NGHIN CU CHIT TCH V XC NH THNH PHN AXIT HU C TRONG L CY SNG I

A STUDY ON THE EXTRACTION AND DETERMINATION OF ORGANIC ACIDSIN LEAVE OF KALANCHOE PINNATA (LAMK.) PERS.SVTH: Phm Th Bch Lin

Lp 07SHH, Khoa Ho, Trng i hc S Phm, i hc Nng

GVTH: GS. TS o Hng Cng

Khoa Ho, Trng i hc S Phm, i hc Nng

TM TT

Bi bo co ny trnh by cc kt qu nghin cu cc i lng vt l nh m, hm lng tro, hm lng kim loi nng v xy dng iu kin ti u qu trnh chit tch axit bng phng php chng ninh v chit soxhlet. Dch chit axit c este ho, kim tra v xc nh thnh phn bng ph hng ngoi (IR) v sc k kh ghp khi ph (GC-MS).ABSTRACT

This report presents the result of physical quantities such as moisture, ash, content of heavy metals and building best conditions for acids extraction process by the method of distillation and soxhlet extraction. Acid extracts are esterified, checked and determined the composition by infra-red (IR) and gas chromatography pair mass spectrometry (GC-MS).1. t vn [3], [5]

Cy sng i, tn khoa hc l Kalanchoe pinnata (Lamk.) Pers., hay cn gi l cy thuc bng, trng sinh, dip sinh cn, bt t..., va l cy cnh, va l mt cy thuc c s dng t lu i trong y hc c truyn khng ch Vit Nam m c trn th gii. N c cng nng tiu thng, gim au, sinh c v cc cng dng nh khng khun, c ch min dch, tiu vim, cha bng, lm lnh cc vt thng, l lot, vim ty, au mt, chy mu, bo v gan thn, an thn, chng tc nhn gy t bin, lm thuc gii c.Externally, the pulp of the leaves or the juice is applied on traumatic injuries to arrest the bleeding as it contract the minute arterioles and promote the healing of wounds.The herb is highly recommended in bleeding disorders, piles and menorrhagia.

Bi bo co ny cng b mt s kt qu bc u nghin cu v l cy sng i nhm ng gp vo ngun t liu v thnh phn axit trong l cy sng i v gp phn pht trin nhng tc dng cha bnh tuyt vi ca n.

2. Nguyn liu v phng php nghin cu 2.1. Nguyn liu, ho cht, thit b

Nguyn liu l l cy sng i c hi phng Ho Hi, Ng Hnh Sn, TP Nng. L cy sng i c loi b l h, ho, ra sch, mt phn ti s dng cho phng php chng ninh, phn cn li hong kh t nhin, sau xay thnh bt, bo qun trong bnh ht m s dng cho phng php chit soxhlet.

Ho cht: Cn 960, axeton, metanol, ietylete, metyl iodua, NaOH 0,01N, phenolphtalein, HCl, tinh th KI, Na2SO4 khan, than hot tnh, nc ct.

Thit b: T sy, l nung, b dng c chng ninh, b chit soxlet, phu chit, cn phn tch, my quang ph hp th nguyn t (AAS), my o ph hng ngoi (IR), my sc k kh ghp khi ph (GC-MS) v cc dng c th nghim n gin.2.2. Cc phng php nghin cu [1]

Bi nghin cu ny s dng cc phng php phn tch c in nh phng php trng lng, phng php chng ninh, chit soxhlet, phng php chun (TCVN 4589-88) kt hp vi cc phng php phn tch hin i nh quang ph hp th nguyn t (AAS), quang ph hng ngoi (IR), sc k kh ghp khi ph (GC-MS).

3. Kt qu v tho lun

3.1. Xc nh mt s i lng vt l

Da vo phng php trng lng, xc nh c m v hm lng tro trong l cy sng i, kt qu nh sau (bng 1 v bng 2)

Bng 1. Kt qu xc nh m ca l ti v m tng i ca nguyn liu bt l cy sng i

MuSTTm1 (gam)m2 (gam)m3 (gam) (%)tb (%)

L ti1103,686,01104,1991,5191,51

2104,076,00104,5891,50

3106,376,02106,8891,53

Bt l kh4108,036,00113,1115,3315,33

5105,266,01110,3515,25

6102,356,02117,4415,41

Trong m1: Khi lng chn s m2: Khi lng mu trc sy

m3: Khi lng chn s v mu sau khi sy

: m ca mi mu TB: m trung bnh.

Nhn xt: m l cy sng i ti l 91,510,1%, m tng i nguyn liu bt l 15,33 0,053%.

Bng 2. Kt qu xc nh hm lng tro trong l cy sng i ti

TTm1 (gam)m2 (gam)m3 (gam)m4 (gam)mtro (gam)H(%)Htb(%)

151,78456,8095,02551,8390,0551,0951,099

251,75756,8075,05051,8120,0551,089

347,25552,2815,02647,3110,0561,114

Trong m0: khi lng cc m1: khi lng cc v mu trc khi tro ho

m3: khi lng mu m4: khi lng cc v mu trc sau tro ho H : hm lng tro trong l cy sng i

Nhn xt: Hm lng tro trung bnh ca l cy sng i ti l 1,099 0,01% .3.2. Xc nh hm lng kim loi nng

Da vo phng php o ph hp th nguyn t (AAS), xc nh c hm lng mt s kim loi nng, kt qu c th hin nh sau (bng 3)

Bng 3. Kt qu xc nh hm lng kim loi nng trong l cy sng i

TTTn

kim loiPhng php th (AAS)Kt qu

(mg/l)Kt qu

(mg/kg)Tiu chun CODEX STAN

(mg/kg)[6]Hm lng cho php

(mg/kg) [4]

1PbTCVN 6626: 20000,05192,5820,32

2CuTCVN 6626: 20000,03331,6575,030

3ZnTCVN 6626: 20000,10945,4435,040

4AsTCVN 6193:19960,00370,1840,21

Nhn xt: Theo Quyt nh s 99/2008/Q-BNN ca B Nng nghip ngy 15/10/2008 v vic ban hnh quy nh qun l sn xut, kinh doanh rau, qu v ch an ton [4] th hm lng kim loi Cu, Zn, As nm trong khong cho php, ring Pb hi cao hn mc cho php.

3.3. Kho st yu t t l rn/lng (R/L) v thi gian chit nh hng n tng lng axit hu c trong phng php chng ninh p sut thng vi dung mi nc Cn khong 10 g l sng i ti, chng ninh vi nc p sut thng vi th tch nc ln lt l 100, 200, 300 ml trong cc thi gian 4, 6, 8, 10 gi, kt qu th hin hnh 1 Nhn xt: Tng lng axit thu c ln nht khi chng ninh vi t l R/L 10gam nguyn liu/200ml nc v thi gian chit l 6 gi, th tch dd NaOH 0,01N trung ho axit trong 5ml dch chit l 30,83 ml.

Hnh 1. th s ph thuc ca tng lng axit vo t l R/L v thi gian chit trong phng php chng ninh

3.4. Kim tra dch chit chng ninh bng ph hng ngoi (IR)

Hnh 2. Ph IR dch chit l sng i ti

Nhn xt: Ph hng ngoi hnh 2 xut hin cc pic v tr 3397,6 cm-1 v 1726,7 cm-1 ln lt l tn s c trng ca nhm OH, -C=O do c th kt lun dch chit l sng i ti chng ninh trong nc c cc axit hu c3.5. Kho st yu t dung mi v thi gian chit nh hng n tng lng axit hu c trong phng php chit soxhlet

Cn khong 10 g bt l sng i kh, chit soxhlet vi cc dung mi cn 960, axeton, metanol trong cc thi gian 6, 8, 10, 12, 14, 16 gi, kt qu chit th hin hnh 3Nhn xt: Tng lng axit thu c cao nht khi chit soxhlet vi dung mi cn 960 v thi gian chit l 14 gi, th tch dd NaOH 0,01N cn trung ho axit trong 5ml dch chit l 26,6 ml.

Hnh 3. th s ph thuc ca tng lng axit vo dung mi v thi gian chit trong phng php chit soxhlet

3.6. Este ho axit hu c [2]

Dch chit axit trong cn 960 c ty mu bng than hot tnh, kim ho bng dung dch NaOH 0,1N. C cn ui bt dung mi, tin hnh este ho bng cch thm vo dung dch mui tinh th KI, cho tip CH3I + CH3OH vo, lc mnh cho hn hp phn ng. Este c chit li 2 ln bng ietylete, ui bt ietylete. Lm khan bng Na2SO4 khan thu c este trong ietylete. Lu gi este chy sc k kh ghp khi ph (GC-MS).

3.7. Xc nh thnh phn bng phng php sc k kh ghp khi ph (GC-MS)

Kt qu nh danh thnh phn axit trong l cy sng i sau khi este ho dch chit bng phng php GC-MS c th hin bng 4

T kt qu bng 4, ta nh danh dc 14 cu t, trong thnh phn axit trong l cy sng i l axit cinamic, axit stearic, axit aipic, axit hexadecenoic, axit octadecanoic v mt loi hp cht c hot tnh sinh hc rt qu l Lupeol trong l cy sng i.4. Kt lun

- Cc tnh cht vt l: m ca l cy sng i ti l 91,510,1%, m tng i ca nguyn liu bt l 15,330,053%, hm lng cc kim loi nng nm trong khong cho php theo quy nh ca B Nng nghip.

- iu kin chit tch ti u: Phng php chng ninh vi t l R/L 10 gam nguyn liu/200ml nc, thi gian chit 6 gi v phng php chit soxhlet vi dung mi cn 960 , thi gian chit 14 gi.

- Kim tra dch chit axit bng ph hng ngoi chng t trong dch chit c axit hu c

- Xc nh mt s axit hu c v cc thnh phn khc trong l cy sng i bng phng php GC-MS l axit cinamic, axit stearic, axit aipic, axit hexadecenoic, axit octadecanoic v mt loi hp cht c hot tnh sinh hc rt qu l Lupeol trong l cy sng i bng phng php GC-MS.TI LIU THAM KHO

[1] Hong Minh Chu, T Vn Mc, T Vng Nghi (2002), C s ho hc phn tch, Nh xut bn Khoa hc v K thut, H Ni.

[2] Tt Li (2004), Nhng cy thuc v v thuc Vit Nam, Nh xut bn Y hc, H Ni[3] Phan Tng Sn, L ng Doanh (1977), Thc hnh ho hc hu c, tp 1,2, Nh xut bn Khoa hc v k thut, H Ni.[4] Quyt nh s 99/2008/Q-BNN ca B Nng nghip ngy 15/10/2008 v vic ban hnh quy nh qun l sn xut, kinh doanh rau, qu v ch an ton.

[5] Anjoo Kamboj, Ajay Kumar Saluja (2009), Bryophyllium pinnatum (Lam.) Kurz: Phytochemical and parmacological profile, Pharmacognosy Review, 364-374. [6] Codex Stan 164-189- General Standard for fruit juices preserved exclusively by physical means not covered by individual stands (world-wide standard).

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