenosineandadenineinLingzhicapsulesonsilicagelwithchloroform-ethylacetate-i-propanol-water16:6:�:1.DetectionunderUV254nm.Themethodissimple,fastandaccurateandcanbeusedforthequalitycontrolofthemedicine.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,herbal,quantitativeanalysis,qualitativeidentification �2c

1042�6 L.YANG (Yang Li)*, SH. ZHANG (Zhang Shengwan),W. DU (DuWen),WWANG (WangWei),M.LI(LiMeiping)(*Coll.LifeSci.&Technol.,ShanxiUniv.,Taiyuan0�00�6,China):(DeterminationofhyperosideintherawextractofHypericumperforatumbythin-layerchromato-graphy)(Chinese).ChineseJ.Pharm.Anal.28(4),608-610(2008).TLCofhyperosideintherawextractofHypericumperforatumonsilicagelwithpetroleumether(60-90°C)-ethylacetate-methanol1:4:2.Detectionunderdaylight.Quantificationbydensitometryat591nm.Linearitywasgivenbetween0.1and14.4µg/spot(r2=0.9892),recoverywasbetween96.4and100.1%.

pharmaceuticalresearch,qualitycontrol,traditionalmedicine,herbal,qualitativeidentification,quantitativeanalysis,densitometry �2c

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1042�7 H.E. ZAAZAA*, S.S. ABBAS, M. ABDELKAWY, M.M. ABDELRAHMAN (*AnalyticalChemistryDepartment,FacultyofPharmacy,CairoUniversity,KasrEl-AiniSt.,11562Cairo,Egypt):Spectrophotometricandspectrodensitometricdeterminationofclopidogrelbisulfatewithkineticstudyofitsalkalinedegradation.Talanta78(�),874-884(2009).Presentationofasensi-tive,selectiveandprecisestability-indicatingmethodforthedeterminationofclopidogrelbisul-fateinpresenceofitsalkalinedegradateandinpharmaceuticalformulations.TLConsilicagelwithhexane-methanol-ethylacetate87:10:�.Quantificationbydensitometryat248nmintherangeof0.6-�µg/band.Recoverywas99.9%.Clopidogrelcouldbedeterminedinthepresenceofupto90%ofitsalkalinedegradate.Methodselectivitywasevaluatedusinglaboratorypre-paredmixtures.Theanalysisofclopidogrelinpharmaceuticaldosageformsispossiblewithoutinterferencefromadditives.

pharmaceuticalresearch,qualitycontrol,quantitativeanalysis,qualitativeidentification,comparisonofmethods �2c

1042�8 CH.ZHENG(ZhengCheng)*,T.YAO(YaoTongwei),ZH.BAI(BaiZhimin)*(Pharm.Coll.,ZhejiangUniv.,Hangzhou�10080,China):(StudyofthequalitystandardforJinlupills)(Chi-nese).J.ChineseTrad.&Herb.Drugs40(6),900-90�(2009).TLCoftheTCMdrugextractsonsilicagelwith1)ethylacetate-formicacid-glacialaceticacid-water15:1:1:2;2)petroleumether(�0-60°C)-ethylacetate-formicacid15:5:1;�)chloroform-ethylacetate-methanol-water�1:81:25:2.Detection1)bysprayingwith10%sulfuricacidinethanolfollowedbyhea-tingat105°Cuntilcoloration;2)underUV254nm.

pharmaceuticalresearch,traditionalmedicine,qualitycontrol,qualitativeidentification,quantitativeanalysis �2e

1042�9 Y.ZHOU(ZhouYing)*,X.NIU(NiuXiuhua)(*Nat.Inst.Cont.Pharm.&Biolog.Prod.,Bei-jing100050,China):(Determinationofrelatedimpuritysubstancesinnisoldipinebythin-layerchromatography)(Chinese).DrugStandardsofChina9(2),144-146(2008).TLCofnisoldipinesilicagelwithchloroform-acetone-triethylamine-water90:5:1.DetectionunderUV254nm.Semiquantificationofimpuritiesbycomparisonofspots.Themethodwassuccessfullyusedforthequalitycontrolofreallifesamples.

pharmaceuticalresearch,qualitycontrol,quantitativeanalysis,qualitativeidentification �2c

33. Inorganicsubstances104240 A. RADOICIC, H. MAJSTOROVIC,T. SABO, Z.TESIC, Dusanka MILOJKOVIC-OPSENI-

CA*(*FacultyofChemistry,UniversityofBelgrade,P.O.Box51,11158Belgrade,Serbia;[email protected]):Hydrophilic-interactionplanarchromatographyofsomewater-solubleCo(III)complexesondifferentadsorbents.J.PlanarChromatogr.22,249-25�(2009).Investiga-tionofthechromatographicbehavoroftwelveneutral,mixedcobalt(III)complexesoftheuns-cis-edda-typeinsixplanarchromatographicsystems.Fourdifferentstationaryphases-silicagel,cyanophase,cellulose,andalumina-werecombinedwithwater-organicsolvent(methanoloracetone)binarymobilephases.Hydrophilic-interactionchromatographywasassumedtobethemechanismdeterminingseparationundernormal-phaseconditions (useofmobilephaseswithsmallamountsofwater),whereastheuseofmobilephaseswithhighwatercontentleadtorever-sed-phasechromatography.

qualitativeidentification ��a

35. Othertechnicalproductsandcomplexmixtures104241 DorinaCASONI*,C.SARBU(*DepartmentofAnalyticalChemistry,FacultyofChemistryand

ChemicalEngineering,Babes-BolyaiUniversity,AranyJanosStr.No11,400028Cluj-Napoca,Romania): Lipophilicity of some preservatives estimated by RP-TLC using stationary phaseswithdifferentpolarity.Chromatographia70(7-8),1277-1282(2009).HPTLCofpreservativesonthreestationaryphasesofdifferentpolarity:RP-18,RP-18Wandcyanophase,withmethanol-watermixturesindifferentvolumeproportions.TheresultingRMvaluesshowedalineardecre-asewithincreasingmethanolconcentrationofthemobilephase(determinationcoefficientsforallstationaryphaseswere>0.98).TheretentionbehaviorofthepreservativesonRPphaseisin

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CAMAGBIBLIOGRAPHYSERVICE No.10451

goodagreementwiththeirpolarity.Principalcomponentanalysisshowedthatforallthreestatio-naryphasesthesamelipophilicinteractionstakeplace.

HPTLC,autoradiography �5b

38. Chiralseparation104242 R.BHUSHAN*,H.BRÜCKNER,V.KUMAR(*DepartmentofChemistry,IndianInstituteof

TechnologyRoorkee,Roorkee247667,India):Indirectresolutionofenantiomersofpenicilla-minebyTLCandHPLCusingMarfey‘sreagentanditsvariants.Bio.Chromatogr.21(10),1064-1068(2008).IndirectchiralTLCseparationofpenicillamine(�,�-dimethylcysteine)enantiomersafterderivatizationwithMarfey‘s reagent (FDNP-Ala-NH2)and twoof itsstructuralvariants,FDNP-Phe-NH2andFDNP-Val-NH2onsilicagelandRP-18withphenol-water�:1andsol-ventcombinationsofacetonitrileandtriethylaminephosphatebuffer.Themethodswereappliedfordeterminationoftheenantiomericimpurityofl-penicillamine,d-penicillamine,andpharma-ceuticalformulationsofd-penicillamine.

pharmaceuticalresearch,qualitycontrol,quantitativeanalysis,qualitativeidentification,comparisonofmethods�8,28a

10424� R.BHUSHAN*,S.TANWAR(*DepartmentofChemistry,IndianInstituteofTechnologyRoor-kee,Roorkee-247667,India):Differentapproachesofimpregnationforresolutionofenantio-mersofatenolol,propranololandsalbutamolusingCu(II)-l-aminoacidcomplexesforligandex-changeoncommercialthin-layerchromatographicplates.J.Chromatogr.A1217(8),1�96-1�98(2010).Sparationofenantiomersofatenolol,propranolol, and salbutamolusingdifferent loa-ding/impregnationtechniquesfortheCu(II)complexesofl-proline,l-phenylalanine,l-histidine,N,N-dimethyl-l-phenylalanine,andl-tryptophan.TLConsilicagelwithacetonitrile-methanol-2mMaqueoussolutionofCu(II)�:4:5.Thedifferenttechniqueswere:A)usingtheCu(II)-l-ami-noacidcomplexaschiralmobilephaseadditive,B)developmentofplatesinsolutionsofCu-complex,andC)withasolutionofCu(II)acetateasmobilephaseadditiveforplatesimpregnatedwiththeaminoacids.Detectionofzonesbyexposuretoiodinevapor.

pharmaceuticalresearch,qualitycontrol,quantitativeanalysis,qualitativeidentification,comparisonofmethods �8

104244 R.BHUSHAN*,S.TANWAR(*DepartmentofChemistry,IndianInstituteofTechnologyRoor-kee,Roorkee,247667,India):DirectTLCresolutionoftheenantiomersofthreebeta-blockersbyligandexchangewithCu(II)-L-aminoacidcomplex,usingfourdifferentapproaches.Chroma-tographia70(5-6),1001-1006(2009).ChiralTLCoftheenantiomersofatenolol,propranolol,andsalbutamolbycomplexationwithCu(II)cationandfiveL-aminoacidsusingdifferenttech-niques:1)usingtheCu(II)-L-aminoacidcomplexaschiralmobilephaseadditivewithuntreatedsilicagelplates,2)bymixingtheCu-complexwithsilicagelbeforepreparingtheTLCplates,�)bydevelopmentwithsolutionsoftheCu-complexonuntreatedsilicagelplates,and4)byusingasolutionofCu(II)acetateasmobilephaseadditiveforplatespreparedbymixingtheL-aminoacidwithsilicagel.Detectionofzonesbyexposuretoiodinevapor.

pharmaceuticalresearch,qualitativeidentification �8

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CAMAGBIBLIOGRAPHYSERVICE No.10452 International Symposium for High-Performance Thin-Layer Chromatography

BASEL, 06th – 08th July 2011

International Scientific Committee Prof. Dr. Colin Poole, USA (chairman) PD Dr. Gertrud Morlock, Germany (co-chairwoman)Prof. Dr. Mario Vega, ChileProf. Dr. Wang Zheng Tao, China Dr. Jacques Pothier, France Prof. Dr. Ilkka Ojanperä, Finland Prof. Dr. Lothar Kroh, GermanyProf. Dr. Imre Klebovich, Hungary Dr. J. Madhusudana Rao, IndiaProf. Dr. Teresa Kowalska, Poland Dr. Wanchai De-Eknamkul, Thailand Dr. Irena Vovk, SloveniaDr. Vicente Cebolla, SpainDr. Eike Reich, SwitzerlandProf. Dr. Joseph Sherma, USA www.hptlc.com

We are enthusiastic to learn how many analysts are now confronted with situations where HPTLC is a suitable solution to their problems and is favored over better known and more widely used analytical methods. At the same time it is rather difficult nowadays to find a place for this “old technique” in the minds of opinion leaders, even if the need exists in analytical laboratories. This has arisen through inadequate infor-mation and training.

How to select the method; how to use HPTLC when it is described as a method of choice; avoidance of usual mistakes; which other samples may be well covered by this technique;… To address these issues an exchange of knowledge is foremost, from which sprang our mo-tivation to hold again an international event with the Interlaken series spirit, last held in 1997. After Lyon 2003, Berlin 2006, and Helsinki 2008, we are pleased to announce that the 4th International Symposium for High-Performance Thin-Layer Chromatography will be organized on 06th – 08th July 2011, in the Congress Centre of Basel, Switzerland. This new major issue will include a workshop, a symposium, and a manufacturers session.

The scientific program will feature invited keynote speakers, selected submitted lectures and poster pre-sentations. Contributions are invited from all areas of high-performance thin-layer chromatography, but especially from colleagues working in the pharmaceutical, food, environmental and medical fields. Papers on theory, method development, validation, instrumental methods, hyphenated techniques, and quantitative applications in all areas of chemistry would be most welcome.

Deadlines for Abstract submission (oral and poster): March 1st 2011 Final registration: May 30th 2011

The participation fee includes the full scientific pro-gram, and added to that, lunches, coffee breaks, the symposium dinner, and the social events. Industrial 500 € Academic 400 € Students 200 € Reduction of 100 € with ISPS or CCCM membership.

Special accommodation rates are available for hotels close to the symposium venue.

[email protected] for general information [email protected] for scientific matters [email protected] for registration concerns

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Separation of triterpenoids on silica gel (A) and RP18 phases (B: ethyl acetate – acetonitril 3:2, C: acetone – acetonitrile 5:1). Tracks: 1 a-amyrin; 2 - amyrin; 3 - amyrin; 4 lupeol; 5 lupeol acetate; 6 cycloartenol; 7 cycloartenol acetate; 8 lupenon; 9 ur-solic acid; 10 oleanolic acid; 11 a-amyrin, -amyrin and lupeol; 12 cabbage; 13 rosemary; 14 sage; 15 oak bark; 16 tomato

Moreover, both reversed phase methods enabled to some extent the separation of triterpenoids with different functional groups, yet with no interference from the structurally related sterols.

For identification of compounds, the character-istic colors and fluorescence of bands obtained after derivatization with anisaldehyde sulfuric acid reagent were helpful. Through this selective, post-chromatographic derivatization for all samples in parallel, HPTLC provides easy, fast and inexpensive screening of triterpenoids.

Further information is available on request from the author(s).

[1] M. Martelanc, I. Vovk, B. Simonovska, J. Chromatogr. A 1164 (2007) 145 and [2] dito 1216 (2009) 6662

* Dr. Irena Vovk, National Institute of Chemistry, Laboratory for Food Chemistry, Hajdrihova 19, 1000 Ljubljana, Slovenia, [email protected]

Characteristic fluorescence of bands under UV 366 nm after derivatization with anisaldehyde sulfuric acid reagent; separa-tion on RP18 plates with ethyl acetate – acetonitrile 3:2 (left) and acetone – acetonitrile 5:1 (right)

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The separation of isomeric triterpenols (a-amyrin, -amyrin, lupeol and cycloartenol) was achieved using the solvent system ethyl acetate - acetonitril 3:2, but with this system the separation of isomeric esters failed. On the other hand, solvent system acetone –

acetonitrile 5:1 separated the mentioned isomeric esters, but cycloartenol was not fully separated from a-amyrin.

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2 min (silica gel plate) or 30 s (RP18 plate).

Note (editor): In case of quantification the plate has to be placed on the cold TLC Plate Heater, being heated to 110 °C. By doing so, homogeneous heating across the whole plate is assured, and thus a good precision guaranteed.

DocumentationWith DigiStore 2 under UV 366 nm and under white light illumination

Results and discussionThe separation of triterpenoids with different func-tional groups (alcohols, acids, ketones and esters) has been generally achieved on silica gel plates, although the use of RP18 plates was crucial for the separation of four isomeric triterpenols and two triterpenol esters.

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Validated determination of secoisolariciresinol diglucoside in flaxseed by HPTLC

Prof. Silvia Coran

Getting the very best results from any analytical system requires a clear understanding of the capa-bilities of each instrument in the system, as well as any attachments, the sampling procedure and of course the software. This is particularly true with HPTLC where the components for each step must be coordinated in order to realize the technique’s full problem solving capabilities. No where is this more apparent than at the University of Florence as promoted by Silvia A. Coran*, Associate Profes-sor of Pharmaceutical Chemistry of Department of Pharmaceutical Science. Since HPTLC affords much flexibility for operative parameter optimization, novel analytical HPTLC methods have been set up as powerful alternative to HPLC. Even validation based on the more demanding HPLC protocols has been successfully carried out here at the University.

IntroductionSecoisolariciresinol diglucoside (SDG) is a plant lig-nan most notably found in flaxseed. The consider-able interest in SDG is driven by the observation that it is the main precursor for mammalian lignans that potentially protect against hormone related cancers. Since SDG is plant-derived and shows a weak estro-genic activity, it is classified as phytoestrogen.

Following a previously proposed novel method for the quantitative determination of SDG in flaxseed using silica gel plates [1], a significant improvement

Planar Chromatography in Practice

Sample preparationFlaxseed was frozen in liquid N2 and very finely ground. 100 mg of the resulting undefatted meal were suspended in 2 mL of aqueous NaOH 0.1 M and sonicated for 60 min at 40 °C. After cooling to room temperature the sample was neutralized with HCl, acidified to pH 3 with 50 µL HCOOH and diluted to 10 mL with MeOH. For the assay, 5 µL of this solution were applied.

Standard solutionThe stock solution was prepared by dissolving

of the procedure was set up by shifting from silica gel phases to C18 phases to assure the essential run to run reproducibility without any need for control of the plate activity [2].

With this change, a selective and robust meth-od was obtained and fully validated by apply-ing the SFSTP (Société Francaise des Sciences et Techniques Pharmaceutiques) Commission protocol [3] tailored for HPLC determinations. This protocol encompasses the calculation of accuracy profiles, the total error measurement and the associated risk. The validated method is competitive with the more popular HPLC approach in terms of simplicity of execution and routine throughput. But above all, HPTLC allows to exclude the time-consuming flaxseed defatting from the sample preparation step.

Chemical structure of secoisolariciresinol diglucoside (SDG)

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Horizontal Developing Chamber (HDC)

The Horizontal Developing Chamber (HDC) allows the development of a plate from both opposite sides toward the middle, thus dou-bling the number of samples per plate com-pared to conventional developing techniques. Here the HDC is used for determination of secoisolariciresinol. In this application, using the HDC 10 x 10 cm, 18 samples are simul-taneously developed in 12 min. Use of the HDC 20 x 10 cm would develop 36 samples in 12 min! This would result in 40 and 20 sec-onds per sample, respectively.

For development, 4 mL solvent were used for chromatography, but already 2.5 mL solvent per side are sufficient. Thus, compared to other chamber types the HDC consumes less solvents, e.g. 75 % less compared to a flat bottom chamber. Also the disposal costs are far below 0.01 Cent per sample.

Easy handling is combined with a high de-gree of flexibility for conditioning in the tank configuration or for chromatography in the sandwich configuration. The HDC is unsur-passed from an economic point of view, in flexibility and reproducibility of the result in routine work. Test it!

4.3 mg of SDG in 5 mL of MeOH (0.86 mg/mL). This solution was diluted with HCOOH 0.1 % to obtain the standard solution of 214 ng/µL.

Chromatogram layerHPTLC plates RP18 W F254 s, 10 x 10 cm (Merck) pre-washed by immersion in MeOH over night, dried in N2 stream under vacuum.

Note (editor): W stands for with water wettable layers, suited for application of aqueous samples.

Sample applicationBandwise with Linomat 5 on the two opposite plate sides resulting in 18 tracks, band length 7 mm, track distance 8.7 mm, distance from the edges 15 mm, application volume 1–5 µL for standard and 5 µL for sample solutions, delivery speed 60 nL/s.

ChromatographyIn the Horizontal Developing Chamber 10 x 10 cm with 8 mL MeOH – HCOOH 0.1% 2:2 (4 mL per side), migration distance 50 mm (development time 12 min).

DensitometryTLC Scanner 3 with winCATS software, absorption measurement at 282 nm, slit dimension 5 mm x 0.45 mm, scanning speed 20 mm/s, data resolution 50 µm/step, polynomial regression by peak area.

Results and discussionThe validation was a two-step strategy based on the accuracy profiles. The acceptance limit was set at 15 % according to the FDA guidelines for bio-analysis. In the pre-validation step five calibration points ranged 214–1071 ng/band were obtained in quadruplicate and repeated on three different days. Four regression functions were calculated: linear model, weighted linear (1/x) model, quadratic model and weighted (1/x) quadratic model. The mean bias, the repeatability and the intermediate precision were back-calculated for each level using the four regression models. The accuracy profiles obtained using the confidence intervals indicated the quad-ratic model as the best choice giving a dosing range index of 1.00 and a smaller bias.

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15a+b

A

B

As blank matrix being not available, the standard addition method was used with the interpolation approach. The standard addition curve, calculated with the quadratic regression function, coincided with the calibration curve obtained for the pure analyte in absence of matrix, assessing the validity of the calibration mode. Both determination coef-ficients were better than 0.999. Using 10 x 10 cm plates, three-point calibration curves (321, 642 and 1071 ng/band) were admitted for routine analysis after successful validation.

The validation standards for accuracy purpose were obtained by spiking a pre-analyzed hydrolysed sample with different standard concentrations. Recoveries were between 100.4 and 103.2 %. The method fulfilled the requirements, having bias largely inside the acceptance limits (95 %) and the relative standard deviation of repeatability and intermediate precision between 2.0 and 3.6 %. To test the method, the SDG content in flaxseed of five different cultivars was determined to be between 0.9 and 1.3 % with residual standard deviations (%RSD) of ≤ 2.3 % (n = 3).

Polynomial calibration curves of the three replicates

Accuracy profile of SDG obtained by the quadratic regression model: u confidence interval, l relative trueness

HPTLC densitograms at 282 nm of SDG standard (A) and flax-seed samples (B and C)

Further information is available on request from the author.*Prof. Silvia A. Coran, University of Florence, Faculty of Pharmacy, Department of Pharmaceutical Science, Via Ugo Schiff 6, 50019 Sesto Fiorentino (Florence), Italy, [email protected]

[1] S.A. Coran, V. Giannellini, M. Bambagiotti-Alberti, J Chro matogr A 1045 (2004) 217. [2] S.A. Coran, G. Bartolucci, M. Bambagiotti-Alberti, J Chro matogr A 1207 (2008) 155. [3] P. Hubert et al., J Pharm Biomed Anal 45 (2007) 82.

Polynomial calibration of SDG: (A) without matrix, (B) in matrix

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Planar Chromatography in Practice

Determination of aloe vera gel in cosmetics

Evamaria Kratz, Jürgen Geisser

The CVUA Karlsruhe* is one of the 4 Official Food Control and Animal Health Laboratories for the Fed-eral state of Baden-Württemberg in southern Ger-many. Its cosmetic team analyzes official samples that have been collected from retail outlets, regional manufactures and importers in order to verify their compliance with cosmetics regulations.

IntroductionThe gel from the inner part of the aloe vera leaves is traditionally used for skin care. In recent years, numerous cosmetic products have been launched where aloe vera extract was labelled as active in-gredient. Aloe vera is an expensive raw material, a fact which may tempt product producers to blend the gel with water and gelling agent, resulting in the dose in the final product being very low, despite promotional activity to the contrary. Aloe vera gel is also offered as concentrated raw material (e.g. 10-times or 200-times).

In the following, an investigation of aloe vera product is described in which aloe vera has been promoted through advertisement in such a way that it would be expected to contain at least 5 %. With a 5% concentration the assumed efficacy is supposed, for example an increase of skin moisture or special care effects. Aloverose was chosen as a marker compound for aloe vera addition. This acetylated polymannose (molecular weight 50– 500 kDa, approx. 1.1 acetyl groups per mannose

molecule) makes approx. 20 % of the approx. 0.5 % solids content of the fresh aloe vera gel and is therefore better suited for analytical monitoring than other ingredients like malic acid and glucose.

Up to now, only a 1H-NMR method was estab-lished for the aloe vera raw material, where aloverose is quantitated by the signals of its acetyl groups. With a newly developed HPTLC method it is possible for the first time to test whether cosmetic finished products containing aloe vera, match the expectation of the consumer and/or the statements of efficacy, or if it is a deception. The quantitation of aloe vera addition is carried out via mannose after hy-drolysis of aloverose. HPLC methods, which have been developed in the food industry for determination of sugars, turned out not to be suitable because of their insufficient limits of detection.

Standard solutionFor stock solutions, 20 mg aloverose are dissoluted in water and added to 20 mL; for glucose and galac-tose, 50 mg at 50 mL are used (can be stored deep-frozen for 1 year). Aloverose stock solution (0.8 mL) are hydrolyzed according to the sample solution and neutralized. For standard mixture solutions, each 1 mL glucose and 1 mL galactose stock solution are added to the hydrolyzed aloverose stock solution (0.8/100 mL and 1 mg/100 mL, respectively).

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Sample preparationDepending on the product, 1 to 5 g sample are homogenized with water. Lipophilic sample com-ponents are separated from the acidulated sample solution by solvent extraction with diethyl ether. Aloverose is degraded to mannose by hydrolysis with sulfuric acid (3.35 M, 3 h, 85 °C) and then neutralized. Some products contain hydrogen peroxide, which has to be destroyed by potassium iodide before hydrolysis.

LayerHPTLC plates silica gel 60 (Merck), 20 x 10 cm, im-pregnated by immersion in 0.5 M NaH2PO4 solution (immersion time 1 s, vertical speed 4 cm/s), pre-dry-ing at room temperature followed by drying on the TLC plate heater (5 min, 60 °C).

Sample applicationBandwise with Automatic TLC Sampler 4, 18 bands per plate, band length 6 mm, application volume 1–10 µL standard solution and, depending on the product, 1–15 µL sample solution, distance from the lower edge 10 mm, distance from the sides 12 mm, track distance 10 mm.

Application of the sample as rectangular area is recommended due to the high matrix load. This is enabeld by the ATS4 (see p. 15).

ChromatographyIn the flat bottom chamber 20 x 10 cm with 20 mL acetone – i-propanol – formic acid (0.1 M) 2:2:1, migration distance 80 mm (developing time approx. 75 min, double development for products with high glucose content is recommendable), drying of the plate on the TLC plate heater (5 min, 60 °C).

Note (editor): It is possible to achieve greater differences in adjacent zone distances using a development of >60 mm, however, this also leads to peak broadening.

Post-chromatographic derivatizationBy immersion of the plate (immersion time 1 s, ver-tical speed 4 cm/s) in 4-aminobenzoic acid reagent (1 g 4-aminobenzoic acid are dissolved in 36 mL pure acetic acid, then 40 mL water, 2 mL of 85 % phosphoric acid and 120 mL acetone are added) and heated on the TLC plate heater (10 min, 110 °C). This reagent is stable for 2 weeks if cooled and stored under nitrogen.

Comparison of the sample extract before and after hydrolysis

In some cosmetics’ formulation maltodextrin might be present, which increases the glucose concen-tration after hydrolysis. Thickening agents also containing mannose are assigned after hydrolysis by comparing the characteristic building blocks like glucuronic acid in xanthan (organic acids are deter-mined by a separate HPTLC method) and galactose in galactomannanes (guar gum or locust bean gum) and their amounts set in relation to mannose.

The limit of quantitation of aloe vera gel in prod-ucts is approx. 3 % which is sufficient for this ana-lytical task. The residual standard deviation of the polynomial calibration is 2.1 % for mannose ranged 8 – 80 ng/band and 4.0 % using matrix calibration.

DensitometryTLC Scanner 3 with winCATS software, fluorescence measurement with Hg lamp at 366 nm, evalutation via peak area with winCATS Planar Chromatography Manager.

Results and discussionAfter hydrolysis of aloverose mannose is well sepa-rated by HPTLC from the other carbohydrates (ex-cept fructose) in the sample. Derivatization of the mannose with 4-aminobenzoic acid forms a fluores-cent product, making detection more sensitive. The sample is compared before and after hydrolysis to find out, if mannose is a regular compound of the sample. If aloe vera is present, glucose as a natural compound of aloe vera gel can be detected before hydrolysis.

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Polynomial calibration (peak area) of mannose (from aloverose) ranged 8 – 80 ng/band

The new method enabled the cosmetic team at the CVUA Karlsruhe to verify the high aloe vera content in cosmetic finished products that had been pro-moted through advertisements. In the last two years several official complaints have led to improved diligence on the part of these producers to actually meet their label claims.

Further information is available on request from the authors.*J. Geisser und E. Kratz, Chemical and Veterinary Investigation Laboratory (CVUA), Weissenburger Str. 3, 76187 Karlsruhe, Germany, [email protected]

Area application with the Automatic TLC Sampler (ATS 4)

For determination of aloverose in cosmetic finished products, the high salt content present after the sample preparation and further constituents like tensides limit the sample volume for bandwise application. In such cases, area application of samples is ad-vantageous: Despite the high matrix loading the sample volume can be increased and the limit of quantification be lowered. Depending on the solvent, a subsequent focusing of the analytes is required.

Additionally, for larger, aqueous sample vol-umes, the ATS4 option with a heated spray nozzle (up to 60 °C) is recommended as it al-lows a considerably reduced application time.

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Key features:• Measurement of reflection, either in absorption or fluorescence mode• Object formats up to 200 x 200 mm• Spectral range 190–900 nm• Automatic start of all lamps: deuterium-, halogen-tungsten, and high pressure mercury lamp• Data step resolution 25–200 µm• Scanning speed 1–100 mm/s• Spectrum recording up to 100 mm/s• Automatic selection of electronic amplification• Rapid data transfer

More information: www.camag.com/tlc-scanner

CAMAG TLC Scanner with winCATS software is the most advanced workstation for densitometric evaluation of planar chromatograms.

Densitogram of antibiotics after their development

Calibration curve of sulfamethazine