TAP CHi V - DVOC HOC QUflN SIT Sd' S-Z014
NGHIEN CLTU DIEU CHE BOX CAO KHO TOI DEN B A N G PHl/ONG PHAP PHUN SAY
Vu Binh Diromg*; Nguyin Trgng Diep' TOM T A T
€a khSo sSt cSc dilu kl$n thich hpp cho phun say cao khd toi den g6m: ta du'pc ho trp phun say. mltodextrin; aerosol (9:1) vdi ty 1$ 1:1 Vci nhi&t 66 phun sly la 140°C; ty le chat rin trong d]ch phun sly: 15%; toe dO cip d]ch: 50 ml/phiit Vdi cac dieu kien da khao sat, bOt cao khd toi den thu di^pc khd loi, tron chay tit, hi^u suit thu hoi hoat chat v^ hieu suit phun sly iln lu'pt 14: 91,60% v4 86,06%
* TO khda: Toi den; Phun sly
PREPARNG BLACK GARLIC DRIED EXTRACT POWDER BY SPRAY DRYING
SUMMARY
The optimal conditions for spray-drying of black Garlic extract including: maltodextrin and aerosll (9'1) were used as carrier agents: temperature: 14(fC: residue content of extract: 15%:
feeding flow rate: 50 ml/m. With the investigated conditions, blackgarlic powder was dry, well- flowing, the bioactlve recovery and spray-drying yield were 91.60% and 86.06%, respectively,
" Key words: Black Garlic: Spray-drying BAT VAN OE
Tdi den li san phim len men tu toi tuai d nhiet dp v^ dp am thich hpp. San phim thu dupc cd m^u den vj ngpt, khong cdn mui vj hSng cay cua toi tupi.
Cie nghien cCru cho thiy djch chiet toi den c6 mpt so tac dgng vupt trpi sp vdi tdi tupi nhu: lic dyng ching oxy hoa, tang cudng miln djch, Cfc c h i t l bao ung thu .. 5, 6]. Q Vi^t Narti, Hpc viSn QuSn y da nghien cuu len men tdi den t u nguIn toi Vipt Nam va danh gia mpt s6 tac dgng sinh hpc cua djch chiit tei den thu duac [1, 2]. T u tei den da nghien cuu chiet xuat djch chiet bang phuang phap chiit sieu am cd hi$u suit thu hdi hoat chit cap [4].
Phun say la ky thuat tao tieu phan khd bang canh phun ddng chit Icng vao budng khi ndng, chit Idng dupc bay hai nhanh ra khdi h6n hpp r i n Idng, nhd dd, chit ran dupc lam kho. Ky thuat phun say dupc si dyng kha pho biln trong dilu c h i bpt cao khd dupc lieu vdi nhieu uu diem: hieu suit cao, thdi gian sly ngan, hoat chat it bj anh hudng bdi nhiet dp, cao thu dupc la dang bpt khd tai va d l hda tan [7]. Vdi nhung uu diem do, chung tdi nghien cuu dilu che bpt cap toi den bang ky thuat phun say ting sdi nhim tao ra ban thanh phim cd chit luang va dp on djnh cao, su dyng bao chi cac san phim chua tdi den.
* Hoc vi$n Quin y
Ngu^ phAn hdi (Corresponding): Vu Binh Duong ([email protected]) Ngay nhfn bii: 07/04/2014: Ngay phin bi$n danh gia bai bao: 1S/OS/2014
Ngay bii bio du^ ding: 26/05/2014
13
TRP CHi V - Dirge Hpc QURN SV SO 5-2014 NGUYEN VAT LlfiU VA PHUONG PHAP
NGHIEN ciru
1. Nguyen vat lieu vi thilt bi nghien CU'U.
* Nguyen li$u:
- Toi den Viet Nam do Trung tam Nghien cuu Lfng dgng San xuat Thuoc, Hpc vi$n Quan y cung d p .
Hda c h i t dung moi: c h i t c h u i n S-Allyl-L-Cystein (Sigma), MeOH, ACN d?t tieu chuin HPLC (Merck); cac ta dupc:
aerpsii; maltodextrin va hda chit dung mdi khac dat tieu chuin dupc dyng hoac tinh khiet phan tich.
* ThiSt bj: may phun s l y LPG5 (Trung Quoc), may chiet sieu am SM30 - CEP (Han Quic); hp thing s i c ky long hipu nang cao Alliance Water 2695D (Hoa Ky);
may ly tam Universal 320 - 1505 (Due);
may xac djnh dp I m AIVIB 310 (Anh); can phan tich Sartprius (dp chinh xac 0,1 mg);
can ky thuat (dp chinh xac 0,01 g).
2. Phu'o'ng phap nghien citu.
' Chief xuat dich toi den:
Djch chiet toi den (1:1) sCr dung d l phun sly dupc chiet xuat bang phuang phap sieu am vdi cac dieu kijn da khao sat gdm: t i n so siSu am 60 MHz, nhiet dp 60°C, chiit 2 lan trong thdi gian 60 phut, ty le dung mdi nudc 10:1, co cao d 60°C bang ap suit giam [4].
* Bleu che bdt cao kho toi den:
Dilu c h i bpt cao kho tdi den bang ky thuat phun s l y t i n g soi [8]. Chp dich chiit toi den vao thilt bj phun say t i n g soi. Cil dat cac thong so: nhipt dp d i u v4o ci3a
budng phun sly, t i c dd d p dich cho voi phun thich hpp. Trong qua trinh nghien cuu, tiin hJnh khao s i t cac thdng s l ky thuat cho phun s l y gdm:
+ Anh hudng cua ta dupc ho trp phun sly.
+ Nhi§t dp d i u vao cua budng phun.
+ Ham lupng chat ran cua djch phun sly,
+ Toe dp d p djch phun.
* Can c(> khao sat lira chon quy trinh phun say:
- Dac tinh v§t ly cua bpt: hinh thai bpt, ham I m .
- Hdm lupng S-ailyl-L-cystein trong bpt cap khd: Djnh lupng bang phuang phap sac ky long hieu nang cao [3].
- Hi$y syat thy hdi hcgt chit:
I r . p ,.,, - " " '"'^"3 ^'^(1^3'a)'i°"g bWpHun riy ' ' " Ham luviig SAC (ug/g) Iheo l> thuyet - Hipu suit phun say (%)
u p c n / i - khoi liBjng cao kh6 thu ai««;(g) , „ „ kh6i li^png cao kh6 theo ly thuyet (g)
KfiT QUA NGHIEN CLTU vA BAN L U A N
1. K i t qua xac djnh cac thong s6 nguyen ll#u ciia djch chiit tdi den 1:1.
Tiin hanh chiit xuat 05 me, mci me 03 kg tpi den vdi cac d i l u ki$n da dupc khao sat [6]. Djch chiet dupc cd d i n cao 1:1.
Gpp cap cua 05 me, trpn deu thu dupc nguyen lieu d i u vao (15 kg cao), dong nhit a l khao sat cac thdng s6 ciJa qua trinh phun sly. T i i n hSnh xie djnh cac chi tieu ty ip chit ran, ham lupng SAC, hieu s u i t chiit x u i t cd dac SAC trong cac 1.1.
TAP CHl V - DVOC HOC OURN SVT SS 5-2014 Bang 1: Kit qua xac djnh mdt s l thdng s6 cua nguyen lieu dau vao q u i trinh phun sly.
THONG s d Toi 3en (NL) Dich chiet 1:1
TV- Lg CHAT RAN (%)
22,5
HAM LUONG SAC (ug/g) 268,5 216,7
Hi$u SUAT CHI£T SAO (%)
80,72 Djch chiit tdi den cd hdm lupng chit ran dat 22,5%, ham lupng SAC dat 216 pg/g, so vdi ham lupng SAC cd trong nguyen iieu, hipu suat chiet thu hdi hoat chit dat 80,72%. Djch chiet ndy dupc su dyng de phun say dilu c h i bpt cao khd tdi den.
2. Anh hirang cua ta dipp'c dpn d i n hi^u s u i t va c h i t lu'p'ng san p h i m . SO' dung ta dupc dpn la maltodextrin cho vao djch phun s l y vdi ty le khac nhay (so vdi lupng chit ran cd trong djch chiit tdi den dem phyn): 0,5:1; 1:1; 1,5:1 va hon hpp maltodextrin:aerosoi (9:1) d ty le 1:1 d l khao sat. Mdi me phyn say 200 g djch chiit.
Nhi#t dp d i u vao budng phun 160°C, t i c do d p djch 20 vdng/phOt.
Bang 2: Ket qya danh gid anh hudng cija ta dupc dpn d i n chit luang vd hi$u suit phun sly (n = 6).
MAU THQ
71
T2
T3
T4
T5
TA DUpc DON VA TY" l e s'Cr DUNG SO Vdi LUONG CHXT RAN CO TRONG CAO
KhOng su' dijng
Mal
Mal
Mal Mal-Ae
(9;1) 0.5.1
1 1
1,5-1
I'l
CHI TIEU CHAT LUONG CAO KHO T6I BEN Khfii iugng
cao kh& (g) 28,45 ± 2.21
60,97 ± 5,02
69,10 ±4,61
90,69 ± 3,52
75,05 ±4,86 BO ^m {%)
7,2 ± 0,32
6,8 ± 0,23
4,2 ± 0,41
4,5 ± 0,32
3,8 ±0,35 rips(%)
58,67 ± 4,67
70,37 ± 6,58
73,56 ± 5,73
77,16 ±5,29
80,22 ± 5,69 HsAc{%) 52,4 ±3,21
75,8 ±6,21
81,7 ±5,54
88,4 ± 4,78
87,8 ± 4,83
HlNH THCfC CAM QUAN Kh6i k^t tg mdu nSu den, mui thom d|c tru'ng Khoi k^ tg mdu vdng n&u, mill thOTTi a^c tivng Bgt khft mdu vdng ndu, hoi kit ty, mCii thorn d^c tmng B9t kh& mdu vdng ndu, hoi k^t ty, mCji thom djc trung BOt kh6 mdu vdng ndu, toi, mCii thom dgc trifng Khi them td dupc dpn vap, qud trinh phun sly xay ra de dang han, san phim thu 6u(?c khd tpi han so vdi cdng thuc khdng su dung td dupc dpn vd hi$u suit phun sly oai thien dang k l . Vipc thdm maltpdextrin da giup tao thdnh khii bpt khd, tai. It vdn cgc, it bj dinh bet vdc bging phgn, hi$u suit phun sly va hipu suit thu hdi hp^t chat d i u cao han so vdi khdng su dyng maltodextrin. So vdi diJng maltodextrin dan dpc (T2 den T4), vlpc phci hpp them aerosol (le ty maltodextrin:aerosil Id 9:1) bpt cap khd tdi den thy duac tPi va tran chay t i t han, hdm I m , hipu.suit phyn s l y vd hiey syat thy hdi hoat chat SAC cao hpn trong khi ty ip td dupc ddn su dgng thip han (T5). Nhu vay, su dyng hdn hpp maltodextrin:aerosil (9:1) vdi ty le 1:1 Id chit them vdo de hd trp cho phyn s l y cao khd toi den phu hpp.
15
TRP cHt y - Dir^c HOC O U S N sir sS 5-2014
3. Anh h y d n g cua nhi#t dp phun s l y d i n hieu s u i t va c h i t lu'p'ng san pham.
Cac cong thuc khao sdt deu cd ciing dieu kien v l ty l§ ta dupc ddn, ty Ip chit ran cua djch phun sly, too dd d p djch va dp suit tao phun quay (0,18 bar), nhung khdc a dieu kien nhipt dp dau vdp budng sly Id: 120 -140 -160 - 180°C.
Sang 3: Kit qua danh gid anh hudng cua nhiet dp d l y vdp den qya trinh phyn say (n = 6).
MAU T H U
T8
T 5
T6
T7
NHIET DO PHUN S A Y
120
160
180
140
C H I T i e u C H A T L U O N G C A O K H d T d i B E N Khoi lUdng
cao kho (g) 71,49 ± 4 , 6 4
75.05 ± 2,21
67,98 ± 2,21
75,26 ± 2,21 Do ^ m (%)
6,7 ± 0,34
3,8 ± 0,21
3,5 ± 0,23
4,2 ± 0,23 Hpa (%)
74,11 ± 4 , 2 7
80,22 ± 4,71
72,89 ± 4,65
80,11 ± 5 , 7 3 HsAc (%}
94,2 ± 5,87
87,8 ± 4 , 1 2
82,5 ± 4.48
95,1 ± 5.37
Hinh thiJccam quan BOt khfi mdu vdng nSu, hoi k^t ty, mui t h o m dSc tryng BOt kh6 mdu n^u den, toi, miJi t h o m dgc tru'ng B$t kh6 mdu vdng nSu, tai, miii t h o m a | c truTig BOt khA mdu vang ndu, toi, mCii t h o m d | c tru'ng
Khi phun sly d nhiet dp khdc nhay, chit lupng, hinh thLKc cao khd cung nhu hipu suit vd hdm lupng hoat chat trong cao cyng khdc nhau. Khi phun d nhipt dp thip dudi 120°C, sdn phim thy dupc cc ham I m cao (6,7%). D i l u ndy co t h i do nhipt dp thap hpn khong du d l sly khd cdc gipt phun, Idm san phim cd hdm I m cao. Khi ndng nhipt dp phun sly tCf 140 - 180°C, bot thy dupc cd hdm I m thip (< 5%). Tuy nhien, ney phn sly p nhiet dd qya cao, hdm lupng SAC se gidm do hoat chat dd bj phan hyy mdt phan.
Nhu vdy, nhipt dp de phun s l y cap khd tdi den thich hpp Id 140°C (cdng thuc T7).
San phim thu dupc cd ham I m bpt thip, khdi bpt thy dupc tai vd tran chay tct, hipu suit thu hdi hoat chat cao.
4. Anh huo'ng cua hdm lyqcng c h i t rdn trong djch phun d i n hIpu s u i t va chit lu'O'ng san p h i m .
Tien hanh phun s l y cao khd tdi den vdi cac dieu kipn da khap sdt, chi thay d i i it ve luang chit ran trong djch phun vdi ty ip 10,15 va 20%.
Bang 4: K i t qua danh gid anh hudng cua hdm lupng chit rdn trpng dich phun din qua trinh phyn say (n = 6).
MAU THCT
T 7
T9
TIO
TS- l e CHAT RAN TRONG D!CH PHUN
15
10
20
CHI T I § U CHAT LUONG CAO K H O T 6 I D E N Khoi luUng
cao kho (g) 75,26 ± 2,21
77.53 ± 5,21
72,51 ± 5,82 B o am (%)
4,2 ± 0,23
4,3 ± 0,31
4,7 ± 0,24 rips{%)
80,11 ± 5 , 7 3
82,44 ± 5 , 4 3 76,78 ± 3,96
/
HSAC{%)
95,1 ± 5,37
92.7 ± 6,04
90,5 ± 5 . 7 6
Hinh thOc c3m quan
BOt kh6 mdu vdng ndu, toi, mOi t h o m d|ic trung BOt kho mdu vang nau, toi, m u i t h o ' m d S c t r u ' n g BOt kh6 mdu vdng ndu, hoi v6n eye. mCii t h o m d^c trynq
Hdm lupng chit rdn khdc nhau trong djch phun it anh hudng den ham I m va hipu suit thu hdi hoat chit, nhung lai dnh hudng d i n hipu suit phun s l y vd k h i i lupng neng cua san phim theo xu hudng cdng tang ty le chit ran trong djch phun cdng lam
TQP CHf V - DirOC H9C QUAN SV sd 5-2014 giam hipu suit phun sly, cdn khoi lupng rieng lai tang d i n Khi dich dem phun cd hdm lupng chit ran 10% (T9), hipu suit phun s l y cao hpn cdng thCfc T7 va TIO. Nhu vdy, lua chpn djch chiit cao tdi den cd hdm lupng chit ran 15% dem phun sly id thich hpp nhit.
5. Anh hu'dng cua tdc d$ d p dich din hieu suit va chit lu'p'ng san phim.
Cac cdng thCrc khdo sat deu c6 cung dieu ki$n phun sly, chi khac nhau ve t i c dp d p djch: 25 - 50 Id 75 ml/phCit.
B^ng 5: Anh hudng cua tec dp d p djch d i n qud trinh phun s l y (n = 6).
MAU THO
T 7
T11
T12
idcDO CAP DICH
75
50
25
C H I T I E U C H A T L U p N G CAO KHO T 6 | DEN Kh6i luQng
cao kho (g) 75,26 ± 2 , 2 1
80,51 ± 5,21
82,57 ± 6,21 Bfl l m (%)
4,2 ± 0,23
3,8 ± 2 , 2 1
4,3 ± 2 , 2 1 Hps {%)
80,11 ± 5 , 7 3
86,06 ± 5,85
87,89 ± 6,02 risAc(%)
95,1 ± 6 , 3 1
91,SI ± 6 , 3 6
87.33 ± 4 . 7 9
Hinh thifc cam quan BOt kho mdu vdng ndu, toi, mOi t h o m ddc tru'ng BOt kho mau vdng ndu, toi, mill thom d | c tru'ng BOt khd mdu vdng ndu, t o i , mjji thom fldc trung
Tie dp d p djch anh hudng din hipu suit phun s l y vd hieu suit thu hoi ho?t chit SAC.
Too dd d p djcli giam t u 75 xudng 50 vd 25 ml/phut dd Idm tdng hi$y sylt phun sly tu 80,11 len 86,06 vd 87,89%. Hidu suit thu hdi hoat chit SAC p t i c dp 75 vd 50 ml/phut (cdng thuc T7 vd T l 1) tuang duang nhau vd deu cap han d t i c dp d p djch 25 ml/phut (ccng thuc T12). Tyy nhien, tec dp d p djch 25 vcng/phyt che bpt cd khdi lupng rieng thdp nhit. Nhu vdy, khi phun s l y cao khd tdi den, t i c dp d p dich thich hpp la 50 ml/phut.
Tu k i t qya khap sdt tren, lua chpn dieu kipn d l phun s l y bpt cac khd tdi den: chit mang thdm vdp Id hpn hpp maltodextrin:aerosil (9:1) vdi ty le 1:1 so vdi hdm lupng chit rIn trcng cao, hdm lupng chit ran trcng djch phun 15%; nhipt dp phun s l y 140°C, t i c dp d p djch 50 ml/phut, dp suit tac phun quay 0,18 bar. Be ddnh gid dp lap lai cua quy trinh, t i i n hanh phun say 5 me khdc nhau d cung dieu kidn. K i t qud xdc djnh chi tieu cua san phim nhu say:
Bing 6: K i t qya xdc djnh cdc chi tieu bpt cao kho tdi den.
MAU THU 1 2 3 4 5
"X RSD
CHi TifeU C H A T L U O N G CAO K H O T 6 I DEN Khoi tildng
cao khS (g) 85,63 81,89 80,51 87,51 80,96 83,30 3,10
B o im {%) 3,8 3,7 3,8 3,7 3,8 3,76 0,06
Hps (%) 80,16 86,54 86,06 84,79 85,04 84,99 3,05
risAc(%) 95,61 92,36 91,64 89,36 85,97 90,988 3,59
Hinh Ehilc cam quan BOt kh6 mdu vdng ndu, toi, mCii thom d^c trung BOI kho mdu vdng ndu, toi, mui thom d^c trung BOt khQ mdu vdng ndu, toi, mOi thom ddc trung BOt kh5 mdu vang ndu, toi, mui t h o m d j c tru'ng BOt kho mdu vdng ndu, toi, mui thom S^c trung
Khi pinun s^y 5 me o cung 6ihu ki$n, chat lu'p'ng san phSm cung nhu" hi$u suat quy trinh phun say l^ha 6n djnh voi gia trj RSD < 5%. Nhu" vay, phu-ang phap phun s l y cao I<h6 toi den co 6Q l$p lai cao, c6 th^ irng dyng dieu ki^n n^y d§ san xulit cao kho toi den phyc vy bao ch6 cac san phim thu6c, thyc pham chu'c nang chi>a toi den.
17
TFIP CHf V - Di;OC Hpc OUfiN S^ sS 5-2014 KST LUAN
Dd xay dung quy trinh dilu che bpt cao khd tdi den bang phuang phdp phun sly tang sdi. Khdo sdt dupc cdc dilu kien thich hpp cho phun s l y cao khd toi den gdm: td dupc ho trp phun sly maltpdextrin:
aerosol (9:1) d ty le 1:1; nhidt dd phun sly: 140°C; ty ip chat rIn trong djch phun sly: 15%; too dp d p djch: 50 mi/phut.
Vdi cac dieu kien da khac sdt bpt cao khd tdi den thy dupc khd tpi, tran chay tot.
Hi$y suit thu hdi hoat chit va hipu suit phun sly iln luat Id: 91,60% vd 86,06%.
TAI LIEU THAM KHAO
1. vo Binh Duong, Trinh Nam Trung. PhSn lap S-ailyl-L-cystein tir toi den Vi$t Nam.
Tap chi Dypc hpc 2014.
2. VO Binh Dunng, HS Anh San, VO Xuin NghTa, Trinh Nam Trung. Sdnh gia tdc dung bao v$ Cff quan mi§n dich cua djch chiet toi den Ly Son trfin chuOt b| chieu xg. Tap chf Dupc hpc. 2013, so thdng 1, tr.61-56.
3. ChCr VSn Min, VO Binh Duong, Bio VSn B6n, Trinh Nam Trung. Nghign cCru dinh
lupng S-allyl-L-cystein trong t61 den Ly Son bing sic ky Idng hi$u nang cao. Tap chi Y - Dupc hpc Qudn sy. 2012, 37 (9), tr.11-15.
4. VO Binh rdn, VO Binh Duang, NguySn Trgng Blip, Phan Binh Chiu, NguySn VSn Bach, xay dung quy trinh chiet xuit SAC tir toi den. Tap chi Y - Duoc hpc Quan su, 2014, 39 (1), tr.58-62.
5. Danan Wang, Yonghui Feng, Jun Uu, JIanzhong Yan, Meiru Wang, JIn-ichI Sasaki, Changlong Lu. Black Garlic (Allium sativum) extracts enhance the immune system. IVled.
Aro Plant Sci Bio. 2010, 4, pp.37-40.
S. Shin J. H, Choi D. J, Lee S. J, Cha J. Y, Kim J. G, Sung N. J. Changes of physicochemlcal components and antioxidant activity of garlic during its processing. Journal of Life Science.
2008, 18, pp.1.123-1.131.
7. Krzysztof Cai, Krzysztof Solk>hub. Reviews:
Spray Drying Technique. II. Cuirent Applications in Pharmaceutical Technology. Journal of Pharmaceutical Sciences, 2010, Vol 99, No. 2
8. Maria Jose Fabra et al Effect of maltodextrins in the water-content-water activity- glass transition relationships of nom (Morlnda citrifolla L.) pulp powder. Journal of Food Engineering. 2011, 103, pp.47-51.