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TAP CH PHAT TRIEN KH&CN, TAP 12, SO 07 - 2009

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NGHIN CU SDNG THIT B SOXHLET-VI SNG LY TRCH MTS HP CHT THIN NHIN

Phm Thnh Lc, L Ngc ThchTrng i hc Khoa hc T nhin, HQG-HCM

(Bi nhn ngy 02 thng 11 nm 2008, hon chnh sa cha ngy 10 thng 03 nm 2009)

TM TT:L vi sng gia dngc chuyn i thnh thit b ly trch Soxhlet-Vi sng,sdng vo vic ly trch hp cht thin nhin. Vic nghin cu sdngc thc hin trn: -cafein t bp tr, Camellia sinensis L.; - steviosid t c ngt, Stevia rebaudiana (Bert.)Hemsl; - artermisinin t hoa thanh hao hoa vng, Artemisia annua L.; - rutin t hoa he,Sophora japonica L.; - tinh du tri i hi, Illicium verum Hook. f.; - tinh du ht th l,Anethum graveolens L.. Cc sly trch ni trn cngc thc hin song song trn h thngSoxhletun nng truyn thng. Sso snh hai phng php kch hotc thc hin da trnthi gian, hiu sut v phm cht ca sn phm ly trch.

T kha: H thng ly trch Soxhlet-Vi sng, ly trch hp cht thin nhin, Camelliasinensis, Stevia rebaudiana, Artemisia annua, Sophora japonica, Illicium verum, Anethumgraveolens.

1. T VN L vi sng do Percy Spencer pht minh u tin nm 1947.[1] Tuy nhin, mi n nm

1978 Michael J. Collin mi thit k l vi sng u tin p dng cho phng th nghim phntch.[2] Sau hng lot thit b vi sng c pht minh phc v vo nghin cu cng nhphc v sn xut cng nghip.[3-9]

Vic p dng nng lng vi sng h tr thc hin phn ng ha hc v ly trch hp chtthin nhin hin ang rt c quan tm.[10] Cc thit b vi sng chuyn dng rt t tin nnvic trang b cc loi thit b ny khng n gin i vi cc phng th nghim Vit Nam.Trong iu kin , l vi sng gia dng tr thnh la chn u tin v chi ph trang b vchuyn i cng nng thp. Hin nay nhiu phng th nghim Vit Nam bt u a l visng vo phc v cho nghin cu, tuy nhin ch mt vi phng th nghim tham gia ci tin lvi sng gia dng thnh nhng thit b chuyn dng phc v cho nhng mc ch nghin cu

chuyn ngnh.Trn c s nghin cu chuyn i l vi sng gia dng thnh thit b ly trch hp chtthin nhin v thc hin tng hp hu c[11] nhm nghin cu v Ha hc Xanh tip tcnghin cu chuyn i l vi sng gia dng thnh thit b Soxhlet-chiu x vi sng. Bi bo nytrnh by kt qu thu c khi s dng thit b ni trn vo vic ly trch mt s nguyn liuthc vt xc nh kh nng v tm cch ci tin hot ng ca thit b ny.

2. THC NGHIM

2.1. Nguyn liuVic ly trch c thc hin trn cc i tng thu mua ti nhng a phng nht nh:- Bp Tr long (Cng ty Tr Tm Chu, Bo Lc, Lm ng).- Phn trn mt t ca cy C ngt (Lm ng)- Hoa Thanh hao hoa vng (TrungQuc)

- Hoa He (Hip Thnh Dc Hng, Qun 6, Tp H Ch Minh).- Tri i hi (Cao Bng).- Ht Th l (Thi Bnh).


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Science & Technology Development, Vol 12, No.07 - 2009

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2.2. Ly trch: Ly trch kit trong nhng iu kin (lng nguyn liu, th tch dung mi)nh nhau, song song trn hai thit b ly trch Soxhlet-un nng cin (A) (Ph lc 1) vSoxhlet-chiu x vi sng (B) (Ph lc 2).

2.2.1. Thc nghim ly trch trn th it b ly trch Soxhlet-chiu x vi sng:Cc mu cyc khi lng (20 g) v 500 mL dung mi c np vo h thng (B). u tin, un bnh chadung mi cho n khi si. Hi dung mi ngng t ri xung phn cha nguyn liu. Khi

ng s chiu x vi sng. Ngng chiu x khi nhn thy dung mi bt u mun si. Lp ilp li thao tc trn cho n khi dung mi bt u quay v bnh cha dung mi th khng chiux na. Sau , chn khi dung mi ngng t, trong ln k tip, ri xung phn cha nguynliu. Lp li cc thao tc nh trn cho n khi s trch kit c xc nh. Thi gian chiu xchung l tng s cc khong thi gian chiu x ngt khong.

Sau khi thu hi dung mi, tt c cc loi cao (cao 1) thu t hai phng php ly trch A vBc x l hon ton ging nhau c c sn phm th (cao 2) t yu cu phn tch.

Vic iu ch cao 2 t cao 1 c thc hin theo cc quy trnh ring:2.2.2. Ly trch caf ein t l tr:[12] Cao 1 c ho tan hon ton vo 100 mL nc ct,

un si nh, thm t t 1 g Ca(OH)2, tip tc un si nh trong 1 pht. ngui n nhit phng, lc qua Bchner, c dng 1 g bt trlc. Dung dch qua lc, c ly trch bng CHCl3(7 x 20 mL). Ra dung dch ly trch vi 15 mL nc ct. Nc ra c ly trch li bngCHCl3 (3 x 15 mL). Gp tt c cc dung dch CHCl3 li, lm khan. Lc, c quay thu hi dung

mi, xc nh khi lng cao 2.2.2.3. L y trch steviosid tphn trn mtt ca cy c ngt: [13]Cao 1c ho tan vo

50 mL nc ct, thm 50 mL dung dch Na2SO4 bo ha, lc u. Ly trch bng n-butanol (10x 50 mL), dung dch ly trch c ra bng nc ct (3 x 20 mL). Nc ra c ly trch libng n-butanol (3 x 20 mL). Gom tt c dung dch ly trch li, lm khan. Lc, thu hi dungmi, xc nh khi lngcao 2.

2.2.4. Ly trch ar termisini n thoa cy thanh hao hoa vng: [14]Cao 1 c ho tan vo20 mL eter du ho, ly trch bng dung dch etanol : nc c t l 1 :1 (10 x 20 mL). Thu cdung dch mu trng sa. C quay, xc nh khi lngcao 2.

2.2.5. Ly t rch ruti n thoa ho: [15]Cao 1 c ho tan vo 200 mL etanol nng, un nhn khi dung dch bt u kt tinh. ngui n nhit phng. yn 24 gi rutin kttinh hon ton. Lc qua Bchner, sn phm th c ra bng eter du ho lnh cho n khinc ra khng cn mu xanh th dng li. kh t nhin n khi lng khng i, xcnh khi lng cao 2.

2.2.6. Ly trch t inh du tht th lvttrii hi: [16,17,18]Cao 1(nha du) c hotan vo etanol. Lm lnh trong 2 gi. Lc nhanh qua h thng phiu lc lnh. C quay thu hidung mi. Xc nh khi lng cao 2(tinh du).

2.3. Xc nh hm lng cu phn chnhHm lng cc cu phn chnh (%) trong cao 2 c cung cp t kt qu ca cc phng

php phn tch HPLC/UV, HPLC/MS/MS, GC/MS.2.3.1.GC/MS: Trn my QP2010. Ct mao qun MDN-5S1: 0.25 mm x 30 m x 0,25 m.

Chng trnh nhit: Nhit u 60 oC gi 4 pht, tng 2 oC/pht cho n 80 oC sau tng 5oC/pht n 180 oC gi 6 pht, tng 10 oC n 200 oC gi 5 pht.

2.3.2.HPLC/UV:

- nh lng cafein: Trn my Shimadzu LC 10A. di sng 276 nm. Dung miacetonitril:H2O (0.05 % H3PO4) l 15:85. Ct C18(250 mm x 4.6 mm). Tc dng: 0.8ml/pht.


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- nh lng rutin: Trn my Shimadzu LC 1100. di sng 254 nm. Dung miMeOH:H2O l 4:6. Ct C18 (250 mm x 2.0 mm). Tc dng: 0.2 ml/pht.

2.3.3.HPLC/MS/MS:

- nh lng steviosid: Trn my Themo Quantum Access. p sut u ct: 10 bar. Dungmi acetonitril (0.1 % HCOOH):H2O (0.1 % HCOOH) l 65:35. Ct C18 (250 mm x 4.6 mm).Tc dng: 400 l/pht. nh lng theo ion c trng c m/z= 664.3-665.3.

- nh lng artermisinin: Trn my Themo Quantum Access. p sut u ct: 10 bar.Dung mi MeOH (0.1 % HCOOH):H2O(0.1 % HCOOH) l 9:1. Ct C18 (250 mm x 4.6 mm).Tc dng: 500 l/pht. nh lng theo ion c trng m/z= 246.4-247.4

2.4. Hiu sut cc ln ly trch c xc nh nh sau:

Hieu suat cao 1 =Khoi lng cao 1

Khoi lng nguyen lieux 100

Hieu suat cao 2 =Khoi lng cao 2

Khoi lng nguyen lieux 100

Khoi lng cau phan chnh = Khoi lng cao 2 x Ham lng cau phan chnh (*)

(*) Khi lng cu phn chnh l khi lng l thuyt ca cu phn chnh trong cao 2 datheo kt qu phn tch.

3. KT QU V THO LUN

3.1. Xc nh cng sut chiu x

Cng sut chiu x thch hp cho mi nguyn liu v dung mi tng ng l cng suttha iu kin: Cho hiu sut ly trch cao, dung mi ly trch ti bu ly trch khng bun siqu nhanh khi chiu x.

tm cng sut chiu x thch hp cho tng loi nguyn liu v dung mi, u tin thigian ly trch c cnh l 30 pht. Chiu x vi sng cc cng sut khc nhau t thp ncao. Ngng chiu x, thu hi dung mi, cn cao 1, xc nh hiu sut.

Bng 1. Kt qu kho st hiu sut ly trch theo cng sut chiu x, trong 30 pht.

Hiu sut (%)

Bp tr C ngt Hoa heHoa thanh

hao hoa vng Tri i hi Ht th lCng sut(W)

H2O H2O EtOH Eter du ha60-80 oC

Eter du ha30-60 oC

Eter du ha30-60 oC

80 10.36 8.06 15.42 1.81 10.27 5.76

150 13.02 13.43 19.54 2.19 11.20 6.05

300 16.65 15.65 21.31 2.93 (*) (*)

450 19.19 19.70 23.56 (*) - -

750 19.95 20.36 (*) - - -

900 20.72 20.74 - - - -

(*): Khng kho st tip v dung mi si qu nhanh khi tin hnh chiu x.


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V th biu din v chn cng sut ph hp.

th 1. Hiu sut cao 1 theo cng sut chiu x

3.2. So snh kt qu ly trch trn hai thit b ly trch Soxhlet-un nng cin vSoxhlet-chiu x vi sng

Chng ti thc hin vic ly trch kit cc loi nguyn liu nu trn vi 2 phng php (A)v (B). Kt qu ghi trong Bng 2.

th 2. So snh thi gian v khi lng cu phn chnh khi p dng phng php ly trch (A) v (B)


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th 3. So snh thi gian v khi lng cu phn chnh khi p dng phng php (A) v (B) ly trchsteviosid v artermisinin (khng thy r th 2)

Kt qu th 2 v 3 cho thy khi ly trch kit cc hp cht thin nhin bng thit b lytrch Soxhlet-chiu x vi sng kt qu thu c nhanh 12-16 ln hn so vi ly trch kit bngthit b ly trch Soxhlet-un nng cin.

Khi lng cao 1 v cao 2 thu c bng thit b ly trch Soxhlet-chiu x vi sng cngcao hn, iu chng t h thng ny ly trch c nhiu sn phm hn phng phpSoxhlet un nng cin khi p dng trch kit trn cng khi lng nguyn liu v dungmi.

Trong trng hp artermisinin, hm lng cu phn chnh trong phng php (B) cao hnphng php (A) v hiu sut cao 2 phng php (A) li thp hn phng php (B). iu nyc th gii thch l do thi gian ly trch artermisinin bng phng php (A) kh di (1.560pht), m artermisinin d b phn hy. Qua ta thy thm mt u im ca h thng (B) lthi gian thc hin ly trch nhanh nn t gy phn hy hot cht.

Tuy nhin nhn chung, c hai phng php u trch kit sn phm nh mong mun, nnhiu sut chung gn bng nhau.

4. KT LUNu im ca thit b ly trch Soxhlet-chiu x vi sng: nhanh, an ton i vi nhng cht

d b phn hy do thi gian cp nhit rt ngn, tit kim nng lng.Khuyt im ca thit b ly trch Soxhlet-chiu x vi sng l cha tng ha c qu

trnh ly trch, tt c mi hot ng iu khin u thc hin bng tay. Lng mu np vo giihn.

5. PHNG HNG PHT TRIN

Thng qua thc nghim, thit b ly trch Soxhlet-chiu x vi sng cho thy cn mt sim cn khc phc vic ly trch mi ny c hon thin hn:

- Lp t thm mt thit b kim sot nhit n nh nhit ni v tr t nguynliu.

- Lp t thm mt cm bin kim sot mc dung mi ni v tr t nguyn liu.


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- Lp t thm mt b phn theo di nng dung dch ly trch chy ra t bu t nguynliu nhm xc nh thi im hon thnh qu trnh ly trch kit.

- Mt mch in t kt hp cc b phn ni trn v ni vo b phn iu khin thi gianchiu x ca l vi sng.

Nu thc hin c cc ci tin trn, thit b ly trch Soxhlet-chiu x vi sng mi s hotng hon ton tng trong sut qu trnh vn hnh.

USING MICROWAVE-SOXHLET EXTRACTOR TO EXTRACT SOMENATURAL PRODUCTS

Pham Thanh Loc, Le Ngoc ThachUniversity of Science, VNU-HCM

ABSTRACT: Domestic microwave oven was modified into Soxhlet-MicrowaveExtractor for extracting of natural products. The study of its extracted capacity was realized

on: - caffein from Camellia sinensis L.; - stevioside from Stevia rebaudiana (Bert.) Hemsl.; -artermisinin from Artemisia annua L.; - rutine from Sophora japonica L.; - fruit oil from

Illicium verum Hook. f.; - seed oil from Anethum graveolens L.. These extracted results werecompared with the Soxhlet-conventional heating on the time, yield and quality.Keywords: Soxhlet-Microwave Extractor, natural product extraction, Camellia sinensis,

Stevia rebaudiana, Artemisia annua, Sophora japonica, Illicium verum, Anethum graveolens.

TI LIU THAM KHO

[1]. Mike Taylor, Bhuwan Singh Atri, Sonal Minhas. Developments in MicrowaveChemistry, Evalueserve 5-18 (2005).

[2]. Michael J. Collins, Dennis P. Manchester. United States Patent4835354 (1988).[3]. C. Oliver Kappe. Angew. Chem. Int. Ed. 43, 6250-6284 (2004).[4]. J. L. Luque-Garca, M. D. Luque de Castro.Anal. Chem. 73, 5903-5908 (2001).[5]. J. Parera, F. J. Santos, M. T. Galceran. Journal of Chromatography A 1046, 19-26

(2004).[6]. J. R. Jocelyn Par, Michel Sigouin, Jacques Lapointe. United States Patent5002784

(1991).[7]. M. Letellier, H. Budzinski.Analusis 27, 259-271 (1999).[8]. V. Fernndez-Prez, L. E. Garca-Ayuso, M. D. Luque de Castro. Analyst125, 317-

322 (2000).[9]. Xiaolan Zhu, Qingde Su, Jibao Cai, Jun Yang. Analytica Chimica Acta 579, 88-94

(2006).[10].F. Chemat, M. -E. Lucchesi, Chapter 22:Microwave-assisted Extraction of Essential

Oils, A. Loupy, Ed.. Microwaves in Organic Synthesis, VCH, Weinheim, 959-983(2006).

[11].L Ngc Thch. Nghin cu chuyn i l vi sng gia dng thnh thit b ly trchhp cht thin nhin v thc hin tng hp hu c. Tuyn tp Hi tho Sng to khoa


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hc vi s nghip cng nghip ha, hin i ha t nc. Nng, 19-23/07/2006,204-212 (2006).

[12].Md. Mumin Abdul, Farida Akhter Kazi, Md. Zainal Abedin, Md. Zakir Hossain.Malaysian Journal of Chemistry 8(1), 45-51 (2006).

[13].Georgia J. Persons, United States Patent3723410 (1973).[14].14. A. R. Bilia, P. Melillo de Malgalhaes, M. C. Bergonzi, F. F. Vincieri,Phytomedicine 13, 487-493 (2006)

[15].Farouk S. Elferaly, Hala N. ElSohly. United States Patent4952603 (1980)[16].Nguyn Th Hoi, L Ngc Thch.Bo co Khoa hc, Ngy Ha hc Tp HCM ln

5, 11/10/2007, 78-83 (2007).[17].Wang Qin, Jiang Lin, Wen Qibiao. Wuhan University Journal of Natural Sciences

12(2), 529-534 (2007).[18].Nguyn Th Kim Phng, L Ngc Thch. Tuyn tp cc cng trnh, Hi ngh Khoa

hc v Cng ngh Ha hc Hu cTon quc ln th 4, H Ni 20/10/2007, 485-489(2007).

PH LC

Ph lc 1. Thit b Soxhlet-un nng cin (A) Ph lc 2. Thit b Soxhlet-chiu x vi sng (B)


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Bng 2. So snh kt qu ly trch theo hai phng php (A) v (B)

Nguyn liuCu phn

chnhPhngphp

Thigian

(pht)

Khilng

cao 1 (g)

Hiu sutcao 1 (%)

Khilng cao

2 (g)

Hiu sutcao 2 (%)

Hm lngcu phn

chnh (%)*

Khi lngcu phnchnh (g)

A 1670 8.2516 41.72 0.2477 1.25 84.97 0.2105Bp tr lng Cafein

B 137 8.3925 42.00 0.2629 1.33 83.78 0.2203

A 2340 6.4654 33.76 1.3673 7.01 16.05 0.0157C ngt Steviosid

B 150 6.7951 35.49 1.5344 8.01 14.16 0.0174

A 1380 8.2085 44.18 3.3142 17.84 99.45 3.2959Hoa he Rutin

B 112 8.7970 47.18 3.5073 18.81 93.69 3.2860

A 1560 0.8742 4.41 0.3514 1.77 0.65 0.0023Hoathanh hao hoa

vngArtermisinin

B 118 1.1098 5.62 0.4280 2.17 0.84 0.0036

A 1500 2.9199 16.68 2.3876 13.64 94.10 2.2467Trii hi

(E)-AnetolB 95 3.1406 17.90 2.3960 13.66 94.10 2.2546

A 1260 1.9537 10.20 1.1692 6.14 32.93 0.3850Ht th l Apiol

B 85 2.1051 11.02 1.2969 6.79 29.39 0.3812

* Theo kt qu % ca GC-MS, HPLC-MS, hoc HPLC-UV

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