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KHO ST CC YU T NH HNG N QU TRNH CHNG CT TINH DU GNG


Tng Th nh Ngc1 v Nguyn Vn Kin2

ABSTRACT
The main objectives of this research were to test the effects of storage time after harvesting and the distillation time on the yield of ginger oil. Further investigation was carried out to evaluate the chemical, physical properties as well as sensory characteristics of ginger oils which were extracted by conventional hydrodistillation and microwave-assisted hydrodistillation. The results showed that the storage time of ginger rhizomes should be within 4 days before distillation. The total time of distillation was 16 hours and only 80 minutes at 300W, respectively. Moreover, not only the quality of ginger oils but also the type of components in the essential oils were moderately dependent on the hydrodistillation methods. The major compounds in ginger oils from both such hydrodistillation ways consisted of Neral (13,99-24,04%), Zingiberene (10,62-10,88%), alpha-Farnesene (7,3-8,05%), Nerol (6-7,09%) and beta- Sesquiphellandrene (5,315,37%). Keywords: Ginger oil, distillation, microwave Title: Investigation of several parameters affecting hydrodistillation of ginger oil

TM TT
Mc tiu chnh ca nghin cu ny l kho st cc yu t nh hng n qu trnh chng ct tinh du gng nh thi gian lu tr ( ho) v thi gian chng ct. Bn cnh , nh hng ca phng php chng ct n gi tr cm quan v cc thng s ha-l ca tinh du gng cng c tin hnh nh gi. Kt qu nhn thy gng sau khi thu hoch c lu tr 4 ngy v chng ct trong thi gian 16 gi bng phng php li cun hi nc hay 80 pht khi c s h tr ca vi sng vi cng sut 300W l ph hp v hiu sut v cht lng ca tinh du thu c. Cht lng tinh du v hm lng cc cu phn c trong tinh du gng th ph thuc vo phng php chng ct. Cc cu phn chnh trong tinh du gng thu c t hai phng php chng ct trn gm Neral (13,99-24,04%), Zingiberene (10,62-10,88%), alpha-Farnesene (7,3-8,05%), Nerol (6-7,09%) v betaSesquiphellandrene (5,31-5,37%). T kha: Tinh du gng, chng ct, vi sng

1 T VN Gng (tn khoa hc: Zingiber officinale Roscoe thuc gii Plantae, ngnh Magnoliophyta, lp Liliopsida, b Zingiberales, h Zingiberaceae, chi Zingiber, loi Zingiber officinale) l loi cy tho c trng t rt lu i. Ngy nay, cy gng c trng khp ni trn th gii, ring Vit Nam gng trng rt ph bin ng bng sng Cu Long v n c c im trng xen canh trong cc vn cy n tri v c gi tr kinh t tng i cao ( Huy Bch et al., 2004). Gng khng nhng c s dng kh ph bin nh mt loi gia v (Ravindram and Babu, 2005) m cn c b sung vo cc khu phn n cha bnh bun nn
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Khoa Nng nghip v Sinh hc ng dng, Trng i hc Cn Th Cng ty Savipharm

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(Kawai, 1994; Vutyavanich et al., 2001; Borrelli, 2005) chng say tu xe (Chrubasik, 2005); chng oxi ha v khng vim (Shogi et al., 1982). Chnh v c im trn m dch trch cng nh tinh du t c gng c s dng ph bin trong ch bin thc phm hay trong dc phm. Dch trch t c gng gm cc hp cht bay hi v cht tan to ra mi hng c trng v v cay ca gng. Trong , hai hp cht chc nng 6-gingerol v 6-shogaol th to ra v cay c trng hn cc hp cht khc c trong gng (Zancan, 2002). Ngoi ra, chnh hai hp cht trn cn mang tnh khng khun v c s dng trong iu tr cc bnh nhn b suy gim min dch (Hiserodt et al., 1998). Mt khc, tinh du gng l mt hn hp cha cc hp cht d bay hi, trong zingiberene l thnh phn chnh to ra mi hng ca gng, chnh c im ny m tinh du gng thng c s dng nhiu trong lnh vc dc phm, m phm hay thc phm c th trong cc thc ung, gia v, kem, ko... Tinh du gng thng c trch bng phng php li cun hi nc. Vic trch ly tinh du gng cho hm lng ti u ph thuc nhiu yu t nh phng php trch hay nguyn liu dng trch. Tuy nhin, cc yu t quan trng c nh hng n qu trnh trch ly tinh du gng t c quan tm Vit Nam. Do , vic kho st phng php trch ly hiu qu v kho st cc thng s ha-l ca tinh du gng l mc tiu chnh ca nghin cu ny. 2 PHNG TIN V PHNG PHP NGHIN CU 2.1 Chun b mu Th nghim c tin hnh ti b mn Cng ngh ha hc, Khoa Cng Ngh, Trng i hc Cn Th. Nguyn liu c gng 7 thng tui (Zingiber officinale Roscoe) c thu mua trc tip ti vn Hu Giang, m bo ti, khng dp nt hay thi hng. Sau khi vn chuyn gng n phng th nghim, tin hnh chn la s b, loi tp cht, ra sch, xt lt nh, xay nhuyn trc khi thc hin cc nghin cu. 2.2 Phng php b tr th nghim 2.2.1 Chng ct li cun hi nc Cho gng vi khi lng l 250 g, lng nc chng ct l 400 ml vo bnh ct ca h thng chng ct Clevenger. Mu c gia nhit bng bp in, khi hn hp si hi nc to thnh s li cun tinh du i ln v i vo h thng ngng t. Sau khi ngng t, hn hp lng gm tinh du v nc c chit vi diethyl eter (Trung Quc sn xut). Hn hp thu c gm tinh du, diethyl ether v mt t nc. Tinh du c lm khan nc bng mui Na2SO4 (Merck, c sn xut) khan. Sau hn hp cn li c c quay chn khng ui diethyl ether thu c sn phm tinh du. -Kho st nh hng ca thi gian ho n hm lng tinh du gng Gng 7 thng tui c thu hoch v lu tr ( kh t nhin trnh nh nng mt tri) vi cc khong thi gian 0, 1, 2, 3, 4, 5, 6 v 7 ngy. Sau mi ngy lu tr, cn 250 g v tin hnh chng ct trong 4 gi. Sau khi chng ct, loi nc v xc nh lng tinh du thu c.
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-Kho st hng ca thi gian chng ct n hm lng tinh du gng. Gng c thu hoch v lu tr theo thi gian xc nh t th nghim trn, sau tin hnh kho st thi gian chng ct t 2, 4, 6, 8, 10, 12, 14, 16, 18 v 20 gi. Tinh du sau chng ct c loi nc v xc nh khi lng. ng thi cc ch s ha l v cm quan ca tinh du thu c t iu kin chng ct ti u cng c xc nh. 2.2.2 Chng ct li cun hi nc c h tr ca vi sng Gng thu hoch thi im 7 thng tui sau lu tr vi thi gian ti u t th nghim trn (2.2.1). Mu c t vo bnh ct ca h thng chng ct Clevenger vi khi lng nguyn liu l 250g v lng nc l 400ml, sau h thng chng ct c t vo l vi sng (Sanyo fan-assisted microwave oven 1200W) v tin hnh chng ct tinh du cc mc nng lng v thi gian khc nhau: - Cng sut 300W thi gian chng ct t 40, 50, 60, 70 v 80 pht. - Cng sut 450W thi gian chng ct t 40, 45, 50, 55 v 60 pht. - Cng sut 750Wthi gian chng ct t 10, 15, 20, 25 v 30 pht. Tinh du sau chng ct c kh nc v xc nh khi lng, tinh du thu c t iu kin chng ct ti u c nh gi cm quan v xc nh cc ch s ha l. 2.3 Phng php o c v x l s liu - Xc nh hm lng tinh du bng cn phn tch Sartorius YDK 01 (200 0,0001g). S liu c tnh ton thng k thng qua phn tch phng sai t chng trnh Statgraphics 4.0 vi s kim tra mc ngha ca cc nghim thc qua LSD (Least Significant Difference). - Xc nh ch s vt l: T trng xc nh bng cn phn tch Sartorius YDK 01 (c sn xut). Ch s khc x c o bng khc x k HR901 Kruss (c sn xut). -Xc nh ch s ha hc: Ch s acid chun bng dung dch KOH 0,1N (Merck, c sn xut). Ch s savon ha chun bng dung dch HCl 0,1N (Merck, c sn xut). Ch s ester ha l hiu s ca ch s savon ha v ch s acid. Thnh phn ho hc ca tinh du c xc nh bng phng php sc k kh ghp khi ph GC-MS (Gas Chromatography Mass Spectrometry) ti Trung Tm Phn Tch Cng Ngh Cao Hon V (S 112A Lng Th Vinh, Phng Tn Thi Ha, Qun Tn Ph, Thnh Ph H Ch Minh).

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3 KT QU V THO LUN 3.1 Chng ct li cun hi nc Chng ct nhm li cun tinh du bng hi nc l phng php ph bin s dng tch hn hp khng ln vo nhau nh nc v tinh du khi tip xc trc tip nhau. Nhm thit lp quy trnh chng ct tinh du hiu qu, mt trong cc yu t nh hng n hiu sut ca qu trnh chng ct nh thi gian lu tr mu (hay cn gi l thi gian ho) c kho st v kt qu th hin bng 1.
Bng 1: Hm lng tinh du theo thi gian lu tr

Thi gian lu tr (ngy) 0 1 2 3 4 5 6 7

Hm lng tinh du (g) 0,5707d 0,5720d 0,6347c 0,6478bc 0,6922a 0,6623b 0,6556b 0,6524b

Cc ch ci khc nhau trong cng mt ct biu th s khc bit c ngha tin cy 95%

T s liu ca Bng 1 nhn thy hm lng tinh du tng theo thi gian lu tr t 0 n 4 ngy (khong 0,57 g n 0,69 g) nhng sau li gim dn t ngy 5 n ngy 7 (gim t khong 0,69 g n 0,65 g). Theo cc ti liu nghin cu cho thy gng sau thu hoch th hm lng cc monoterpene gim xung cn cc sesquiterpene th tng ln (Sasidharan et al., 2010). C th, thi gian ho t 0 n 4 ngy th hm lng cht kh tng ln v lng cc cu phn sinh ra nhiu hn cc cu phn mt i; ngc li i vi thi gian ho t 5 n 7 ngy, mt s cc cu phn b phn hy theo thi gian tn tr nh zingiberene v -sesquiphellandrene di tc dng ca nh sng v khng kh (Connell v Jordan, 1971) nn hm lng tinh du gim. Theo s liu thng k th thi gian sau thu hoch 4 ngy c hm lng tinh du cao nht v khc bit c ngha so vi cc thi im khc. Do , gng sau thu hoch 4 ngy c chn la kho st nh hng ca thi gian chng ct n hm lng tinh du gng.
Bng 2: Hm lng tinh du theo thi gian chng ct

Thi gian chng ct (gi) 2 4 6 8 10

Hm lng tinh du (g) 0,5511g 0,6922f 0,7182e 0,7370d 0,7540c

Thi gian chng ct (gi) 12 14 16 18 20

Hm lng tinh du (g) 0,7680c 0,8176b 1,0858a 1,0860a 1,0861a

Cc ch ci khc nhau trong cng mt ct biu th s khc bit c ngha tin cy 95%

T Bng 2 cho thy hm lng tinh du tng theo thi gian chng ct. Thi gian t 2 gi n 16 gi lng tinh du tng u nhng sau th hm lng tinh du khng tng khi ko di thi gian chng ct. iu ny cho thy khi thi gian chng ct ngn th cha trch tinh du c trong mu nn lng tinh du thu c t. Ngc li, khi thi gian chng ct di th tinh du c trong t bo khuch tn ra ngoi v c hi hc li cun theo cho n ht tinh du c trong mu. Khi thi
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gian chng ct l 16 gi v ko di n 20 gi th trong mu hu nh ht tinh du nn lng tinh du thu c hu nh khng i (khong 1,08g). Mt khc, khi thi gian chng ct t 16 n 20 gi hm lng tinh du thu c khc bit khng c ngha thng k. Do , tit kim nng lng cng nh thi gian th thi gian chng ct tinh du thch hp nht l 16 gi. 3.2 Chng ct li cun hi nc c h tr ca vi sng
Bng 3: Hm lng tinh du theo thi gian chng ct cc mc cng sut khc nhau

Cng sut 300W Thi gian Hm lng (pht) tinh du (g) 40 0,5968e 50 0,6403d 60 0,6566c 70 0,6823b 80 0,7185a

Cng sut 450W Thi gian Hm lng (pht) tinh du (g) 40 0,5264d 45 0,5868c 50 0,6379b 55 0,6461ab 60 0,6729a

Cng sut 750W Thi gian Hm lng (pht) tinh du (g) 10 0,3300e 15 0,5104d 20 0,6601a 25 0,6012b 30 0,4780c

Cc ch ci khc nhau trong cng mt ct biu th s khc bit c ngha tin cy 95%

Nhn chung, hm lng tinh du tng theo thi gian chiu vi sng (Bng 3). Khi chng ct tinh du bng l vi sng, hm lng tinh du cao nht 80 pht ng vi cng sut 300W hay ch 60 pht mc cng sut 450W. Ngha l, khi chng ct mc nng lng cao th thi gian cn chng ct ngn. C th, cng sut 750W, thi gian chng ct l 20 pht s thu c hm lng tinh du cao nht, nu ko di thi gian chng ct th nguyn liu b kh, tinh du b kht v c mi l. Kt qu nh vy l do di tc dng ca vi sng, nc trong t bo nng ln, p sut bn trong gia tng nhanh chng, lm cho cc tuyn tinh du b v ra, kt qu l tinh du cha trong cc tuyn c gii phng ra ngoi (Wang et al., 2010). Tuy nhin, cng sut cao 750W, khi tip tc chiu vi sng na th vn tc bc hi ln nn mt phn hi c ln tinh du b thot ra ngoi. Do , hn ch s tht thot tinh du khi chng ct mc nng lng cao, cng sut 300W trong thi gian chng ct 80 pht l ph hp v hiu qu v cht lng ca tinh du thu c. 3.3 c im cm quan v ch s ha l ca tinh du gng
Bng 4: So snh c im cm quan v ch s ha l ca tinh du gng trch ly bng hai phng php chng ct

c im Mu sc Mi V T trng Ch s khc x Ch s acid Ch s savon ha Ch s ester

Chng ct khng h tr vi sng Vng nht Thm du v c mi rt c trng ca gng Cay 0,8806 1,4884 0,8507 9,2540 8,4033

Chng ct c h tr vi sng Vng nht Mi thm rt c trng ca gng nhng hng cay v nng hn Cay 0,8916 1,4834 1,4210 15,1175 13,6965

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Bng 5: So snh thnh phn cc cu t trong tinh du gng trch ly bng hai phng php chng ct

STT 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25 26 27 28 29 30 31 32 33 34 35

Tn cu phn 2-Heptanol Tricylene alpha-Pinene Camphene beta-Pinene beta-Myrcene 2-Thujene Eucalyptol 4-Carene Linalool Camphor Citronellal Borneol 4-Terpineol alpha-Terpineol Citronellol Nerol Neral Bornyl Acetate cis-2,6-Dimethyl-2,6-octadiene Copaene Beta-Farnesene Eugenol Alloaromadendren Curcumene Beta-Cubebene Zingiberene alpha-Farnesene Beta-Bisabolene Epi-bicyclosesquiphellandrene beta-Sesquiphellandrene Nerolidol gama-Elemene beta-Selinol Farnesal

Thnh phn phn trm khi lng (%) Khng h tr vi sng C h tr vi sng 0,14 0,11 2,03 0,31 5,01 0,90 0,45 2,18 0,37 3,38 0,64 5,67 1,87 0,30 1,41 1,18 0,11 0,32 0,38 0,97 1,31 0,21 0,24 1,44 1,92 1,59 1,89 6,00 7,09 13,99 24,04 0,32 0,38 0,46 0,43 0,25 0,21 0,27 0,24 0,21 0,23 0,20 2,57 2,06 1,08 10,62 10,88 8,05 7,30 2,94 2,59 0,37 0,39 5,37 5,31 0,78 0,91 0,33 0,32 0,63 0,97 0,12 0,28

Theo Bng 5, cc cu phn chnh trong tinh du gng sau khi chng ct bng hai phng php: chng ct li cun hi nc v khi chng ct li cun hi nc c h tr ca vi sng gm Neral, Zingiberene, alpha-Farnesene, Nerol, betaSesquiphellandrene. Hn na, tinh du gng sau khi trch ly c mi thm rt c trng, iu ny l do cc hp phn alpha-Terpineol, beta-Sesquiphellandrene, Curcumene, Nerolidol, chnh l thnh phn to ra hng thm c trng ca tinh du gng (Smith v Robinso, 1981). Hm lng v loi tinh du cn ph thuc nhiu vo tui thu hoch, ging, ngun gc v phng php chng ct (Bednarczyk et al., 1975). Cc thnh phn km phn cc (alpha-Pinene, Camphene, beta-Myrcene, Eucalyptol, Copaene, Curcumene, alpha-Farnesene, beta-Bisabolene, beta-sesquiphellandrene) trong tinh du gng thu c bng
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phng php chng ct c h tr ca vi sng thp hn. Ngc li, nhng thnh phn phn cc hn do c cha oxi nh: Neral, Borneol, alpha-Terpineol, Nerol, Bornyl Acetate, Nerolidol, beta-Selinol, Farnesal li chim hm lng cao hn, bi v vi sng u tin tc dng ln nhng hp cht phn cc, gip nhng thnh phn ny tng nhit rt nhanh, thot ra t bo v b li cun theo hi nc d hn. y cng l l do chnh dn n s khc nhau v c tnh cm quan v cc ch s ha l ca tinh du gng khi chng ct vi cch khc nhau (Bng 4). 4 KT LUN C gng 7 thng tui c thu hoch, lu tr trong 4 ngy v chng ct trong thi gian 16 gi hay 80 pht khi chng ct c s h tr ca vi sng vi cng sut 300W l ph hp v hiu sut v cht lng ca tinh du thu c. Tuy nhin, chng ct c s h tr ca vi sng c th gia nhit nhanh, tit kim c thi gian nhng hiu sut trch ly km, c th hiu sut ca qu trnh chng ct tinh du l 0,43432 % so vi chng ct c s h tr ca vi sng l 0,2874 %. Cc cu phn chnh trong tinh du gng sau khi chng ct bng hai phng php trn gm Neral (13,99 24,04 %), Zingiberene (10,62 10,88 %), alphaFarnesene (7,3 8,05 %), Nerol (6 7,09 %) v beta- Sesquiphellandrene (5,31 5,37 %). TI LIU THAM KHO
Bednarczyk A. Allen, William G. Galetto and Amihud Kramer. 1975. Two new sesquiterpene alcohols from oil of ginger (Zingiber Officinale) (Cis- And Trans-.Beta.Sesquiphellandrol) J. Agric. Food Chem., 23, 499. Borrelli F., Capasso R., Aviello G., Pittler M.H., Izzo A.A., 2005. Effectiveness and safety of ginger in the treatment of pregnancy-induced nausea and vomiting. Obstet Gynecol; 105, 849-56. Chrubasik S., Pittler M.H., Roufogalis B.D., 2005. Zingiberis rhizoma: a comprehensive review on the ginger effect and efficacy profiles. Phytomedicine;12, 684-701. Connell, D.W.; Jordan, R.A.,1971. Composition And Distinctive Volatile Flavor Characteristics Of The Essential Oil From Australian-Grown Ginger. J. Sci. Food Agric, 22, 9395. Huy Bch, ng Quang Chung, Bi Xun Chng, Nguyn Thng Dong, Trung m, Phm Vn Hin, V Ngc L, Phm Dung Mai, Phm Kim Mn, on Th Nhu, Nguyn Tp, Trn Ton. 2004. Cy thuc v ng vt lm thuc Vit Nam, NXB Khoa hc v K thut, tp I, trang 613-618. Hiserodt R.D., Franzblau S.G., Rosen R.T., 1998. Isolation of 6-, 8-, and 10-gingerol from ginger rhizome by HPLC and preliminary evaluation of inhibition of Mycobacterium a_ium and Mycobacterium tuberculosis, Journal of Agricultural and Food Chemistry 46, 25042508. Kawai, T., Kinoshita, K., Koyama, K.and Takahashi, K. 1994. Anti-emetic principles of Magnolia obovata and Zingiber officinale. Planta Med. 60, 17-20. Ravindran, P.N. ; Nirmal Babu, K. 2005. Ginger: The Genus Zingiber, Medicinal And Aromatic Plants: Industrial Profiles; 41, 87-181. Sasidharan1 Indu, A. Nirmala Menon, 2010. Comparative Chemical Composition And Antimicrobial Activity Fresh & Dry Ginger Oils (Zingiber Officinale Roscoe). Journal Of Current Pharmaceutical Research; 2, 40-43. Shogi N., Iwasa A., Takemoto T., Ishida Y., Ohizumi Y., 1982. Cardiotonic principles of ginger (Zingier officinale Roscoe). J Pharm Sci.; 71, 1174. 68

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