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CRUDE DRUGS CONTAINING CARBOHYDRA TES AS ACTIVE COSTITUENTS

1. MACROSCOPICAL TESTS

Acaciae gummiAgarAlthaeae folium et radixFarfarae foliumLichen islandicusLini semenMalvae sylvestris flosPsyllii semenTiliae flosGummi arabicumTragacanthaTrigonellae foenugraeci semen

Maydis amylumOryzae amylumSolani amylumTritici amylumCichorii radixCyamopsidis semenGraminis rhizomaTaraxaci radix et foliumMelPlantaginis ovatae semenPlantaginis ovatae seminis tegumentumVerbasci flos

2. MICROSCOPICAL TESTS

Powdered drugs: Amylum maydisAmylum oryzaeAmylum solani

Amylum tritici

Cross section: Althaeae radix et foliumLini semen

Powdered preparation: Althaeae radix et foliumLini semenMalvae sylvestris flosPlantaginis lanceolatae foliumPlantaginis ovatae semenTiliae flosTrigonellae foenugraeci semen

3. CHEMICAL TESTS

3.1 Investigation of starches3.1.1 Identification of starches3.1.2. Tests for impurities3.2 Identification of inulin3.3 Mucilage3.4 Mel qualification

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4. QUANTITVE DETERMINAnON

4.1 Swelling value4.2 Enzymatic degradation of starch

1. MACROSCOPICAL TESTS

Amylum maydis - Maize starchZea mays L. Poaceae (Gramineae)Ph.Hg. VIII., Ph. Eur.

Amylum solani - Potato starchSolanum tuberosum L. SolanaceaePh.Hg. VIII., Ph.Eur.

Amylum tritici - Wheat starchTriticum aestivum L. Poaceae (Gramineae)Ph.Hg. VIII, Ph. Eur.

Amylum oryzae -Rice starchOriza sativa L. Poaceae (Gramineae)Ph.Eur.

Starches are white to pale creamish or greyish-white powders or irregular masses whichcrepitate when crushed: odourless and almost tasteless.

AIthaeae radix - Marshmallow RootAlthaea officinalis L. Malvaceae

Ph.Hg. VIII., Ph. Eur.

The root pieces are cylindrical, not ramified. The thicker pieces in commerce are split intwo. Theyare 10 to 30 cm long, 1 to 2 cm thi ck, white or yellowish white in colour, withbrown spots where root branches have been cut off. Bast fibres can be pulled off in finethreads from the root surface. When broken, the cortex is hardly dusting. The cortexbreaks in filamentary, the xylem in splintery form. The cross section is white, except forthe circular cambium, which is brownish yellow. Observed through a hand magnifier, themoistened cortex is annual and lamellar, the xylem radial.

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AIthaeae folium - Marshmallow LeafAlthaea officinalis L. Malvaceae

Ph.Hg. VIII.

Lini semen - LinseedLinum usitatissimum L. .Linaceae

Ph.Hg. VIII., Ph. Eur.

MaIvae foIium - Wild MaIlow LeafMalva neglecta Wallr.Malva silvestris L. Malvaceae

Ph.Hg. VIII.

The leaf has a short petiole, it is thi ck, on both surfaces denselycovered with velvety hairs: greyish green, silky.The lamina is ovate or cordate, with acuminate apex, obtusebase and irregulary crenated-dentate margin. The upper leavesthe are vaguely obtusely pinnated lobate, on the lower leaves the3 to 5 lobes be come more distinct with a centrallobe much longerthan the others.The leaf is plicate between the veins, its pinnatevenation strongly protrudes on the abaxial surface.

The linseed is 4 to 6 mm long, 2 to 3 mm wide, l to 1.5 mm thick, fiat, ovate, light or dark brown, smootb, shiny, rounded-doffon one end and acute onother. At the acute end a sarcocarpicsmall cauncle, somewhat lower the hilum of lighter colour. Thehand magnifier shows a slightly uneven surface.The seed-coat is rigid, fragile, when macerated in water, itbecomes slippery due to swelling of the mucilaginousepidermalcells,. And is covered with a thick mucilage layer.White albumen, greenish white embryo, both oleaginous.Odourless, taste, mild oily, mucilaginous

Simple granules, approximately 5 to 30 nm indiameter, polyhedral to subspherical with acentral hilum occurring as an irregular sp lit or,more usually, as a cleft with three to five rays.Striations arenot visible.

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MaIvae sylvestris flos - Wild MaIlow FlowerMalva silvestris L. Malvaceae

Ph.Hg. VIII.

The drug consist of the pinkish violet flower. Radially zygomorphous hermaphrodite,pentemerous flower sitting in groups of 2 to 6 in the axil of the leaves. Double calyx.External 3 free sepals 4 to 5 mm long, oblong-Ianceolate, glabrous inside, setoselyciliate at the margin, mostly pilose outside. The 5 internal sepals are gamosepalous upto 2/3 of their lengh, about 6 mm long, lacinia triangular, pilose free, obovatetapered, at the base densely long-ciliate, otherwise very short-pilose, deeply and broadlyemarginate, blue colour, 3 dark longitudinal striae.Nomerous stamina, columnar prominent filaments grown together to a 10 to 12 mmlong, cylindrical reddish tube (monadelphous). Free, reniform uniseptate anthers. Whitepollen. The base of petals and the tube of filaments are grown together and fan offtogether after deflorescense. FIat disciform pistil, dinted above, with 9 to 10 lateral sulciáccording to the carpels. Filose styles, grown together at the base; stigmata reddish,filose.Odourless: taste, mucilaginous, when masticated.

Graminis rhizoma - Couch-grass (Quack grass Roots)Agropyron repens L. Poaceae (Gramineae)

Ph.Hg.VIII.

The drug consists of the numerous branched, wide-creeping, sweet-tasting rhizomes ofthe perennial grass. Active ingredients: triticin (polysaccharide), mucilage, traces ofessential Dit, silicic acid, saponin.

Taraxaci radix - Dandelion RootTaraxacum officinale Web, Asteraceae (Compositae)

Root and rhizome yielding the drug are 15 to 20 cm long and 1 to 2 cm thick. Reddishbrown outside, greyish white inside. On the cross-section of the root softened in waternumerous wide concentricai belts in the cortex, readly visible to the naked eye. Xylemyellowish ad hardly radial structure. The transversaIly annular rhizome has severalheads. It continues in the main root, which is lengtwise wrinkled, striated and slightlyramified only. Even not farinaceous fracture.

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Farfarae folium - CoItsfoot LeavesTussilago farfara L. Asteraceae (Compositae)

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Lichen islandicus - Iceland MossCetr'aria islandica L. (Ach) Parmeliaceae

The thaIlus is strap-like, deeply divided, shrubby and forms entagled mats, 1-15 cmhigh, only loosely attached to the substratum. The lobes are thin, either curled inwardsalmost into tubes of fiat, shilling chestnut-brown on the upper surf ace and lighter on thelower; the margins comewhat incised and ciliate.

Salep tuber - Orchid tuberOrchis morio L. Orchidaceae

The drug consist ofthe subglobular to ovoid tubers of the perennial herb.

Agar - AgarGelidium speciesAhnfeltia plicata (Huds.) Fries Rhodophyta

Ph.Hg.VIII., Ph. Eur.Greyish white or brownish yellow, translucent strips or bands, usually 0.1 to 0.3 mm thi ck, 3 to 4mm broad. Odourless and tasteless mass of bands, which swells in water to form ajelly.

Acaciae gummi - Arabic gumAcacia senegal Willd. Mimosaceae

Ph.Hg.VIII., Ph. Eur.

The drug consists of the gummy exsudation of the stem and branches of Acacia senegatindigenaus mainly in Cordovan, Sudan and in other parts of tropic Aftica. Odourless;tasteless. Rarely colourless, mosdJ yellowish, the spehrical pieces of acacia are pea- orhazelnut-sized. Being cracked, they are rarely transparent. Generally hard and ftagile.Fracture conchoidal, when ftesh of a glassy, sometimes iridescent surface. Dry it at atemperature not exceeding 300 C for powdering. The power is white or yellowish white.

The drug consist of basal, leaves, which are 8-30 cmwide, almost circular in out line but polygonal, with up to12 acute lobes. Whitish-tomerntose on boot, late onlyon the lower surface

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Tragacantha - Tragacanth gumAstragaIus species Fabaceae

Ph.Hg.VIII., Ph. Eur.

FIat, greyish white ho'm-like, sometimes transceIucent and slightly yellowish plates,incurved in crest or crescent shape, about 5 mm wide and 1 to 3 mm thick. Semicircular,sinuous layers on their surface.

2. MICROSCOPICAL TESTS

Starches

White to pale creamish or greyish-white powders or irregular masses which crepitatewhen crushed; odourless and almost tasteless.Many crystalline substances show brillant colours when examined in polarised light.Starch grains often show a black cross, a phenomenon due to the crystalline refractionof the material. Polarised light is usefui for the detectiori of calcium oxalate, especiallywhen only small quantities are present in the tissues under examination. It appearsbright on a black background.

Maize starch - Amylum maydis

Simple granules, approximately 5 to 30 nm in diameter, polyhedral to susbpherical with a centralhilum occuring as an irregular split or, more usually, as a cleft with three to fiye rays. Striationsaré not visible.

Potato starch - Amylum solani

The granules are mostly simple with occasianal compound granules having two or threecomponents; they show great variation in size, the larger granules measuring up toapproximately 100 um in length. Individual granules are ovoid to subspherical andffequently show tuberosities; they have an eccentric point hilum which is situated nearthe narrower end in ovoid granules. Most ofthe granules show well-marked concentricstriations.Wheat starch - Amylum tritici

Mainly simple granules of two distinct size ranges; the larger granules measureapproximately 25 to 45 um in diameter and the small er ones measure approximately 3to 15 um in diameter; a few granules intermediate in size are also found. A smallnumber of compound granules with two or three components are also present. Individualgranules are lenticular and they appear oval, circular or biconvex in outline, dependingon their orientation. The central point hilum appears as a line when the granules areseen in edge view. Faint concentric striations are visible in some ofthe larger granules.

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Rice starch - Amylum oryzae

Simple granules or aggregations from compound granules; individual granules areapproximately 2 to 10 ulI} in diameter, polyhedral or subspherical. A small central pointhilum is visible in a few of the granules; there are no striations.

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Althaeae folium

Cross-section. The structure of the le af is dorsiventral. The stellate trichomes of bothepidermises are composed of as many epidermal cells as they have rays. The basalpart of every trichome branch has aq sclereid-like thiekened wall. The stocky glandulartrichomes are composed of a short hasal (stem) part and of a multicellular vertcillategland bead. Some of the epidermal cells are larger and contain mucilage. The columnedparenchyma has sometimes two layers. In the spongy parenchyma sometimes. Thereare larger mucilage cells as weIl as cells with c1ub-chaped calcium oxalate crystals. Thevascular bundle is collateral.

Althaeae radix

Cross-section. Part of the "external c011ex" is usually found outside. In the "internalc011ex" there are medullary rays of 1 to 2 cell width, hard and seft phloem partsaltenating layers. The hast fibres of the hard pholem are free of lignin 'or but slightlylignified, sometimes with a bifurcated tip. The soft phloem consists mainly of bastparenchyma, with sporadic cells containing mucilage or club-shaped calcium oxalatecrystals and with somewhat compressed bundles of bast sieve tubes.In the xylem, the medullary rays are also mostly two cells broad. The xylem rays aremostly filled up with parenchymatous cells and sometimes with xylem fibres. Thetracheae and tracheids are arranged in small groups, with a major vascular group to befound only in theroot. Both in the cortex and in the xylem, club-shaped calcium oxalate crystals and lotsof starch are to be found. The starch grains are simple, generally 3 to 5 um in length,spherical, irregularly ovular or reniform. There are many mucilage cells also in thecorticai and xylem parenchyma. They are larger in size and have stratified mucilaginouswalls.

Powder test. The drug powder is white. Under the microscope, parechyma portionsfilled with starch and grains can be öbserved. The latter are various in shape (spherical,ovular, reniform etc.) There is often a longitudinal fissure on them. The powder containscolourless, largecavemed fibres, singly or in bundles, as weH as vessei fragments, club-shaped calcium oxalate crystals, colourless mucilage cells an small mucilage lumps. Nosuberine parts can be seen.

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Lini semen

Cross-section. In cross-section five layers of the seed coat. Epidermis radially somewhatelongated, the tangential walls of its cells very thi ck, stratified and mucilaginous.Celllumina mosdJ not recognizable. The hypoderma consists of a so call ed annularlayer of 2 to 3 rows offiat cells, whit small intercellularies between them. Further inside, a layer of sclereids,consisting of 120 to 190 um long and 8 to 15 um wide elements, with thi ck, lignified,simply pitted walls. Under the sclereids, severallayers of tangentially elongated, fIatenedtransversal cells. The innermost pigment layer ofthe seed.coat consists of a single rowof square, reddish brown cells of pitted walls and containing phlobaphene.Under the pigment layer 3 to 7 cell rows endosperm, with polyhedral thinwalled cellscontaining numerous ale_ron granules and fixed oil drops. The thinwalled cells of theembryo contain fix ed oil and heterogeneous aleuron granules of up to 20 um size,consisting of a globoid and one or more crystalloids. Palisade layer and the bundleprimordia readily recognizable in the two cotyledons.

Linseed - longitudinal section

1. seed coats2. endosperm3. cotyledon

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3. CHEMICAL INVESTIGA TIONS

3.1 Investigations of starch

3.2.1. Identification of starches

Boi! 1 g of drug with 50 ml of water: after cooling it becomes a translucent, odourlessstarch jelly.

Shake 10 mg of drug with 5 ml of hot water. Add 1 drop of 0.01 N iodine solution to theliquid, it will tum blue. .

The colour disappears from heating or if R- sodium hydroxide is added, but reappears atcool ing, or if acidified by R-hydrochloric acid.

\ /

Amylose

Amylopectin

3.1.2 Quantitative tests

Soluble starch. Shake 1 g in 10 ml of cold water and fitter. Add to filtrate one drop of 0.1N iodine solution. The filtrate may tum yellow or reddish, but must not tum blue.

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3.3 Mucilage

Althaeae radix Tiliae flos

Make 5% suspension from 2.5 g of crude drug with 50 ml water, left to extract on 20 oC,and mix a few times. Filtrate on millI, squeeze out the moisture. Centrifuge for 10 minute(4500/ min) due to eliminate starehes. (The starches take place on the bottom ofcentrifuge tube). For testing succesfull elimination of starches may add Lugol-solutionAdd 4x quantity of etil-*alkohol to the mucilage solution during mixing it. The extractedmucilage precipitates. Centrifuge the mixture, then dry mucilage on 60°,C

3.4 AduIteration of honey by artificial invert sugar

It can be examined by detecting furfurol, which gives a red colour with resorcinol inhydrochloric acid. It has to be noted that certain amount of furfurol may be formed ingenine honey by prolonged heating or lengthy storage

5 g of honey is carefully mixed with lOg of chloroform in a porcelan mostar. The mixtureis filtrered and the chloroformic phase is evaporeted in a separate porcelan disk. To theresidue a few drops of fteshly prepared resorsinol solution is added ( 1 % resorcin in cc.HCL) The colour is pinkish or light orange for a short time, but cant be red for longerperiod of time.

4. QUANTITY DETERMINA TIONS

4.1 Determination of SwelIing Value

Agar-agarAlthaeae radixAlthaeae foliumFarfarae foliumLini placentae farinaLini semenPsylii semen

SweIling value is the sweUing of 1 g air-dry drug in water or in the different liquidsspecified by the monographs, observed at room temperature after 4 hours, related todried drug, expressed in ml.Moisten the prescribed quantity of air-dry drug comminuted to the fineness specified bythe monographs with the specified moistening liquor (acetone, alcohol) in a 25 ml glass-stoppered volumetric cylinder graduated to 0.2 ml, where the graduation ranging from Oto 25 ml is 10 to 12 cm in length. Shake up the fluid thoroughly with 25 ml of water orwith the liquid specified for the different drugs. Agitate the mixture every 10 minutes foran hour and then maintain for 4 hours at room temperature. Read off the volume of thedrug in ml together with any adhering mucilage. Calculate the mean value of at least twosimultaneous tests related to 1 g of drug dried.

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Drug (g) Moistening liquor (ml) Swelling valueAgar-agar 1.0 -Althaeae folium 1.0 Aceton 2.0Althaeae radix 0.5 Aceton 1.0Farfarae folium 1.0 Aceton 1.0 .Lini placentae farina 1.0 Aceton 1.0Lini semen 1.0 -

Psvllii semen 1.0 Aceton 2.0

4.2 Acidity of starches

Shake a 20 g sampie with 100m1 of freshly boiled and cooled water. Titrate the mixturewith 0.1 N sodium hydroxide solution, using I-phenolphtalein solution as indicator. Nearto the end point, add a few more drops of the indicator.