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Phn 1.

M U
1.1.

t vn
Bnh tiu ng hin ang l mt thch thc ln i vi vn sc khe

cng ng. Mi nm c thm hng triu ngi mc bnh tiu ng. Theo t
chc y t th gii (WHO), t l mc bnh tiu ng Chu 10 - 12%, cc
quc o Thi Bnh Dng l 30 - 40%. y l cn bnh c th gy ra khng
hong y t th gii trong th k 21, v n c th gim tui th ca ngi dn
trong vng 200 nm ti. c tnh ti nm 2025 th gii c 333 triu ngi mc
bnh chim 6% dn s. T l tng ln cc nc pht trin l 40%, cn cc
nc ang pht trin l 70%[2]. nc ta c khong 2 - 2,5 triu ngi mc l
mc bnh tiu ng. Trong c on c ti 1,3 triu ngi tui di
30 - y l iu ng lo ngi. Theo s liu iu tra mi nht ti 4 thnh ph ln
H Ni, Hu, H Ch Minh, Hi Phng, t l ngi mc bnh tiu ng l 7-8%
trong khi t l mc bnh tiu ng la tui 30 - 64 l 4,2% [2].
Trc thc trng trn c nhiu t chc v c nhn tham gia nghin cu
tm ra thuc iu tr cn bnh nguy him ny. c nhiu loi thuc ha dc
c nghin cu thnh cng, v c hiu qu iu tr cao, nhng khi s dng lu
di li mang ti nhiu bt li vi c th, v vy vic nghin cu cc loi thuc c
ngun gc thin nhin c h s an ton cao hn khi iu tr lu di l xu hng
tt yu. Theo nghin cu ca cc nh khoa hc Nht Bn, n , Hn Quc
trong l du tm c hp cht alkaloit tn gi l 1 deoxynojimycin (DNJ) cu
to tng t nh D - Glucoza c kh nng c ch cc ezim trong h tiu ha nh
- amylaza lm thay i s trao i glucoza cng nh tnh trng ng mu
cao. Cho n nay, l du tm l ngun thc vt duy nht pht hin c cha DNJ
- hot cht c vai tr quan trng trong vic h ng huyt. Do vic nghin
cu ch bin cc sn phm giu DNJ t l du phc v cho vic phng chng
bnh tiu ng ang c quan tm c bit cc quc gia Chu ni c din
tch trng du tm ln.

Vit Nam c nhiu cng trnh nghin cu v tc dng ca DNJ trong


l du tm i vi bnh tiu ng. Tuy nhin cc nghin cu ny mi ch dng
li bc thm d m cha a ra c quy trnh c h thng c th p dng
vo sn xut. Mt khc c nhiu loi thc phm chc nng chuyn bit c ngun
gc t thc vt nh: Diabetna, tiu ng nam dc, NADIAdng cho ngi
b bnh tiu ng. Tuy nhin cc sn phm ny phn ln c nhp khu nn
gi thnh kh cao. Trc nhng yu cu trn chng ti tin hnh ti: Nghin
cu quy trnh ch bin tr t l du tm.
1.2.

Mc ch yu cu

1.2.1. Mc ch
Xc nh quy trnh ch bin tr t l du tm c hm lng DNJ cao dng
trong vic h tr iu tr v phng chng bnh tiu ng.
1.2.2. Yu cu
- Xc nh nguyn liu thch hp cho ch bin tr
- Xc nh c phng php tch chit v thu nhn cao l du ph hp
vi iu kin thit b nc ta.
- a ra c quy trnh ch bin tr t l du c hm lng DNJ cao

Phn 2. TNG QUAN TI LIU

2.1. Tng quan v cy du tm


2.1.1. Ngun gc, phn loi v c im hnh thi ca cy du
2.1.1.1. Ngun gc, phn loi
Cy du tm:
Tn khoa hc: Morus alba L
Ngnh: Spermatophyta
Lp: Angiospermae
Lp ph: Dicotyledoneae
B: Urticales
H: Moraceae
Chi: Morus
Loi: Alba

Hnh2.1. Cy du tm
Cy du c tn chung l Mulberry, mc nhiu ni trn th gii, v c
phn chia thnh ba loi ln.
- Morus alba L. (du trng): Mc ch yu chu , qu mu trng hoc
, l c s dng chn nui tm.
- Morus rubra L. (du ): Mc vng Bc M, qu c mu ta.
- Morus nigra L. (du en): Mc ch yu chu u, qu c mu en.
Cy du c tc sinh trng nhanh va sng vng n i va sng
vng nhit i. Chng c th cao t 10 15m, l mc so le hnh bu dc, hnh
tim hay chia thy. u l nhn phn cung l bu mp l c hnh rng ca, qu
c th n c.
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Theo FAO trn th gii hin c khong 30 nc trng cy du tm, ch


yu l cc nc thuc Chu (chim 60%), trong Trung Quc chim gn
60% lng du c sn xut, H Bc l mt trong nhng vng trng du ln
Trung Quc vi trn 23.000 ha.
Vit Nam, hin nay (ti thi im 5/2010) nc ta c 31 tnh tham gia sn xut
du tm vi tng din tch du l 17.653ha, chim 0,17% din tch t nng nghip.
2.1.1.2. Mt s ging du chnh c trng Vit Nam
Nc ta c khong 165 ging du, bao gm c du a phng, ging mi
lai to trong nc v ging nhp ni, ang c trng khp ni trn c nc,
nhng qua la chn hin nay ph bin trng cc ging du sau:
a) Ging du H Bc
Thu thp c H Bc, hin nay c trng nhiu Hng H, V Th
Thi Bnh, ging gc c lu gi trung tm ging du tm Vit Hng. Thi
gian sinh trng 280 - 290 ngy. L c hnh tim trn, kch thc 15x11cm, mu
xanh nht, t cnh tm, cho nng xut cao vo v xun v v h. Nng sut trung
bnh 20 - 25 tn/ha. C kh nng chng chu tt vi bnh g st, vi khun, vi rt.
Ging thng c trng bng hom nhng vng ngho dinh dng.
a) Ging du Qu
Ch yu trng t ct ven bin Nam nh, Thi Bnh, l c kch thc
thuc loi trung bnh, l dy nhn, mu xanh m. Nng sut l t 35-40 tn/ha.
d) Ging du ngi
Trng ph bin Vnh Phc, Ha Bnh, H Ty c L to, phng, nhn
khng chia thy, thng c mu xanh vng. Nng sut c th t 15 20 tn/ha.
e) Ging du lai tam bi th
y l ging du lai to, trong iu kin thm canh tt c th cho nng sut rt
cao (t trn 40 tn/ha. Cc ging du tam bi th c trng ph bin hin nay
- Ging du lai VH13: L to kch thc trung bnh 18,5x15 cm, dy bng
v phng, mu xanh m. VH13 hu nh khng c qu nn rt thun li cho thu
hi l. Nng sut cao, t trn 40 tn/ha/nm.

- Ging du VH15: Chiu cao cy trung bnh 2,6m, thn mu xanh nht,
cnh nhiu, tn gn, l mu dy mu xanh m, thch nghi vi vng i ni
trung du pha bc. Nng sut l n nh t 25-30 tn l/ha
- Ging du VH1: Nng sut n nh vi trn 35 tn l/ha
f) Ging du VH9
L ging mi lai to, l to, dy, mu xanh m, gi nc tt, thch ng
c vi nhiu loi t trng k c vng i, trung du, Ty Nguyn v vng b
nhim mn. Cho nng xut l kh cao c bit l v thu, nng sut ti a c th
ti 50 tn/ha.
g) Ging du Sa nh lun
L ging du mi nhp t Trung Quc, hin nay c trng nhiu ti Sn
La, Lm ng, Qung Ngi, Bnh nh v ng Nam B. Nng sut rt cao t
trn 35 tn/ha.
2.1.2. Tnh hnh trng trt v s dng l du mt s tnh ca Vit Nam hin nay
Vit Nam l nc giu truyn thng vi ngh trng du nui tm, tuy
cng c nguy c thu nh dn do ngi dn khng khng th duy tr thu nhp n
nh t ngh ny nhng vi chin lc pht trin ca nh nc nhng nm gn
y v nhng nm ti trong c nh hng thc y s pht trin ngnh du
tm t th trong tng lai sn lng l du tm ca Vt Nam s rt di do.
Theo s liu thng k nm 2008 ca Cc Trng trt - B Nng nghip v Pht
trin nng thn th c th thy l cy du tm c trng trn hu khp cc min
ca t nc ta, t min Bc, min Trung n min Nam, trong sn lng tp
trung ch yu ti min Bc, min Trung v Ty Nguyn vi din tch trn 16
nghn ha.

Bng 2.1. Din tch du tm chia theo vng sinh thi


(Tnh n thng 12 nm 2008)

TT

Vng Sinh thi

Din tch du (ha)

T l (%)

ng bng sng Hng

4.597

26,04

II

ng Bc

726

4,11

III

Ty Bc

386

2,19

IV

Bc Trung B

2.999

16,99

Duyn Hi Nam Trung B

1.388

7,86

VI

Ty Nguyn

7.137

40,43

VII

ng Nam B

410

2,32

10

0,06

17.653

100,00

VIII ng bng sng Cu Long


Tng cng

(Ngun : Tng cc thng k; S nng nghip v PTNT cc tnh)

Qua bng chng ta nhn thy cy du tm c trng khp ni trn c


nc, tuy nhin c 4 vng trng du tp trung l : ng bng Sng Hng, Bc
Trung B, Duyn hi Nam Trung b v Ty nguyn. Trong Ty nguyn l
vng sn xut tp trung ln nht c nc vi 7.137ha chim 40,43% din tch.
Vng c din tch t nht l ng bng Sng Cu long, ch c 10ha ti Tnh An
giang.
Do vy, ngoi vic s dng l du cho ngh nui tm th vic pht trin
cc sn phm mi c li cho sc khe cng ng t ngun nguyn liu l du
tm s l mt ng lc thc y s pht trin ca ngnh trng du, mang li
nhng gi tr kinh t cao hn cho ngi trng du.
2.1.3. c im, thnh phn ho hc ca l du
Trong thnh phn ca cy du ni chung v l du ni ring c cha mt
lng ln cc thnh phn dinh dng nh saccarit v cc axit amin, vitamin v
cc nguyn t vi lng v cc cht c hot tnh sinh hc.
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2.1.3.1. Flavon v flavon glycozit


L du cha cc thnh phn: rutin, quercetin, izoquercitin v quercetin-3triglucozit...
2.1.3.2. Steroit
Bao gm -sitosterol, stigmasterol, campesterol, -sitosteryl, -Dglucozit, mezoinositol v mt s hoocmon metamorphic c th l inokosteron v
ecdysteron.
2.1.3.3. Cc cht bay hi
Axit axetic, axit propionic, axit butyric, axit izobutyric, axit valeric, axit
izovaleric, axit caproic, axit izocaproic, methyl salicylate, guaiacol, phenol, ocresol, m-cresol, eugenol. Ngoi ra cn c axit oxalic, fumarat, axit tartaric, axit
xitric, axit succinic, axit palmitic, ethyl palmitat, henthriacontan v
hydroxycoumarin.
2.1.3.4. Saccarit v cc axit amin
Bao gm sacaroza, fructoza, glucoza v 17 loi axit amin nh axit aspartic,
axit glutamic. Hm lng cc axit amin chim 10,1 mg/100g l du kh, axit
khng 2.1.3.5. Vitamin v cc nguyn t vi lng
L du cha mt s vitamin nh A, B1 (0,59 mg/100g l kh), B2 (1,35
mg/100g l kh), C (31,6 mg/100 g l kh), axit nicotinic, caroten (7,4 mg/100g
l kh), cht x thc phm chim 52,9% trong x ha tan l 7,9%. N rt
giu canxi, kali, photpho, ngoi ra cn gm cc kim loi nng vt nh km,
ng, boron, mangan, magie, st.
2.1.3.6. Cc cht c hot tnh sinh hc
Trong l du cn cha nhiu cht alkaloid, c bit quan trng trong s
l DNJ (1-deoxynojirimycin).

Bng 2. 2. Thnh phn ha hc chnh ca l du (% cht kh)


Thnh phn

Hm lng

Protein (%)

32,8

Cht bo (%)

2,56

Cht x (%)

52,9

ng ha tan (%)

9,6

Nhm amino axit (mg/100g)

20,96

Vitamin B1 (mg/100g)

0,59

Caroten (mg/100g)

7,4

Chlorophyl (%)

0,01

Alkaloid (%)

0,42

Amyloza (%)

1,86

Sterol (%)

0,05

DNJ (%)

0,1

Fkavibe (%)

3,3

2.1.4. Alkaloid trong l du tm


2.1.4.1. Khi nim
Alkaloid l nhng hp cht hu c c cha d vng nit, c tnh baz. c
bit, alkaloid c hot tnh sinh l rt cao i vi c th con ngi v ng vt,
nht l i vi h thn kinh. Vi mt lng nh c alkaloid l cht c gy cht
ngi nhng li c khi n l thn dc tr bnh c hiu.
2.1.4.2. Tnh cht ca alkaloid
a)Tnh cht vt l
- Khi lng phn t: khong t 100 900
- Th cht: Phn ln alkaloid trong cng thc cu to c oxy thng th
rn nhit thng. Cc alkaloid th rn thng kt tinh c v c im

chy r rng, nhng cng c mt s alkaloid khng c im chy v b phn hy


nhit trc khi chy.
Nhng alkaloid th lng bay hi c v thng bn vng, khng b phn hy
nhit si nn c ly ra khi dc liu bng bay hi nc.
- Mi v: a s cc alkaloid khng c mi, c v ng v s t c v cay.
- Mu sc: Hu ht cc alkaloid u khng mu tr mt s t c mu vng.
- tan: Ni chung cc alkaloid dng baz gn nh khng tan trong
nc nhng tan trong cc dung mi hu c nh eter, cloform, benzen,
metanolMt s alkaloid do c thm nhm phn cc nh OH, nn tan c
mt phn trong nc hoc trong kim ( Morphin, Cephalin).
Ngc li vi baz, cc mui alkaloid ni chung tan c trong nc v
cn, hu nh khng tan trong dung mi hu c t phn cc.
C mt s ngoi l nh Ephedrin, Colchixin, Ecgovonin cc base ca
chng tan c trong nc, ng thi cng kh tan trong dung mi hu c, cn
cc mui ca chng th ngc li.
Da vo tan khc nhau ca alkaloid dng baz v dng mui m ngu
ta s dng dung mi thch hp chit sut, phn lp v tinh ch alkaloid.
b)Tnh cht ha hc
* Alkaloid ni chung c tnh kim yu l do trong phn t c nit. Ngi ta
c th tnh c kim ca cc cht v chia thnh:
+ Alkaloid c kim mnh th gi tr pKB<3.
+ Alkaloid c kim trung bnh th gi tr pKB: 3 7 (alkaloid trong h
c, thuc phin).
+ Alkaloid c kim yu th gi tr pKB: 7-10 (alkaloid trong v
canhkina).
+ Alkaloid c kim rt yu th gi tr pKB: 10-12 (alkaloid c nhn
purin).

Bn cnh cng c alkaloid khng c tnh kim nh: Ricinin, colchicin,


theobromin.
- Tc dng vi acid thng to mui tan trong nc v kt tinh.
Khi dng mui, cc alkaloid bn vng hn v khng b phn hu hoc
chuyn mu trong qu trnh bo qun. Ngi ta s dng tnh cht to mui ca
cc alkaloid chit sut, tinh ch alkaloid. Cc mui alkaloid c bo ch
thnh cc dng vin nn, vin nang, thuc tim lm thuc v bo qun lu
hn.
- Cc alkaloid kt hp vi kim loi nng (Hg, Bi, Pb) to ra cc nui phc.
- Cc alkaloid c phn ng tng t nhau nh i vi mt s thuc th, gi
tn chung l cc thuc th alkaloid. Nhng phn ng ny c chia lm 2 loi:
+ Phn ng to mu.
+ Phn ng to ta.
2.1.4.3. Cc alkaloid c trong l du tm
Trong thnh phn ho hc ca l du tm c cha mt lng ln cc cht
alkaloid, chim hm lng khong 0,52%. Trong bao gm rt nhiu cc hp
cht alkaloid khc nhau nh:
Bng 2.3. Thnh phn cc cht alkaloid c trong l du tm
T trng so vi alkaloid

STT

Hp cht alkaloid

HL trong l du (%)

DNJ

0,32

61,54

-sitosterol

0,046

8,07

Stigmasterol

0,004

0,07

Cc hp cht khc

0,2

30,69

TS (%)

Trong s cc hp cht alkaloid c trong l du tm th hp cht DNJ


chim hm lng ln nht v y cng l hp cht quan trng nht trong vic
iu tr v phng nga cn bnh tiu ng.

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2.1.5. Hp cht DNJ trong l du tm


2.1.5.1. Bn cht v cu trc ho hc
DNJ c bn cht l Polyhydroxylat alkaloid, ph bin vi cc tn gi nh
iminosugar hay azasugar l mt loi hot cht ang gy s ch mnh m i
vi khoa hc nh mt tin cht tim nng c th ng dng rng ri trong y hc,
cng ngh sinh hc v cng ngh thc phm trong vi nm gn y. Thnh phn
c bn ca cht ny l chui D- glucoza, trong vng pyranoza c phn t oxy
lin kt vi nitro. Polyhydroxylat alkaloid c cu trc tng t nh monosacarit
v c kh nng c ch cnh tranh i vi enzym - glucosidaza v - amylaza,
do vy c tc dng iu tr s mt cn i ca qu trnh trao i cht c lin
quan n cacbohydrat, cng nh l mt hot cht tim nng trong vic iu tr
nhiu loi bnh him ngho nh ung th, tiu ng, bnh lin quan n virus
(HIV, HBV...).
Hin nay mt lng ng k cc polyhydroxylat piperidin c bit
n, c cc cht c ngun gc t nhin v cc cht c tng hp. Trong s cc
hp cht gi ng th DNJ l mt alkaloid tn ti trong t nhin in hnh
vi hot tnh sinh hc ha hn nh c ch cc enzym - glucosidaza v amylaza tiu ha. Hp cht ny c cu to tng t nh phn t D- glucoza vi
mt nhm NH thay th cho nhn oxy ca vng pyranoza.

Hnh 2.2. Cu trc ha hc ca hp cht DNJ

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Hp cht DNJ t nhin ln u tin c phn lp t l du vo nm 1976.


Cht DNJ c ngun gc t nhin ny thc y tng rng ch n c
DNJ ca l du c th c tc dng lm gim s cao bt thng ca ng mu
v do ngn nga bnh ny.
2.1.5.2. Tc dng v c ch lm gim ng huyt ca DNJ
Hot cht 1- deoxynojirimycin (DNJ) trong thnh phn l du tm l mt
cht c ch mnh hot ng ca enzym - glucosamindaza, ngn nga phn ng
xc tc ca - glucosehydrolaza, do vy ngn cn hot ng v c ch s phn
gii tinh bt trong thc phm thnh ng n l glucoza v fructoza....Do ,
n ngn cn qu trnh to glucose ti thnh rut v gan, t lm gim lng
glucose i vo mu, c ch s tng ln nhanh ca ng mu ngay sau khi n.
Glucosaminidaza tham gia nhiu qu trnh sinh hc khc nhau, c th l
phn ng phn gii cacbohydrat v sinh tng hp glycoprotein. DNJ c tc dng
v hot enzym -glucosehydrolaza trong tt c cc ng vt c v. Cc kt qu
nghin cu cng cho thy rng DNJ c kh nng nng lm gim ng trong
mu bng cch lm gim kh nng tiu ha cacbonhydrat v hp th glucoza.
DNJ cng lin kt vi - glycosidaza ca maltaza, sucaraza v lactaza trong rut
non, do ngn chn qu trnh chuyn ha c cht thnh ng n gin v s
hp th ng vo mu, do vy hn ch s tng ng mu t ngt.
Cho n nay, l du tm l mt trong nhng ngun thc vt c pht hin
c cha DNJ kh cao . Bn cnh , trong thnh phn cao du tm cn cha
nhiu polyphenol m in hnh l resveratrol. Hot cht ny gip lm tng tnh
nhy cm ca th th insulin vi hormon, do lm tng phn hu glucose d
tha. Nh vy, chit xut du tm va c ch tng hp mi, va lm tng phn
hy glucose v lm h lng ng trong mu. Thm na, cc polyphenol cn
c tc dng chng oxy ho sinh hc mnh, gip chng li qu trnh peroxit ha
lipid, t gip ngn nga cc ri lon chuyn ha lipid nguy c gy bin
chng thnh mch ph bin bnh nhn T.

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Do c tnh u vit ca DNJ i vi bnh tiu ng, cng nh s sn c


ca n trong cc loi thc vt nh cy du, nn vic nghin cu ch bin thc
phm chc nng t l du, mt loi cy rt nhiu v ph bin mi ni trn t
nc ta l rt kh thi, d thc hin.
2.1.6. Mt s cng dng ca l du
Tt c cc b phn ca cy du, t l, r n qu u c dng lm
thuc vi nhng tc dng cha bnh rt khc nhau. Ngay c nhng loi cy hoc
con c lin quan n cy du tm nh cy k sinh trn cy du (tang k sinh), t
b nga trn cy du (tang phiu tiu).... cng c dng lm thuc.
Trong Y hc c truyn (YHCT), l du c gi l tang dip, cnh du
gi l tang chi, v trng r du gi l tang bch b, qu du gi l tang thm t.
L du v ngt ng, tnh mt, c tc dng b m, pht tn phong nhit, gii
cm, thanh nhit lng huyt, mt gan, mt phi... Ch tr cc chng mt ,
mt m, au nhc chy nc mt..., c th va ung, va nu nc ra
ngoi. L du c tc dng cha bnh m hi trm tr em. L du cn c tc
dng dng m. Thng c dng cha tng huyt p, mt ng, pht ban
chn, au mt ... Liu dng mi ngy t 6 - 12g. Trong Nam dc thn hiu,
Tu Tnh cng rt ch trng n vic dng l du cha bnh [1].
Theo Dc in Vit Nam: L du c cc cng dng nh s tn phong
nhit, thanh ph nhun to, thanh can, minh mc. Ch tr: Cm mo thanh nhit,
ph nhit ho ro, chng mt, nhc u hoa mt....
Theo cc nghin cu c xa nht ca ngi Trung Quc ch ra rng l
du c tc dng lm gim m mu, cn bng huyt p, lm gim lng ng
mu v tng cng qu trnh trao i cht, ngn nga qu trnh lo ha v tng
cng sinh lc.
Trong nhng nghin cu gn y, cc nh khoa hc cng b cc cng
trnh nghin cu v thnh phn, chc nng v c ch hot ng ca cc thnh
phn trong l du. Theo cc kt qu , h nhn thy rng l du cha mt

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lng ln cc thnh phn dinh dng v cc cht c hot tnh sinh hc, nht l
hot cht c kh nng lm gim lng ng mu, huyt p, m mu v duy tr
lo ha. c bit trong s l hot cht DNJ mt alkaloid m trong cc loi
thc vt v ng vt khc khng c, n c chc nng ch ng s tng ng
mu v phng nga bnh tiu ng.
Bng 2.4. Thnh phn dc tnh ca l du
Cc cht c dc tnh

Cht chnh

Tc dng tt cho sc khe

Alkaloid

DNJ

Gim ng mu

Steroid

- -sitosterol

Gim m mu

- stigmasterol
Axit -amino

Axit -amino

Butyric (GABA)

Butyric (GABA)

Nhm izoflavon

- Izoquercitrin

Gim huyt p
Chng oxy ha v lo ha

- quercitrin

2.2. Cc phng php tch chit cc hp cht alkakoid trong l du


Nh nu phn trn, trong s cc alkaloid ca l du tm th hp cht
DNJ l hp cht chim khi lng ln nht v c ngha quan trng nht trong
vic phng chng bnh tiu ng.
2.2.1. Phng php v iu kin chit xut l du
chit rt cc loi cht t l du mt cch hon ton v nhanh nht th
ngoi vic la chn dung mi phi to iu kin ti u cho qu trnh khuch tn.
- Da vo trng thi ca nguyn liu v c tnh ca dung mi trch ly,
ngi ta chia trch ly thnh 2 loi:
+ Trch ly tnh: Nguyn liu c nghin nh ti kch thc thch hp ri
ngm trong dung mi nhit phng, trong mt thi gian nht nh (c hai
u khng chuyn ng) trong sut qu trnh trch ly.
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+ Trch ly ng: Dung mi hoc nguyn liu chuyn ng hoc c hai


cng chuyn ng nh cnh khuy lm tng kh nng tip xc, tng khu nh
hiu sut trch ly cao hn.
- Da vo phng php v s bc trch ly c th chia trch ly thnh trch
ly gin on mt bc, nhiu bc v trch ly lin tc.
+ Trch ly mt bc: Ton b qu trnh c thc hin trong mt thit b
trch ly, nguyn liu v dung mi ch tip xc mt ln, phng php trch ly ny
thng cho hiu sut thp.
+ Trch ly nhiu bc: Nu h s phn b khng ln trch mt ln th
phi trch ly thm nhiu ln. Ngha l sau khi chit mt ln, trong dung dch cn
li mt lng cht tan ng k th thng ngi ta thm mt lng dung mi
chit mi v chit mt hay nhiu ln na. Hiu sut cao hn hiu sut chit n
nhng tn dung mi, thi gian v cng sut.
Tu thuc vo chiu chuyn ng ca dung mi v nguyn liu ta c th
trch ly nhiu bc xui chiu v trch ly nhiu bc ngc chiu.
Ngoi ra tu theo tnh cht ca nguyn liu v dung mi c th gia nhit
trong qu trnh trch ly. Nu nguyn liu hay dung mi t b bin i hay bin
i theo chiu hng c li, th khi gia nhit lm tng ho tan cc cu t vo
trong dung mi do rt ngn thi gian trch ly.
Mt s phng php trch ly c th:
Phng php ngm trong dung mi: Nguyn liu c nghin nh ti kch
thc thch hp v dung mi vo mt bnh kn nhit phng. Ngm trong thi
gian nht nh, Sau gn, p b ly dch chit. lng ni mt loi tp cht l
lng, ri lc ly dch trong. C th ngm n gin hoc ngm phn on.
- Ngm n gin: Ngm mt ln vi ton b lng dung mi
- Ngm phn on: Chia dung mi lm nhiu phn ngm vi nguyn liu,
sau tin hnh gn p nh trn ri tp hp dch chit li. Ngm phn on hiu
xut thu hi cao hn tuy nhin tn nhiu thi gian.

15

Phng php ngm kit: y l phng php chit xut bng cch cho

dung mi chy rt chm qua khi nguyn liu ng trong mt dng c c bit
gi l bnh ngm kit. Qu trnh chit xut khng c khuy trn. Trong phng
php ny nguyn liu cn kh v c mn thch hp. Sau lm m nguyn
liu bng cch cho chng ht m t dung mi ui ht khng kh trong
nguyn liu. Nguyn liu sau ht m c cho vo bnh dn u sau kho
bnh ri rt dung mi ngp nguyn liu, ngm trong khong thi gian nht
nh. M kho cho dch chit chy tng git vo bnh hng. Ch dung mi
ngp nguyn liu 2 3 cm.
2.2.2. Chn dung mi chit xut l du
Cc alkaloid c th c chit sut t nguyn liu di dng mui hoc
dng baz. Trong chit xut alkaloid t nguyn liu di dng mui s dng
cc dung dch axit hoc cc dung mi phn cc axit ho, cn chit xut
alkaloid t nguyn liu di dng baz s dng cc dung mi hu c sau khi
kim ho nguyn liu.
C th s dng mt trong ba phng php sau y chit xut alkaloid t
nguyn liu v loi bt nhng tp cht:
* Chit xut alkaloid bng dung mi hu c mi trng kim
Gm c hai bc:
Bc 1 Chit xut: Trc khi chit xut tin hnh kim ho nguyn liu
bng dung dch kim chuyn cc alkaloid dng mui sang dng baz (cc
alkaloid tn ti trong thc vt di dng baz v dng mui). Sau khi kim ho,
tin hnh chit xut alkaloid bng dung mi h c (thng dng chloroform,
dietylether, cn). Thu hi dung mi, thu c alkaloid ton phn.
Bc 2 Tinh ch: Chuyn cc alkaloid dng baz sang dng mui bng
cch ho tan alkaloid ton phn bng cc dung dch axit long nh axit sunfuric,
axit hydrochloric 5-10%. Lc ly dung dch axit. Kim ho dung dch axit
chuyn cc alkaloid t dng mui sang dng baz. lng, lc, thu c kt ta
alkaloid ton phn th.
16

Phng php ny thng c p dng trong nghin cu c bn chit


tch v xc nh cu trc ho hc, nh danh cc alkaloid cha bit. S dng
kim khc nhau ca cc alkaloid tch chng trong qu trnh kim ho dch chit
Nu mun thu c alkaloid tinh sch hn c th chit alkaloid t dung
dch axit kim ho bng dung mi t phn cc nh chloroform hoc hn hp
chloroform + dietylether.
Do phng php ny s dng nhiu dung mi hu c chit xut alkaloid
trc tip t nguyn liu, v vy t c s dng trong sn xut.
* Chit xut alkaloid bng dung dch axit long hoc cn axit ho
Bc 1 Chit xut: Tin hnh chit xut alkaloid bng dung dch axit
long nh axit sunfuric, axit hydrochloric (hoc cn axit ho). Thu hi dung
mi, thu c alkaloid ton phn.
Bc 2 Tinh ch: Kim ho chuyn cc alkaloid t dng mui sang
dng baz. Tin hnh chit xut alkaloid bng dung mi hu c (thng dng
chloroform, dietylether). Thu hi dung mi, thu c alkaloid th. Tip tc tinh
ch bng phng php kt tinh, thu c hn hp alkaloid tinh ch, hoc kt
tinh phn on c th thu c alkaloid chnh di dng tinh th.
Phng php ny c p dng nhiu trong sn xut v dung mi l cc
dung dch axit long hoc cn axit ho c gi thnh r v an ton.
* Chit xut alkaloid bng cn trung tnh
Bc 1 Chit xut: Tin hnh chit xut alkaloid bng cn. Thu hi dung
mi, c cao cn ton phn.
Bc 2 tinh ch: Chit alkaloid t cn ton phn bng dung dch axit
longit long, lc b ta, kim ho dch chit axit. lng ta alkaloid, lc, thu
c alkaloid ton phn. Tip tc tinh ch bng phng php kt tinh.
Phng php ny cng c p dng trong sn xut (tu theo loi nguyn
liu) nhng t hn phng php trn v dung cn trung tnh thng ko theo
nhiu tp cht, kh khn cho vic tinh ch sau ny.

17

2.3. Tnh hnh sn xut v tiu th cc loi thc phm chc nng cha bnh
tiu ng trn th gii v Vit Nam hin nay
2.3.1. Tnh hnh sn xut v tiu th cc loi thc phm chc nng cha
bnh tiu ng trn th gii
Bnh tiu ng l mt bnh nguy him, lm tng nguy c mc cc chng
bnh v tim, thn, thn kinh, m la, vt thng chm lnh, d nhim bnh.... S
ngi mc bnh tiu ng trn ton cu ang ngy cng gia tng.

Hin nay,

thuc iu tr bnh tiu ng tng nhanh v s lng, chng loi v nhm mc


tiu khng ch s tng nng glucose mu; phng nga v iu chnh cc ri
lon lipid, hot ng ca gc t do, t c th kim sot tt mc glucose mu v
ngn nga, hn ch cc bin chng c th xut hin bnh l tng glucose mu.
Trn th trng hin c rt nhiu loi thc phm chc nng phng nga
bnh tiu ng v sng lc c nhiu loi dc liu c tc dng rt tt vi
cn bnh ny, nht l tiu ng Tp II nh cy tri mu, nhu, mng chu,
mp ng, bng lng nc
Trn th trng th gii hin nay, c mt s sn phm chc nng c
lm t l du tm dng cho ngi b bnh tiu ng. Ti Trung Quc, Nht
Bn, cc cng ty nh Mori, Nangtong Sihai Plant Extract Co.Ltd a ra th
trng mt s sn phm chc nng c lm t l du tm nh tr du, m l
du, bnh ngt l du...c tc dng phng v cha bnh tiu ng. Cc sn
phm ny ang c ngi dn a chung.
2.3.2. Tnh hnh sn xut v tiu th cc loi thc phm chc nng cha
bnh tiu ng Vit Nam
T l bin chng ca bnh tiu ng ngy cng tng, do khng c pht
hin sm v iu tr kp thi. c tnh khong 44% ngi b bnh tiu ng nc
ta b bin chng thn kinh, 71% bin chng v thn, 8% bin chng v mt
Hin nay trn th trng nc ta c rt nhiu cc sn phm thc phm chc nng
chuyn bit cho ngi b bnh tiu ng, trong c mt s loi ph bin nh:

18

2.3.2.1. Diabetna (Cng ty dc phm ch Nhn)


y l thuc c bo ch t dy tha canh, dc liu qu him mi c
tm thy ti Vit Nam. Thuc c tc dng h ng huyt, n nh v kim sot
ng huyt, gim cholesterol mu, gip cho bnh nhn i tho ng kim
sot ng huyt mc an ton, gip phng nga bin chng tiu ng, gim
tc dng ph ca thuc iu tr ty y.
2.3.2.2. Nadia (Cng ty c phn dc phm Hong Giang)
Thnh phn ca thuc bao gm c: Chit xut t kh qua, c rt, hoi sn,
nm Linh chi, gip lm gim ng mu cao v hn ch mt s bin chng ca
bnh tiu ng.
2.3.2.3. Metabosol
L mt thc phm chc nng gm 8 loi tho dc qu nhm kch thch
cc c ch t nhin a n s cn bng ng trong c th. Tho dc trong
thuc c kh nng phc hi knh vn chuyn glucose trn mng t bo, lm tng
s nhy cm ca t bo vi insulin do c tc dng tng vn chuyn glucose
vo t bo s dng.
2.3.2.4. H tng ng
Thnh phn chnh ca thuc l axit - lipoic, cu k, mch mn, hoi sn,
nhu. Tc dng ca thuc da trn s kt hp gia acid lipoic vi cc cht
dc tho c tc dng iu ha ng huyt, bi b cc c quan.
2.3.2.5. Tiu ng nam dc (Cng ty c phn Nam Dc)
Thnh phn ca thuc bao gm cam tho, ct cn, mch mn, ng v t,
sinh a, thin hoa phn v cc ph liu va . Thuc c tc dng tng cng
bi b, phc hi chc nng cc c quan gan, thn, tuyn ty do c tc dng
trong h tr iu tr bnh tiu ng.
2.3.2.6. Ayubes (Cng ty Ph Hi)
Thnh phn bao gm cc loi dc tho sau: cao l dy tha canh, cao v
qu mp ng, cao cy xuyn tm lin, cao l tri mm, cao ht vi rng, cao
l cy su u, cao c hng ph (c gu).

19

Hnh 2.3. Mt s sn phm cho ngi bnh tiu ng


2.4. Tnh hnh nghin cu lm sng v tc dng ca cht chit l du i vi
s gim ng huyt
2.4.1. Tnh hnh nghin cu ngoi nc
T xa xa ngi Trung Quc s dng l cy du tm trong cc bi
thuc cha tr v ngn nga bnh tiu ng, tuy nhin cha c s cp no
ti cc thnh phn c tc dng m hon ton da theo kinh nghim.[17]
Trong nhng nm gn y, t cc cng trnh chuyn su, cc nh khoa hc
Nht Bn, Hn Quc, n cng b v thnh phn, dc tnh v c ch hot
ng ca cc thnh phn chc nng c trong l du tm. Cc kt qu nghin cu
cho thy trong l du cha mt lng ln cc thnh phn dinh dng v cc
cht c hot tnh sinh hc, nht l cc hot cht c kh nng lm gim lng
ng mu, huyt p, m mu v tr hon qu trnh lo ha. c bit l hp cht
DNJ - y l cht c chc nng ch ng s tng ng mu v phng nga bnh
tiu ng.
20

Nm 1976, ln u tin DNJ c tch t r v l ca cy du bi Yagi v


cng s. iu ny lm c s cho vic s dng cy du lm thc phm chc nng
c tc dng lm gim nng ng mu v ngn nga bnh tiu ng nh
vo s c mt ca hot cht DNJ trong thnh phn ca cy du tm.
Nm 2003, Jin-Won Kim dng sc k lng cao p nh lng thnh
phn hot cht DNJ trong l du vi tin cy v chnh xc cao [11].
Nm 2007, Nitra v cng s thc hin cc th nghim so snh thnh
phn DNJ trong l du tm cc gi khc nhau v nhn thy hm lng DNJ
c trong chi l cao hn l bnh t [16].
Cng theo nghin cu ca Lin-Ling Wang v Ze- Yang Zhou vo nm
2008, cho thy dch chit t l du tm c kh nng km hm enzym glycosidaza, gip lm gim hm lng ng trong mu c tc dng r rt n
vic h tr iu tr bnh tiu ng [14]. T cc kt qu nghin cu ny,
Kimura v cng s [13] nghin cu to ra bt chit l du tm c nng
DNJ 1,5% v tin hnh th nghim bt chit ny trn 24 ngi mnh khe bng
cch cho s dng cc lng bt chit khc nhau v sau ung 50g ng
sacaroza, hm lng ng mu c xc nh sau 30, 60, 90, 120, 150 v 180
pht th kt qu cho thy liu lng c hiu qu n vic hn ch s tng ng
mu l 0,8-1,2 g bt chit c nng DNJ l 1,5% tng ng vi 12-18 mg DNJ.
Tuy nhin mt cu hi c t ra l vic s dng bt chit giu DNJ c th gy
tc dng ph cho ngi s dng hay khng. kim tra iu ny tc gi nghin
cu th nghim trn 12 ngi mnh khe t nguyn mi ln s dng 1,2 g
bt chit l du nng 1,5% trc mi ba n (tc l khong 3,6 g/ngy) trong
38 ngy th thy rng hm lng ng mu ca h lun n nh gii hn bnh
thng, nh vy c th thy l bt chit l du s dng thng xuyn khng gy
hin tng h ng huyt. Kt qu ny cho thy ngi mnh khe nu dng
thng xuyn bt chit l du s c dng phng bnh m khng c tc dng ph
no, do vy c th coi bt chit l du nh mt loi thc phm chc nng an ton.

21

Mt nghin cu th nghim lm sng sn phm tr l du b dng Mori


chit xut t l du do cng ty sn xut phi hp vi trung tm nghin cu ng
dng thc vt thin nhin, trng i hc Y Phng Nam (tn c i hc Y khoa
Qun i s 1- Trung Quc) nh gi tc dng ca sn phm trn ngi. Kt
qu l vi liu lng 20ml/ngi/ngy, dng u n trong 3 thng, cn 3 thng
sau th ty theo biu mu ca ngi dng th cho thy hiu qu r rt, mc
ng mu ca bnh nhn tr v mc bnh thng l 50,88%.
Cc nghin cu trn ngi ny cho thy rng loi bt chit giu DNJ tch
chit c t l du c tc dng lm h thp lng ng mu, do loi sn
phm ny c th s dng trong vic h tr iu tr bnh tiu ng h khng ph
thuc insulin (tiu ng tup 2).
2.4.2. Tnh hnh nghin cu trong nc
Ti Vit Nam cha c cc nghin cu mt cch h thng v vn tch
chit hp cht DNJ t l du tm v dng sn xut cc thc phm chc nng.
Nm 2007, Vin Cng nghip thc phm (ch tr l TS.ng Hng nh)
thc hin ti Nghin cu cng ngh sn xut bt l du tm giu 1deoxynojirimycin [6], do thi gian thc hin ngn (01 nm) v kinh ph c hn
nn kt qu mi dng li quy m th nghim thm d.
Ngoi ra, cn c mt s cng trnh khc nghin cu v tch chit l du
tm ca tc gi Phm Thin Ngc, L Ngc Lin, i hc Y H Ni khi thc
hin ti Chit sut, xc nh hm lng polyphenol v nh gi tc dng
chng Oxy ha ca cc mu bt chit l du[4] vo nm 2005 v
TS.BS.Nguyn Quang Trung, bnh vin Ung B Qung Ninh khi thc hin
ti nh gi tc dng bt chit l du trn cc ch s lipid v trng thi chng
oxy ha trong mu chut nht trng gy ri lon lipid mu v i tho ng
thc nghim vo nm 2006 [5], tuy nhin y ch l nhng nghin cu v dc
tnh ca mt thnh phn khc trong l du.
Trc nhng tc dng ca l du ni chung v hp cht DNJ ni ring, cn
phi ng dng c sn phm bt l du tm giu DNJ ny to ra mt s sn
phm chc nng mang tnh hng ha vi mc ch phng chng, h tr iu tr
cho ngi bnh tiu ng vi tiu ch d s dng, gi thnh h nhm a dng
ha cc sn phm chc nng cho ngi bnh tiu ng trn th trng Vit
Nam, y ang l vn quan tm ca cc c quan chc nng.
22

Phn 3. I TNG - NI DUNG


PHNG PHP NGHIN CU
3.1. i tng v nguyn vt liu
3.1.1. i tng nghin cu
L du tm thu hi ti cc a phng c din tch v sn lng ln l
Thi Bnh, H Ni, Sn La, Lm ng tp trung ch yu vo 4 ging l H Bc,
Qu, VH13 v Sa nh lun
3.1.2. Ho cht
Cc ho cht xut x t Nht, Trung Quc, c bao gm: axit formic,
axetonitril, ammonium axetat, axit sulfuric, chloroform, diethylether, NH 4OH
m c, Na2SO4 khan, HC, axit axetic, Ethanol, ng asprtame, maltodetrin,
enzyme Ultra SPL,
3.1.3. Dng c v thit b
- Dng c: ng ong, phu thu tinh, phu chit, bnh nh mc.
- Thit b:
My HPLC- FL, Shimadzu, ct ODS-3.
Cn in t Presisa 62A, Thy in.
Thit b lc chn khng
Bnh ht m
My o hm m
Micropipet cm tay c
My ht chn khng - TQ.
My o mu MINOTA- CHROMAMETER CR200/231
Cn phn tch - SHIMADZU & MONO BLOC - Nht Bn
3.2. Ni dung
- Nghin cu xc nh ging, gi v phng php bo qun thch hp
- Nghin cu quy trnh sn xut bt l du c hm lng DNJ cao
- Nghin cu t l phi ch bt trit l du vi bt l du kh v vi cht
iu v
23

3.3. Phng php nghin cu


3.3.1.Phng php chung
V mt tng th ti s dng phng php thc nghim, c s h tr
ca cc l thuyt ton hc xc nh cc iu kin ti u trn mi quan h
gia cc yu t nh hng ng thi v kim chng cc c s gi thuyt.
Phng php ton hc cc thc nghim trong nghin cu tm ti u
Ti u ho mt s qu trnh, c bit l qu trnh trch ly i vi l du m
c th l xc nh cc gi tr ti u ca cc bin s nhit , thi gian v t l
nguyn liu/dung mi bng phng php quy hoch thc nghim.
Bng ngn ng, ti u ho qu trnh l tm gi tr ca cc yu t X i ti
qu trnh trch ly t hiu sut cao nht (tc l hm lng DNJ c chit tch ln
nht), ngha l cc hm mc tiu Yi t cc tr.
t c mc ch nghin cu chng ti chn ma trn DOEHLERT. Ma
trn ny cho php tm c vng ti u trong khong gii hn chn. Ma trn cho
php phn chia rt cn i cc im th nghim trong gii hn theo bt k hng
no. Da vo ma trn, ta c th thm cc bin s khc na m khng lm mt i tnh
ng n ca ma trn.
Trong ma trn ny, s ln th nghim N v cc bin s K c xc nh nh sau:
N= K2+ K+1.
Trong trng hp K= 3 th s im th nghim cn thc hin l N=13.
Vi 3 yu t nh hng, ma trn c xc nh nh hnh sau:

24

Tt c cc im chn c xc nh theo phng trnh hi quy c dng sau:


Y= b0+ b1X1+ b2X2+ b3X3 + b11X12+ b22X22+ b33X32+ b12X1X2+ b13X1X3 + b23X2X3.
Trong : Y- Hm mc tiu ( hay cc i lng cn xc nh)
b- Cc h s hi quy
X- Cc bin s.
Qu trnh tnh ton v kt qu c x l bng my tnh theo chng trnh
NEMROD- New Efficient Methodology For Research Using Optimal Design.
3.3.2. Phng php thit k th nghim v x l s liu
- Thit k th nghim theo phng php yu t ngu nhin hon ton
- Kim tra gi thit thng k theo ANOVA
3.3.3. Phng php phn tch cc ch tiu ha l
- Xc nh mu sc ca nguyn liu v sn phm trong qu trnh nghin cu
bng my o mu MINOTA.
- Xc nh hm lng cht kh ha tan bng refactometer (chit quang k)
theo TCVN 5610-1991.
- Xc nh m theo TCVN 5613-1991.
- Xc nh hm lng alcaloit ton phn bng sc k lng cao p.
- Xc nh hm lng DNJ bng phng php sc k lng cao p: Xc nh
hm lng DNJ bng phng php to dn xut vi 9-fluorenylmethyl
chloroformat trn h thng HPLC pha ngc.
- Xc nh s lng nm men, nm mc theo TCVN 4886-89.
3.3.4. Phng php nh gi cm quan
S dng php th th hiu nh gi mc a thch i vi sn phm
(theo thang im hedonic 1-9)
3.3.5. Phng php c th
Cc th nghim u c lp li ba ln.
Ni dung 1: Nghin cu ging, gi l du v phng php bo qun thch
hp

25

Trn c s kho st, ta la chn 4 ging c nng sut v din tch trng
ln, phn tch xc nh ging c hm lng DNJ cao.
V gi: Tin hnh xc nh cc gi khc nhau t l non (l 1 4 t nn
tr xung) thun thc (t l th 5 ti l th 9) l gi (t l th 9 xung gc)
Th nghim1: Nghin cu nh hng ca trng thi nguyn liu n s thay i
hm lng DNJ
Tin hnh phn tch cht lng ca l du sau khi thu hi hai trng thi
CT1: L du ti
CT2: L du kh, m 10%
Bo qun l du iu kin thng trong khong thi gian t 1-10 ngy.
Sau , xc nh hm lng alkaloid TS trong l du trong khong thi gian bo
qun, kim tra 2 ngy/ln.
Th nghim 2: Xc nh phng php lm kh thch hp
Tin hnh lm kh l du sau thu hi bng 3 phng php
CT1: Phi nng
CT2: Sy i lu nhit 60-70oC
CT3: Sy lnh n m n khi l du c m 10%
Sau l du kh c ng trong bao b PE buc kn v bo qun trong
iu kin thng.
Tip tc theo di s thay i hm lng alkaloid TS trong l du kh 3
phng php trong thi gian bo qun 3 thng, kim tra 1tun/ln.
Cc ch tiu kim tra hm lng alkaloid tng s
Ni dung 2: Nghin cu quy trnh cng ngh sn xut bt l du tm giu DNJ
Th nghim 1: Nghin cu xc nh phng php trch ly thch hp
Phng php: L du xay nh sau khi x l enzim cc iu kin thch hp (c
c t th nghim 1) tip tc c kho st hiu sut trch ly bng 3 phng
php trch ly ph bin p dng vi vic chit dc liu, gm 3 cng thc TN

26

- Cng thc 1: Phng php ngm vi dung mi


- Cng thc 2: Phng php ngm kit bng dung mi
- Cng thc 3: Phng php trch ly Soxhlet
* Cc ch tiu kim tra: Hm lng alkaloid v DNJ trong dch chit (hay hiu
sut trch ly)
Th nghim 2: Nghin cu la chn loi v nng dung mi trch ly thch hp.
* Phng php: L du xay nh c chia thnh cc mu c khi lng nh
nhau ri tin hnh trch ly trong cng mt khong thi gian, cng nhit , cng
t l dung mi/nc chit v cng phng php trch ly vi cc loi dung mi
c cc nng sau:
Loi dung mi: Do sn phm cui cng ca qu trnh tch chit c s
dng lm thc phm chc nng nn m bo an ton v sinh thc phm v
n gin cho qu trnh chit tch d kin s dng 03 loi dung mi l nc,
ethanol trung tnh, ethanol axit ha (y l cc dung mi thng c s
dng trong qu trnh chit xut cc dc liu)
Nng dung mi (i vi dung mi ethanol trung tnh v ethanol axit
ha): 30%V- 96%V.
Trn c s xc nh hm lng DNJ c trong dch chit cc mu m xc
nh c loi dung mi cng nh nng dch chit thch hp nht. Tuy nhin
trong qu trnh ny cng cn ch ti hiu qu kinh t, y cng c coi l
mt tiu chun la chn loi dung mi thch hp.
Th nghim 3: Nghin cu xc nh nhit trch ly, t l dung mi/ nguyn liu
v thi gian trch ly thch hp.
* Phng php: Tin hnh xc nh min nh hng ca tng yu t trong qu
trnh trch ly (nhit trch ly, t l dung mi/ nguyn liu, thi gian trch ly)
bng cch thc hin cc th nghim thm d n yu t nhm xc nh vng dng
ca tng tham s cng ngh, c th:
+ Nhit trch ly (X): T 300C- 1000C.

27

+ Thi gian trch ly (Y): 4 24 gi.


+ T l l du/dung mi (Z): 1/6, 1/8, 1/10, 1/12.
T s dng phng php ton hc (nh nu) tm min ti u ca cc
yu t trn.
Th nghim 4: Nghin cu xc nh s ln trch ly thch hp.
* Phng php: Tin hnh trch ly vi cc ln trch ly n =1 - 4 ln cc iu
kin chn (c c t th nghim 4).
Da vo hiu sut trch ly (hay hm lng DNJ c trong dch chit) kt hp
vi hiu qu kinh t xc nh s ln trch ly thch hp.
Th nghim 5: Nghin cu xc nh cht mang v nng cht mang thch hp
Dch chit l du c c cn ti 19.60bx. Sau ly mi mu dch chit
c th tch l 100ml c b sung cc cht mang: maltodextrin, ng isomalt,
tinh bt bin tnh ba nng kho st ln lt l: 4,5,6% c sy phun
cng mt ch sy nh nhau. Xc nh Hm lng DNJ/g sn phm, m,
mu sc, mi v, bm dnh, kh nng ht m ca sn phm, kh nng ha tan
trong nc t xc nh c cht mang v nng cht mang thch hp. Cc
th nghim u c tin hnh trong iu kin sy phun:
- Lu lng nhp liu: 432ml/h
- p sut kh nn: 8bar
- Nhit u vo: 125oC
Th nghim 6: Xc nh nhit sy phun thch hp

Dch l du sau khi trch ly c c cn ti 19.6oBx, sau tin hnh ly


mi mu dch chit c th tch l 100ml c b sung cht mang v nng
cht mang thch hp t th nghim 1 ri tin hnh sy phun cc khong nhit
khc nhau: 115,125,135,145,155.
Xc nh Hm lng DNJ/g sn phm, m, mu sc, mi v, bm
dnh, kh nng ht m ca sn phm, kh nng ha tan trong nc t xc
nh c nhit sy thch hp. Cc th nghim u c tin hnh trong iu
kin sy phun:
28

- Lu lng nhp liu: 432ml/h


- p sut kh nn: 8bar
Th nghim 7: Xc nh lu lng nhp liu thch hp cho sy phun bt chit l
du tm
Dch l du sau khi trch ly c c cn ti19.6oBx, sau tin hnh ly
mi mu dch chit c th tch l 100ml c b sung cht mang v nng
cht mang thch hp t th nghim 1 ri tin hnh sy phun cc lu lng
nhp liu khc nhau:
Xc nh Hm lng DNJ/g sn phm, m, mu sc, mi v, bm
dnh, kh nng ht m ca sn phm, kh nng ha tan trong nc t xc
nh c lu lng nhp liu thch hp. Cc th nghim u c tin hnh
trong iu kin sy phun:
- Nhit u vo: nhit thch hp c tm t th nghim 2
- p sut kh nn: 8bar
* Cc ch tiu xc nh: Hm lng DNJ/ml sn phm, mu sc, mi v sn
phm.
Ni dung 3: Nghin cu t l phi ch gia bt chit l du vi bt l du kh
v cht iu v
Th nghim 1: Nghin cu t l phi ch bt l du v l du kh
T hm lng DNJ c trong l du kh v trong bt chit l du ta phi ch
c hm lng DNJ theo yu cu ri em nh gi cm quan
CT
CT1
CT2
CT3
CT4
CT5
CT6
CT7
CT8
CT9
CT10

T l bt l du
kh(%)

T l bt chit
(%)
98
96
94
92
90
88
86
84
82
80

2
4
6
8
10
12
14
16
18
20

29

Hm lng DNJ
(mg/ti 3g)
7.5
8.4
9.4
9.8
11.4
12.3
13.3
14.3
15.2
16.2

Th nghim 2: Nghin cu t l phi ch cc cht iu v.


S dng tr c phi ch thu c th nghim trn. Ta b xung cht iu v
l ng Isomailt theo cc t l 4 - 10% theo cc cng thc di y ri nh
gi cm quan.
CT

T l ng Iso malt (%)

CT1

4.0

CT2

4,5

CT3

5.0

CT4

5.5

CT5

6.0

CT6

6.5

CT7

7.0

CT8

7.5

CT9

8.0

CT10

8.5

CT11

9.0

CT12

9.5

CT13

10

30

Phn 4. KT QU NGHIN CU V THO LUN


4.1. Nghin cu ging v gi l du thch hp
Theo s liu thng k nm 2000 ca Cc trng trt B Nng nghip v
Pht trin nng thn th c th thy l cy du tm c trng trn hu khp cc
min ca t nc ta, trong sn lng tp trung ch yu nht ti min Bc, min
Trung v Ty Nguyn. Trong mi a phng trng loi ging cy khc nhau,
cho nng sut v cht lng khc nhau. Tuy nhin do gii hn thi gian v phm vi
ti nn chng ti la chn ngun nguyn liu l du ca tnh Thi Bnh vi 4
ging du l H Bc, Qu, Sa nh lun v VH13 3 gi khc nhau l l non, l
thnh thc v l gi. Qua kho st th bng vic la chn l du em phn tch
nng DNJ bng phng php sc lng cao p ti Vin cng nghip thc
phm, kt qu ch ra nng DNJ trong l du tnh Thi Bnh t 0,32%
Do vy chng ti chn l du thu hi ti Thi Bnh lm nguyn liu
cho nghin cu trong ti ny v l du vng ny c nng DNJ cao v y
cng l vng giu truyn thng trng du nui tm nn thun tin trong vic
pht trin vng nguyn liu.
Tuy nhin do iu kin v thi gian th nghim, chng ti ch xc nh c
hm lng alkaloid TS thay cho vic nh lng chnh xc hm lng DNJ
4.1.1. nh hng ca gi thu hi n hm lng alkaloid TS
Trong cng mt ging du th cc non gi khc nhau, hm lng
alkaloid TS cha trong cng khc nhau. Vi ging du Qu, khi thu hi
chng ti phn thnh ba loi l: l non (l th 14 k t nn tr xung), l bnh
t (l th 58 k t nn xung) v l gi (t l th 9 xung gc). Kt qu phn
tch hm lng alkaloid TS c ch ra trn bng 4.1

31

Bng 4.1. nh hng ca gi thu hi n hm lng alkaloid TS


trong l du Qu
non gi

Hm lng alkaloid TS (%)

L non

0,48

L bnh t

0,46

L gi

0,23

5%LSD

0,002

CV%

0,3

T kt qu bng 4.1, chng ti thy s sai khc v hm lng alkaloid


trong l du non v l bnh t l khng ln. iu ny cng ph hp vi nghin
cu ca Nitra v cng s (2007) khi thc hin cc th nghim so snh thnh
phn DNJ trong l du tm cc gi khc nhau v nhn thy hm lng DNJ
c trong chi l cao hn l bnh t [16].
Tuy nhin do s lng l non rt t, khong 3 - 4 l, hn na l nhng l
mi hnh thnh nn khi lng cng thp, sn lng thu hi khng cao. Trong
khi , l bnh t c khi lng nhiu hn, mt khc khi thu hi vn m bo
cy ra l u n, do vy chng ti s dng l bnh t cho qu trnh tch chit.
4.1.2. Nghin cu nh hng ca trng thi nguyn liu n s thay i
hm lng DNJ
Bng 4.2. S bin i hm lng alkaloid ca l du ti v l du kh
trong 10 ngy theo di

Ngy
0 ngy
2 ngy
4 ngy
6 ngy
8 ngy
10 ngy

L du ti (10g)
Khi lng
m
alkaloid ton phn
(%)
(g)
0.074
70.62
0.137
46.59
0.165
33.24
0.197
19.06
0.213
14.48
0.220
12.44

32

L du kh (10g)
Khi lng
m
alkaloid ton phn
(%)
(g)
0.227
10.23
0.226
10.23
0.224
10.46
0.22
10.58
0.221
10.72
0.220
10.89

Da trn bng 4.2, chng ti nhn thy, khi lng alkaloid TS trong l du
ti sau thu hi c s bin ng mnh trong 10 ngy theo di. iu kin
thng, c th thi gian bo qun cng di th m cng gim v hm lng
alkaloid tng ln c th thy m ca l du t l nghch vi hm lng
alkaloid. iu ny chng t hm lng alkaloid t b bin ng.
Trong 10 ngy theo di th khi lng alkaloid lin tc tng. Nguyn
nhn l do bo qun iu kin thng, l du ti b mt nc dn ti gim
hm lng nc. n ngy th 10 th l du ti c kh dn tng ng
vi l du c lm kh ti m 10%.
Khi l du c lm kh chng ta cng d bo qun hn do hm m
thm vi sinh vt kh pht trin, khi lng l nh hn d dng ct gi trong cc
kho cha. Mt khc, trong thc t khng th s dng nguyn liu ti lm
nguyn liu cho c qu trnh sn xut v nguyn liu ti c thi v nht nh,
nu mun gi c trng thi ti trong thi gian di phi c ch bo qun,
gy tn km m cht lng vn gim.
Nh vy, chng ti thy cn sy kh l du bo qun nguyn liu n
gin v lu di.
4.1.3. Xc nh phng php lm kh nguyn liu thch hp
C rt nhiu phng php sy kh, trong khun kh ti v kh nng
thc hin chng ti la chn ba phng php l: Phi nng, sy i lu nhit
60 700C v sy lnh a nguyn liu v m 10%.

33

0,250

Hm lng DNJ (%)

0,200

0,150

0,100

0,050

0,000
1

10

11

12

13

Thi gian (tun)


Hong ho t nhin

Sy i lu

Lanh ng

Hnh 4.1. thi s bin i hm lng alkaloid TS qua 1 thng theo di


ca l du kh
Kt qu cho thy hm lng alkaloid tng s gim dn theo thi gian bo
qun, tuy nhin mc gim trong 1 thng theo di l khng ln. Trong ba
phng php th phng php sy lnh ng v sy i lu cho hm lng
alkaloid n nh hn, nhng s chnh lch ny rt nh. iu chng t khi
a l du v m 10% th thu c hm lng alkaloid TS n nh. Mt
khc, trong cc phng php sy kh chng ti thy phi nng c nhiu u im
v khng tn nng lng, vi vic thu hoch l du hai v xun, h th thi tit
lun m bo nhit 28 33oC nn ch sau t 3 5 ngy l du c th t ti
kh cn thit. Trong khi phng php sy i lu v sy lnh cho cht
lng l du n nh v ng u hn, nhng tiu tn nhiu nng lng, nhng
khng ph thuc vo th tit.
Nh vy xt v cht lng l du v hiu qu kinh t, trong ma nng nn
s phng php phi nng. Trong ma ma m l du ln, nhit khng
thun li chng ta nn s dng phng php sy i lu.

34

4.2. Nghin cu quy trnh cng ngh sn xut bt l du tm giu DNJ


4.2.1. Nghin cu phng php trch ly thch hp
Trong nghin cu ca ti chng ti la chn so snh hiu sut chit
gia ba phng php trch ly l phng php ngm nguyn liu trong dung mi,
phng php ngm kit v phng php trch ly Soxhlet.
Kt qu phn tch hm lng alkaloid TS, hm lng DNJ thu c ba
phng php c th hin trong bng 7
Bng 4.3. nh hng ca cc phng php trch ly n hm lng alkaloid
c trong l du
CT1

CT2

CT3

67.55

72.25

85.17

Hm lng DNJ (%)

0,017b

0,018ab

0.019a

Hm lng DNJ (%)

CV (%)

4.605

4.605

4.605

CV (%)

Cng thc
Hiu sut thu hi
alkaloid (%)

Cng thc
Hiu sut thu hi
alkaloid (%)

Ghi ch : Trong cng mt hng, cc kt qu c chung t nht mt ch ci th khng khc


nhau c ngha mc p<0,05
CT1: Phng php ngm kit
CT2: Phng php ngm trong dung mi
CT3: Phng php soxhlet

Kt qu bng cho thy hm lng alkaloid thu c trong l du bng


phng php Soxhlet cho hiu sut chit alkaloid cng nh DNJ trong sn phm
cao hn so vi phng php ngm kit v ngm trong dung mi. Tuy nhin
phng php ny khng th p dng trong quy m sn xut v n mt nhiu thi
gian, tn nng lng v i hi trang thit b phc tp.
Trong hai phng php cn li th phng php ngm kit cho hm lng
alkaloid thu c cao hn phng php ngm trong dung mi, hn na phng
php ngm kit c u im tn t dung mi m vn chit kit c hot cht.

35

Do vy chng ti la chn phng php ngm kit l phng php chit


hot cht DNJ trong l du tm.
4.2.2. Nghin cu la chn loi v nng dung mi trch ly thch hp
Sn phm chit xut c dng lm ung v thc phm nn khng
c php dng cc ho cht c hi cho sc kho. V vy trong ngnh thc
phm th loi dung mi duy nht c s dng l dung dch cn v ch dung mi
ny mi m bo c yu t an ton thc phm cho ngi s dng. Cn 90%V
c phn cc km nn ch ho tan c cc cht kh phn cc, cn 30%V c
phn cc gn nh tng ng vi nc nn c kh nng ho tan cc cht
c phn cc mnh, trong khi nhiu loi cht c kh nng ho tan mnh
trong dung mi c phn cc mc trung bnh nh cn 70%V. Da trn
phn cc ca cn bc u nghin cu nh hng ca nng cn n hiu
sut trch ly cc hp cht alkaloid trong l du.
V hm lng DNJ trong l du tm rt thp ch xp x 0,18%, trong khi
mc tiu ca ti l chit xut sn phm bt chit l du vi hm lng
DNJ t 0,5 n 1% c th to ra sn phm tr dnh cho ngi b tiu ng.
V vy, vic chit xut khng ch nh hng vo chit xut c nhiu alkaloid
m cn phi thu c sn phm tan tt trong nc, cho dung dch trong, hp dn
ngi s dng. c bit alkaloid dng baz hu nh khng tan trong nc,
trong khi mui ca cc alkaloid li tan tt trong nc. Li dng tnh cht to
mui vi cc axit ca cc alkaloid la chn phng php chit xut thch
hp, c th l chit xut bng cn trong mi trng axit c th cho sn phm t
cc yu cu nu trn. Trong s cc axit c th la chn axit axetic mt axit
c dng trong thc phm, s an ton hn cc axit v c khc axit ho cn,
ngoi ra y l axit bay hi nn c th d dng loi b khi c c dch chit. Do
vy ngoi 3 dung mi cn 30, 50, 70, 90%V chng ti s dng c dung mi cn
b axit ho bng axit axetic 1% cc nng 30, 50, 70, 90%V xc nh xem
loi dung mi no l thch hp nht trch ly alkaloid trong l du. Kt qu thu
c trnh by bng 4.4.

36

Bng 4.4. nh hng ca loi v nng dung mi n hm lng alkaloid


TS v DNJ thu c trong l du
Hiu sut thu hi

Hm lng

alkaloid(%)

DNJ(%)

CT1

75,18

0.015de

2,977

CT2

83,99

0.016dc

2,977

CT3

86,64

0.016bc

2,977

CT4

72,54

0.014e

2,977

CT5

80,47

0.017ab

2,977

CT6

83,41

0.017ab

2,977

CT7

85,16

0.018a

2,977

CT8

87,81

0.018a

2,977

ng thc

CV(%)

Ghi ch : Trong cng mt hng, cc kt qu c chung t nht mt ch ci


th khng khc nhau c ngha mc p<0,05
CT1: Dung mi cn 30%V

CT5: Dung mi cn 30%V c 1% axit axetic

CT2: Dung mi cn 50%V

CT6: Dung mi cn 50%V c 1% axit axetic

CT3: Dung mi cn 70%V

CT7: Dung mi cn 70%V c 1% axit axetic

CT4: Dung mi cn 90%V

CT8: Dung mi cn 90%V c 1% axit axetic

CT1: Dung mi cn 30%V

CT5: Dung mi cn 30%V c 1% axit axetic

Kt qu cho thy v mt hiu sut th cn 70%V trung tnh v axit ho


u cho hiu sut thu hi alkaloid ton phn cao (85,15 86,67%) nhng sau
qu trnh chit th vic loi tp cht thu dch trong rt kh khn (dch chit c
nhiu sp, nha, chlorophyl v cc cht ny ho tan tt trong dung mi ny do
vy rt kh lc dch chit). Cn 90%V cho hiu sut thu hi thp nht, c th
thy y khng phi l dung mi thch hp cho vic chit xut. Cn 30% trung
tnh v axit ho u cho dch chit lc d dng, t nha v chlorophly. c bit
nhn thy dch chit cn c axit ho cho hiu sut thu hi alkaloid tng ln
ng k so vi khi dng dung mi cn 30%V trung tnh t 74,85% ln 80,83%,
37

iu ny cho thy tc dng rt tt ca vic axit ho dung mi chit. Nguyn


nhn c th l do khi dng cn axit, tp cht chit ra t hn, do t gy cn tr
vic ho tan chit xut alkaloid ton phn cng nh DNJ t l du.
Ngoi ra v cm quan s b sn phm thu c th thy rng sn phm
chit bng cn 70%V trung tnh v cn 70%V axit ho c mi thm, v nht,
d ht m thnh dng chy nho, khi ho trong nc nng cho dung dch trong
sut. Cn sn phm chit bng cn 30%V trung tnh v cn 30%V axit ho
c mi thm, v nht, d ht m nhng ch b vn cc ch khng thnh dy chy
nho nh bt chit bi cn 70%V, khi ho trong nc nng cng cho dung dch
trong sut.
i vi dung mi axit ho th theo mc tng dn ca nng cn th
hiu sut thu hi alcaloit l tng ln, tuy nhin nng dung mi cn cng cao
th vic tch cn khi dch sau khi chit l kh khn hn nng cn thp, iu
ny cho thy vic chit xut vi dung mi cn 30%V gip thao tc cng ngh
c d dng hn. Khi chit nng cn 70%V th hiu sut thu hi alcaloit
t 85,15% trong khi nng cn 30%V th hiu sut alkaloid l 80,83%, s
tng ln v hiu sut ny so vi vic tng gi thnh khi dng dung mi cn
70%V thay cho 30%V th l khng c hiu qu kinh t.
Do vy cn nhc c yu t cht lng cm quan bt chit v ngha kinh
t th c th thy vic chn dung mi cn 30% V c axit ho bng axit nng
1% l hon ton thch hp cho qu trnh tch chit alcaloit l du.
4.2.3. Nghin cu xc nh nhit trch ly, t l dung mi/nguyn liu v
thi gian trch ly thch hp
4.2.3.1 Nghin cu xc nh nhit trch ly thch hp
T cc kt qu nghin cu phn trn, trong th nghim tip theo ny
chng ti ch kho st nh hng ca nhit chit sut n vic chit tch
alkaloid TS. Chng ti tin hnh tch chit dch l du cng iu kin kch
thc nguyn liu, dung mi, t l dung mi/nguyn liu, s ln chit, vi

38

khong nhit trch ly t 2590oC, thng qua 4 khong nhit 25-30oC


(nhit phng), 45-50oC, 65-70oC, 85-90oC. Kt qu xc nh hm lng
alkaloid TS c hin trn bng 4.5
Bng 4.5. nh hng ca nhit chit xut n hm lng alkaloid TS v
DNJ thu c trong l du
Cng thc

CT1

CT2

CT3

CT4

Hiu sut thu hi alkaloid(%)

80,76

81.35

81,64

82,23

Hm lng DNJ(%)

0,017a

0,017a

0,017a

0,018a

CV(%)

3,707

3,707

3,707

3,707

Qua bng 4.5, chng ti thy khi nng nhit chit xut ln 65 700C
hoc 85 900C th hm lng alkaloid TS ch tng nh. Nh vy vic tng nhit
chit xut hu nh khng lm tng thm s trch ly alkaloid, thm vo gia
nhit s lm tng chi ph sn xut ln ng k.
Theo kt qu nghin cu ca Kimura v cc cng s khi tin hnh tch
chit v thu nhn hp cht DNJ c nng cao 0,3-0,5% kt lun nhit
trch ly ti u nht l 32oC [15]. Theo nghin cu ca Nitra (2007) khi so snh
hm lng DNJ cc gi ca nguyn liu tin hnh nhit 28oC [16].
Nh vy qu trnh chit alkaloid t l du ch nn tin hnh 25 30oC
(nhit phng) l thch hp.
4.2.3.2. Nghin cu xc nh t l dung mi/ bt l du thch hp
Sau khi chn c dung mi thch hp l cn 30%V axit ho bng 1%
axit axetic v nhit chit thch hp l 25oC 30oC chng ti tin hnh kho
st nh hng ca t l dung mi/nguyn liu. Vi vic la chn kch thc
nguyn liu l du c xay th qua ry c ng knh 1mm, chng ti thy cn
t l dung mi/nguyn liu ti thiu l 8:1 n 16:1 ngp nguyn liu, thun
li cho qu trnh chit tch sau ny. V vy chng ti kho st vic chit tch
hm lng alkaloid TS cc t l dung mi/nguyn liu l 6:1, 8:1, 10:1 v 12:1.

39

Kt qu xc nh hm lng alkaloid tng s v DNJ c trnh by trong


bng 4.6
Bng 4.6. nh hng ca t l dung mi n hm lng alkaloid TS v
DNJ thu c t l du
Cng thc
Hiu

sut

thu

hi

alkaloid(%)
Hm
DNJ(%)
CV(%)

lng

CT1

CT2

CT3

54,85

65,15

80,61

0,014c

0,015bc

0,018ab

3,707

3,707

3,707

T bng 4.6, chng ti thy rng khi tng t l dung mi so vi nguyn liu
th hm lng alkaloid tng s thu c c tng ln.
Khi s dng t l dung mi/ bt l du l 10:1 th hiu sut chit tng ln
ng k so vi t l dung mi 6:1 v 8:1, nhng khi tng n t l 12:1,th hm
lng alkaloid n nh, khng tng thm so vi t l 10:1.
Mt khc t l ny hm lng alkaloid TS thu c trong qu trnh chit
tng thm khng nhiu m phi tn thm gp 1,52 ln lng dung mi, sn
phm li c nguy c ln thm tp cht, ngoi ra li tiu tn nng lng c c
dch chit cho nn tnh v ngha kinh t l khng c li.
Nh vy, khi dng l du c xay th qua ry c ng knh 1mm
trch ly th nn dng t l dung mi/nguyn liu l 10:1 l tt nht, cn nu nh
dng cc loi bt l du c kch thc nghin th hn th c th tng thm lng
dung mi m bo ton b nguyn liu c ngp trong dung mi.
4.2.3.3. Nghin cu xc nh thi gian trch ly thch hp
T cc kt qu nghin cu phn trn, chng ti thy rng vic chit xut
alkaloid TS v DNJ mi ln trong 24 gi cho kt qu rt tt . Tuy nhin
kim tra xem thu c hm lng alkaloid TS cao th cn thit phi tin hnh

40

chit xut nhiu ln hn na khng, chng ti kho st thi gian cho mi


ln chit thay i t 4 gi n 24 gi.
Kt qu nh gi hm lng alkaloid TS v DNJ thu c trong qu trnh
chit c ch ra trong bng 4.7
Bng 4.7. nh hng thi gian chit n hm lng alkaloid TS v DNJ
thu c trong l du
Cng thc

CT1

CT2

CT3

CT4

CT5

Hiu sut thu hi alkaloid(%)

61,97

68,43

76,36

80,47

80,76

Hm lng DNJ (%)

0,013c

0,014bc

0,015b

0,018a

0,018a

Cv(%)

3,707

T bng 4.7 cho thy nu ch chit 4h/ln chit hay 10h/ln chit th cha
th chit c ti a lng alkaloid c trong l du.
Do vy thu c hm lng akaloid TS ti a c trong l du th cn
thit phi . Kt qu cho thy mun tng hm lng DNJ v alkaloid thu c
trong l du th khi chit xut cn thit phi ko di thm thi gian trong mt ln
chit. T kt qu thu c nhn thy thi gian cho mt ln chit ko di 24h l
hp l v cng thu c hiu sut chit cao nht.
4.2.4. Nghin cu xc nh s ln trch ly thch hp
Sau khi la chn c thi gian trch ly l 24h/ln chit, chng ti tip tc
tin hnh nghin cu xc nh c s ln trch ly thch hp
Kt qu nh gi hm lng alkaloid TS v DNJ c trong qu trnh chit
c ch ra trong bng 4.8

41

Bng 4.8. nh hng s ln trch ly n hm lng alkaloid TS v DNJ thu


c trong l du
Cng thc
Hiu sut thu hi
alkaloid(%)
Hm lng
DNJ(%)
CV(%)

CT1

CT2

CT3

CT4

62,26

80,47

80,76

81,06

0,014b

0,017a

0,018a

0,018a

3,707

3,707

3,707

3,707

T bng 4.8 cho chng ti thy nu ch chit sut 1 ln th cha th chit


c ti a lng alkaloid c trong l du, d cho ko di thm thi gian chit xut
gp i th hu nh cng khng lm tng ng k lng alkaloid ton phn thu c,
nguyn nhn l do kh nng ho tan ca cht chit trong dung mi ch c gii hn
nn vic ko di thi gian chit hn na cng khng lm tng hiu sut chit.
Do vy thu c hm lng akaloid TS ti a c trong l du th cn
thit phi lp li qu trnh chit mt s ln na. Kt qu cho thy khi chit xut
thm ln 2 th hm lng tng cao, iu ny khng nh vic chit xut ln 2 l
rt cn thit. Khi lp li qu trnh chit sut n ln th 3, 4 th hm lng
alkaloid TS thu c trong sn phm cng ch tng ln rt t, trong khi chit 3, 4 ln
s lm tng thm thi gian chit ln v mt thm mt lng dung mi na, thm vo
nng lng c thu dch c cng s hao tn ng k. T kt qu ny c th thy
rng vi ngha kinh t th vic dng qu trnh chit xut sau ln chit th 2 l hp l
nht, hiu sut chit cng t n mc gn nh ti a m li khng gy nn lng
ph v dung mi v nng lng.
Nh vy, chng ti chn s ln chit thch hp l 2 ln, mi ln trong 24
gi vi lng dung mi ln u l theo t l dung mi/ nguyn liu l 10:1, ln
sau do khi nguyn liu ngm dung mi nn ch dng lng dung mi bng
60% ln 1.

42

T cc kt qu kho st trn chng ti chn cc iu kin chit xut


alkaloid t l du nh sau:
- Phng php trch ly: Ngm kit
- Dung mi: Cn 30%V c 1% axit axetic
- Nhit chit: Nhit phng
- S ln chit: Hai ln, mi ln trong 24 gi
- T l dung mi/ nguyn liu = 10:1 ln chit 1, ln 2 bng 60% ln 1
4.2.5 Kho st mt s thng s k thut nh hng n qu trnh sy phun
bt chit l du tm
Sau qu trnh trch ly, dch chit c lng trong khong 16 gi sau
c tch cc cn b ln khng ha tan, ri c a qua my lc trn khng
lc cc cn b nh v cc cht l lng. Sau lc dch chit c a c c
my c dc trn khng nhit 600C. Trong qu trnh c c nng cn
gim dn do cc tp cht t phn cc nh chlorphyl, sp, cht bo... tan tt
trong cn nhng khng tan trong nc s c tch ra, v vy sau c c cn
tin hnh lc loi b.
Qu trnh c c s dng li khi thu c dch chit theo t l nguyn
liu/ dch chit l 1:1, tc l 10kg nguyn liu ban u sau qu trnh chit v c
c s thu c khong 10 lt dch chit v dch chit c nng l 19.6oBx. T
dch chit ny chng ti bt u kho st cc thng s k thut nh hng n
qu trnh sy phun bt chit l du tm.
4.2.5.1. Nghin cu xc nh cht mang v nng cht mang thch hp
Sn phm bt sy phun khng ch c hm lng DNJ cao m cn c gi
tr cm quan tt ( mu sc, mn, ti, ha tan tt trong nc) do n c dng
ch bin tr. Khi tin hnh sy phun th dch chit bt l du 125oC, lu
lng dng nhp liu l 432ml/ph khng b sung thm cht mang th sn phm
to ra dng keo nu, qunh c, khng to thnh bt, v vy chng ti nghin
cu b xung thm cht mang. V bt c s dng lm thc phm cho ngi b
tiu ng nn cht mang b sung khng c hi vi sc khe. Qua qu trnh
43

tm hiu v cc loi cht mang thng c hay s dng trong cng ngh sy
phun bt sa, bt tri cy, bt dinh dng, chng ti quyt nh tin hnh trn
ba loi cht mang: isomalt, maltodextrin, tinh bt bin tnh vi nng kho st
ln lt l 5, 6, 7%.

Hnh 4.2. th biu din nh hng ca cht mang v nng cht mang
ti hm lng DNJ c trong bt sy phun
Sau khi sy, chng ti nhn thy khi s dng isomalt v tinh bt bin tnh
sn phm thu c trng thi keo, mu nu cnh gin, hiu sut thu hi bt
thp, hm lng DNJ thp. Cn sn phm thu c khi s dng maltodextrin c
mu vng ti, sn phm thu c trng thi mn, ti, c hiu sut thu hi bt
v hm lng DNJ cao. Tuy nhin trong ba nng maltodextrin s dng th
nng 6% cho sn phm bt c mu vng ti, mi thm d chu, hiu sut
thu hi bt cao hn khi s dng nng 7%. Do , chng ti quyt nh la
chn cht mang maltodextrin nng 6% b sung vo dch chit ri tin
hnh sy phun.

44

4.3.2 Nghin cu xc nh nhit sy phun thch hp


Dch chit sau khi c c c nng l 19.6oBx, b sung lng
maltodextrin l 6%. Hm lng cht kh ca hn hp nguyn liu i vo thit b
sy phun l 25%.Trong th nghim ny, chng ti ch kho st nhit dng kh
vo, v nhit dng kh ra ph thuc nhiu yu t. Tin hnh th nghim vi
o

cc nhit dng kh vo ln lt l Tv = 115; 125; 135; 145 v 155 C. Cc


thng s cn li ca thit b sy l p sut kh nn P = 8 bar; lu lng dng

Hiu sut thu hi DNJ(%)

nhp liu l 432 mL/h. Kt qu th nghim c biu din trn cc hnh 4 v 5


90
80
70
60
50
40
30
20
10
0
105

115

125

135

145

155

165

Nhit (oC)

Hnh 4.3. th biu din nh hng ca nhit khng kh u vo n


hiu sut thu hi DNJ ca qu trnh sy phun

m sn phm(W%)

5,80
5,50
5,20
4,90
4,60
4,30
4,00
3,70
3,40
105

115

125

135

145

155

165

Nhit (oC)

Hnh 4.4. th biu din nh hng ca nhit khng kh u vo n


m sn phm
45

Nhit qu thp hay qu cao u bt li cho qu trnh sy dch chanh dy.


Nhit khng kh sy thp th m cc ht vt liu sy vn cn kh cao, nn
bm nhiu ln thnh bung sy, lm gim hiu sut thu hi sn phm sau sy.
Nhit khng kh sy cao mc d t m kh tt nhng s c mt t vt liu
sy b chy, bm ln thnh, sn phm sau sy gim mi thm, v mu vng ti
b chuyn sang vng sm. Qua th nghim ny chng ti chn nhit khng
o

kh u vo l Tv = 135 C, ng vi hiu sut thu hi sn phm ca qu trnh sy


phun l 80,8% v m sn phm l 6,46%.
4.3.3 Xc nh lu lng nhp liu thch hp cho sy phun bt chit l du tm
Lu lng dng nhp liu c lin quan n tc bm nhp liu, nng
sut thit b v c nhit khng kh u ra, Tr. H thng bm nhp liu l bm
nhu ng, lu lng dng nhp liu l 360;396; 432;468 v 498 mL/pht. Cc
o

thng s th nghim gi khng i l P = 8 bar; Tv=135 C (c xc nh t th

Hiu sut thu hi DNJ(%)

nghim trn). Kt qu th nghim c biu din trn cc hnh 6 v hnh 7


85
80
75
70
65
60
55
50
324

360

396

432

468

504

540

Lu lng nhp liu

Hnh 4.5. th biu din nh hng ca lu lng nhp liu n hiu


sut thu hi DNJ

46

m sn phm (%)

5,7
5,2
4,7
4,2
3,7
3,2
2,7
2,2
324

360

396

432

468

504

540

Lu lng nhp liu (ml/h)

Hnh 4.6. th biu din nh hng ca lu lng nhp liu n m


sn phm
Tc bm nhp liu tng, ng ngha vi thi gian lu ca vt liu sy
trong bung sy gim, do , hiu qu sy s khng cao. m s tng, phn
ht m dnh li trong bung sy cng tng dn n hiu sut thu hi sn phm
sau qu trnh sy phun gim. Mc d lu lng dng nhp liu l 324,l/h, kt
qu thu c c cao hn mt t, nhng do iu kin ny, thit b lm vic km
n nh, thi gian sy di, nn cui cng chng ti chn lu lng dng nhp
liu l 360ml/h. Hiu sut thu hi sn phm ca qu trnh sy phun t 56.5%,
hiu sut thu hi DNJ t 80.8% v m sn phm l 3.17%.

47

4.3. Nghin cu phi ch tr


4.3.1. Nghin cu phi ch gia bt l du kh v bt chit l du
Bng 4.9. Kt qu cm quan khi phi ch bt l du kh v bt chit l du
im cm quan trung
CT

Nhn xt cm quan

bnh

CT1

Mu nht, v cht, mi chua

4.2

CT2

Mu nht, v cht, mi chua

4.3

CT3

Mu nht, hi cht

5.5

CT4

Mu nht, hi cht

7.3

CT5

Mu vng, cht nh, nc thanh

7.5

CT6

Mu m, hi snh

5.2

CT7

Mu nu m, hi snh

CT8

Mu nu m, hi snh

4.5

CT9

Mu nu m, hi snh

4.5

CT10

Mu nu m, hi snh

4.2

to ra sn phm tr ti lc cho ngi bnh tiu ng t l bt l du


kh v bt chit l du (m bo hm lng DNJ ti thiu l 10mg/ti 3g),
chng ti tin hnh nghin cu t l phi ch gia bt l du kh v bt chit
l du. Kt qu thu c bng 4.9
Kt qu trnh by bng 4.9 cho thy sn phm c t l bt chit 10%
(CT5) c im cm quan cao nht, trung bnh t 7,5. Trng thi, hng thm
v mu sc ca sn phm c t l bt chit 10% c nh gi v cho im cao
nht so vi nhng sn phm cn li do dch chit thu c c mu sc p,
hng thm du, v ng va phi. Phi ch sn phm vi t l bt chit 10%
cng p ng c yu cu ca sn phm l c hm lng DNJ t ti thiu l
10 mg/ti 3g. Chng ti quyt nh t l phi bt chit 10% tin hnh cc th
nghim tip theo.

48

4.3.2. Nghin cu phi ch tr v ng Isomalt


Bng 4.10. Kt qu cm quan khi phi ch tr v ng Isomalt
CT

Nhn xt cm quan

im cm quan trung
bnh

CT1

Cht nh, v nht

5.5

CT2

Cht nh, t ngt

5.7

CT3

Cht nh, t ngt

6.7

CT4

Cht nh, t ngt

7.3

CT5

Cht nh, t ngt

7.5

CT6

Cht nh, ngt du

8.2

CT7

Cht nh, ngt du

8.0

CT8

Cht nh, ngt

6.5

CT9

Ngt m

6.2

CT10

Ngt m

CT11

Ngt qu

5.5

CT12

Ngt qu

5.5

CT13

Ngt qu

5.5

Nhm mc ch tng thm hng v cho sn phm chng ti tin hnh


nghin cu t l phi ch ng cho sn phm. Do mc tiu ca ti l to ra
sn phm tr ti lc cho ngi mc bnh tiu ng nn chng ti chn ng
Isomalt to v ngt cho sn phm. ng Isomal l sn phm t nhin c
ngun gc t tinh bt c ngt thp ( ngt bng 6/10) v c hm lng
calori thp 240Kcal/100g so vi ng ma thng thng 370Kcal/100g, ng
Isomalt c cu trc phn t di hn v ng ny khng c c th chng ta
hp thu ngay trong d dy nh ng ma, ng Isomalt c hp thu rt
chm khi thc n xung ti rut non nn khng lm gia tng hm lng ng
huyt trong mu ca ngi bnh, do vy s khng lm tng ch s ng huyt
khi n. Kt qu thu c bng 4.10
Kt qu trnh by bng 4.10 cho thy sau khi phi ch ng Isomalt
vi cc t l khc nhau th v ca sn phm c s khc nhau r rt. hm cc
cng thc 1 3 tr vn cn v cht, cng thc 9 13 tr mt hn v cht

49

chuyn thnh v ngt. Khi phi ch 6.5% ng Isomalt (CT6), v 7.0 % ng


Isomalt (CT7), sn phm c nh gi c hng v hi ho v c im cm
quan cao nht. Tuy nhin gim gi thnh sn phm th chng ti chn cng
thc CT6 ( hm lng ng Isomalt/ sn phm l 6.5%).
[

4.3.4. Quy trnh ch bin tr t l du tm


L du ti

Phi ho, nghin


Bt l
du
Dung mi

Thu hi dung mi

Chit 2 ln

Lc

Tp cht

C c
Lc

Maltodextrin

Sy phun
Bt l du

Phi ch

Tr

50

Tp cht

Thuyt minh quy trnh


Chn ging du qu Thi Bnh thu hi cc l bnh t, sau thu hi l du
c loi b tp cht cc l h hng ri em phi nng ti m 10 12%
bo qun. Sau l du c nghin nh ti kch thc 1mm.
L du sau nghin nh c em chit bng phng php ngm trong
dung mi. Dung mi s dng l cn 30% c axit ho bng axit acetic nng
1%. Qu trnh chit lp li 2 ln nhit phng, mi ln trong 24 gi t l
dung mi l 10/1, ln 2 s dng lng dung mi bng 60% ln mt.
Sau mi ln lc dch chit c lc cc cht b, cc tp cht khng ho
tan ri c a v bnh c c chn khng nhit 600C, trong qu trnh c
c dung mi c thu hi ti s dng. Qu trnh c c din ra cho ti khi t
1 kg nguyn liu thu c 1 lt dch chit, nng cht kh xp x 20oBx, sau
tin hnh lc ln 2 loi cc cn khng tan trong. Ri b sung 6%
maltodextrin (so vi tng th tch dch chit) v tin hnh sy phun thu bt chit
l du c hm lng DNJ cao.
Sau sy phun bt chit c em phi ch vi bt l du kh v ng
isomalt to tr thnh phm

51

Phn 5. KT LUN V KIN NGH


5.1. Kt lun
T cc kt qu nghin cu chng rt ra mt s kt lun sau
1) Ging du qu trng Thi Bnh c hm lng DNJ cao, l bnh t thch
hp cho ch bin tr.
2) Phng php lm kh thch hp l phi nng ti m 10 12%, y l
phng php n gin t tn km.
3) La chon c phng php ngm trong dung mi l phng php trch ly
thch hp nht vi cc thng s c th
- Dung mi: cn 30%V c axit ha 1% bng axit axetic
- Nhit chit tch: Nhit phng
- T l dung mi/ bt l du: 10/1 ln chit 1, ln 2 bng 60% ln 1
- Thi gian cho mi ln chit: 24h
S ln chit: Hai ln, mi ln trong 24 gi
4) Phng php sy phun thu hi bt
- Cht mang: Maltodextrin 6 %
- Nhit sy: 135 0C
- Lu lng dng nhp liu: 360 ml/h
5) T l phi ch gia bt chit l du v bt l du kh l 10/9
T l phi ch ng isomalt vo tr l 6,5%
5.2 Kin ngh
Do ti tin hnh quy m phng th nghim nn cn nghin nghin
cu thm p dng trong sn xut.

52

TI LIU THAM KHO


Ti liu Ting Vit
1. B Y t (2002). Dc in Vit Nam III, H Ni, du (l).
2. Nguyn Huy Cng (2005). Bnh i tho ng, nhng quan im hin
i, NXB Y hc.
3. Nguyn Quang Trung (2006). nh gi tc dng bt chit l du trn
cc ch s lipid v trng thi chng oxy ho trong mu chut nht trng gy
ri lon lipid mu v i tho ng thc nghim. Bo co khoa hc.
4. Phm Ngc Thin, L Ngc Lin (2005). Chit xut, xc nh hm lng
polyphenol v nh gi tc dng chng Oxy ho ca cc mu bt chit l du.
Tp ch Nghin cu Y hc. S 38-5. 34-38
5. Trung tm nghin cu Du tm t (2006), Nghin cu lai to v cng
ngh nhn ging du lai F1 trng bng ht. Bo co tng kt ti 2006.
6. Vin cng nghip thc phm (2007). Nghin cu cng ngh sn xut bt
l du tm giu 1-Deoxynojirimycin. Bo co tng kt ti.
Ti liu Ting Anh
7. Bondada Andalulua, N.Ch. (2003). Antioxidant role of mulberry leaves
in streptozotocin-diabetic rats. Elsevier, Clinica Chimica Acta.
8. Bai, Gang, Wang, Dong-Li, Cao, Xue-Lin, Xiao, Hui-Jiao, geng Peng,
Liu Qian and Yang Wen-Bo (2004). Screening -glucosidase inhibitors in
traditional Chinese medicines. Acta Scientiarum Naturalium Universitatis
Nankaiensis (Natural Science Edition) 37(3). 98-102
9. C.S. Cockram, T.Van Binh, G.Gaela (2007). Diabetes prevention and
control in VietNam: demonstration project in two provinces. Global Report
10. International Diabetes Institute (2007). Annual Report.
11. Jin-Won Kim, Soo-Un Kim, Heui San Lee, Iksook Kim, Mi Young
Ahn and Kang Sun Ryu (2003). Determination of 1-deoxynojirimycin in Morus

53

alba L. leaves by derivatization with 9-fluorenulmethyl chloroformate followed


by reversed-phase high-performance liquid chromatography. Journal of
Chromatography A. 1002(2003). 93-99.
12. Fukuhara, Masatsune Kainosho and Sawao Murao, Kenichi (1986).
Isolation and Characterization of Amylase Inhibitors, Deoxynojirimycin. Agric.
Biol. Chem.
13. Kimura, T., Nagakawa, K., KubotaH., Kojima, Y. Goto, Y. (2007).
Food grade mulberry powder enriched with 1-Deoxynojirimycin suppresses the
elevation of postprandial blood glucose in humans. Journal of Agricultural and
Food chemistry.
14. Lin-Ling Wang and Ze-Yang Zhou (2008). Effect of extracts of
mulberry leaves processed differently on the activity of anpha-glucosidase.
Journal of Food, Agriculture & Environment Vol.6 (3&4) : 86-89
15. Liu Xueming, Xiao Gengsheng, Chen Weidong, Xu Yujuan and Wu
Jijun (2004) Quantification and Purifications of mulberry anthocyanins with
macrosporus resins. Journal Bio Medicine and Biotechnol. Vol 5:p326-331.
16. Nitra Nuengchamnon, Kornkanok Ingkaninan, Wiroje Kaewruang,
Sathaporn Wongareonwanakij, Bhinai Hongthongdaeng (2007). Quantitative
determination

of

1-deoxynorimycin

in

mulberry

leaves

using

liqid

chromatography-tandem mass spectromentry. Journal of Pharmaceutical and


Biomedical Analysis ELSEVIER 44 (2007). 853-858
17. Sun, Xing Yan and Lu, Zhao Lin 199 Shen Nong s Herbal Classic
18. Tsuneyuki Okua1, mai Yamada, Mariko Nakamura, Naoki Sadamori
and Sadako Nakamura (2006), Inhibitory effects of extractives from leaves of
Morus alba on human and rat small intestinal disaccharidase activity. British
Journal of Nutrition (2006), 95:933-938 Cambridge University Press.

54

LI CAM OAN

Ti xin cam oan rng, cc s liu v kt qu nghin cu trong lun vn


ny l trung thc v cha h c s dng.
Ti xin cam oan rng, mi s gip trong vic hon thnh lun vn
ny c cm n v cc thng tin trch dn trong lun vn ny c ghi r
ngun gc.
H Ni, ngy ....thng....nm 2011

LI CM N

hon thnh lun vn ny, bn cnh s c gng n lc ca bn thn,


ti nhn c s ng vin v gip rt ln ca nhiu c nhn v tp
th.
Ti xin by t lng bit n su sc ti TS. Hong Th L Hng, trng
B mn Bo qun ch bin Vin nghin cu rau qu Tru Qu - Gia Lm
H Ni tn tnh gip , to mi iu kin tt nht cho ti thc hin v
hon thnh lun vn tt nghip ny.
Ti xin chn thnh cm n ti s gip ca cc anh, ch B mn bo
qun ch bin - Vin Nghin cu rau qu gip ti trong sut thi gian
thc hin ti
Ti xin cm n gia nh v tt c bn b ng vin gip , to iu
kin thun li cho ti trong sut qu trnh thc hin ti ha hon thnh
lun vn ny.
H Ni, ngy .... thng.....nm 2011
Hc vin

ii

MC LC
Phn 1. M U ................................................................................................ 1
1.1. t vn ....................................................................................................... 1
1.2. Mc ch yu cu ........................................................................................... 2
1.2.1. Mc ch ...................................................................................................... 2
1.2.2. Yu cu ........................................................................................................ 2
Phn 2. TNG QUAN TI LIU ..................................................................... 3
2.1. Tng quan v cy du tm ............................................................................. 3
2.1.1. Ngun gc, phn loi v c im hnh thi ca cy du ........................... 3
2.1.1.1. Ngun gc, phn loi ............................................................................... 3
2.1.1.2. Mt s ging du chnh c trng Vit Nam ..................................... 4
2.1.2. Tnh hnh trng trt v s dng l du mt s tnh ca Vit Nam hin nay .. 5
2.1.3. c im, thnh phn ho hc ca l du ................................................... 6
2.1.3.1. Flavon v flavon glycozit ......................................................................... 7
2.1.3.2. Steroit ....................................................................................................... 7
2.1.3.3. Cc cht bay hi ....................................................................................... 7
2.1.3.4. Saccarit v cc axit amin ......................................................................... 7
2.1.3.6. Cc cht c hot tnh sinh hc ................................................................. 7
2.1.4. Alkaloid trong l du tm............................................................................ 8
2.1.4.1. Khi nim ................................................................................................ 8
2.1.4.2. Tnh cht ca alkaloid ............................................................................. 8
2.1.4.3. Cc alkaloid c trong l du tm ........................................................... 10
2.1.5. Hp cht DNJ trong l du tm................................................................. 11
2.1.5.1. Bn cht v cu trc ho hc.................................................................. 11
2.1.5.2. Tc dng v c ch lm gim ng huyt ca DNJ ............................ 12
2.1.6. Mt s cng dng ca l du..................................................................... 13
2.2. Cc phng php tch chit cc hp cht alkakoid trong l du ................. 14
2.2.1. Phng php v iu kin chit xut l du ............................................. 14

iii

2.2.2. Chn dung mi chit xut l du .............................................................. 16


2.3. Tnh hnh sn xut v tiu th cc loi thc phm chc nng cha bnh tiu
ng trn th gii v Vit Nam hin nay .......................................................... 18
2.3.1. Tnh hnh sn xut v tiu th cc loi thc phm chc nng cha bnh
tiu ng trn th gii ....................................................................................... 18
2.3.2. Tnh hnh sn xut v tiu th cc loi thc phm chc nng cha bnh
tiu ng Vit Nam ........................................................................................ 18
2.3.2.1. Diabetna (Cng ty dc phm ch Nhn) .............................................. 19
2.3.2.2. Nadia (Cng ty c phn dc phm Hong Giang)............................... 19
2.3.2.3. Metabosol ............................................................................................... 19
2.3.2.4. H tng ng ........................................................................................ 19
2.3.2.5. Tiu ng nam dc (Cng ty c phn Nam Dc) ........................... 19
2.3.2.6. Ayubes (Cng ty Ph Hi) ..................................................................... 19
2.4. Tnh hnh nghin cu lm sng v tc dng ca cht chit l du i vi s
gim ng huyt ................................................................................................ 20
2.4.1. Tnh hnh nghin cu ngoi nc ............................................................. 20
2.4.2. Tnh hnh nghin cu trong nc .............................................................. 22
Phn 3. I TNG - NI DUNG PHNG PHP NGHIN CU .... 23
3.1. i tng v nguyn vt liu ....................................................................... 23
3.1.1. i tng nghin cu................................................................................ 23
3.1.2. Ho cht..................................................................................................... 23
3.1.3. Dng c v thit b .................................................................................... 23
3.2. Ni dung ....................................................................................................... 23
3.3. Phng php nghin cu .............................................................................. 24
3.3.1.Phng php chung .................................................................................... 24
3.3.2.Phng php thit k th nghim v x l s liu...................................... 25
3.3.3. Phng php phn tch cc ch tiu ha l ............................................... 25
3.3.4. Phng php nh gi cm quan .............................................................. 25
3.3.5. Phng php c th ................................................................................... 25

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Phn 4. KT QU NGHIN CU V THO LUN ................................. 31


4.1. Nghin cu ging v gi l du thch hp .............................................. 31
4.1.1. nh hng ca gi thu hi n hm lng alkaloid TS ...................... 31
4.1.2. Nghin cu nh hng ca trng thi nguyn liu n s thay i hm
lng DNJ ........................................................................................................... 32
4.1.3. Xc nh phng php lm kh nguyn liu thch hp ............................ 33
4.2. Nghin cu quy trnh cng ngh sn xut bt l du tm giu DNJ ........... 35
4.2.1. Nghin cu phng php trch ly thch hp ............................................. 35
4.2.2. Nghin cu la chn loi v nng dung mi trch ly thch hp .......... 36
4.2.3. Nghin cu xc nh nhit trch ly, t l dung mi/nguyn liu v thi
gian trch ly thch hp ......................................................................................... 38
4.2.3.1 Nghin cu xc nh nhit trch ly thch hp..................................... 38
4.2.3.2. Nghin cu xc nh t l dung mi/ bt l du thch hp .................... 39
4.2.3.3. Nghin cu xc nh thi gian trch ly thch hp .................................. 40
4.2.4. Nghin cu xc nh s ln trch ly thch hp .......................................... 41
4.2.5 Kho st mt s thng s k thut nh hng n qu trnh sy phun bt
chit l du tm ................................................................................................... 43
4.2.5.1. Nghin cu xc nh cht mang v nng cht mang thch hp ........ 43
4.3.2 Nghin cu xc nh nhit sy phun thch hp ..................................... 45
4.3.3 Xc nh lu lng nhp liu thch hp cho sy phun bt chit l du tm .... 46
4.3. Nghin cu phi ch tr ............................................................................... 48
4.3.1. Nghin cu phi ch gia bt l du kh v bt chit l du ................... 48
4.3.2. Nghin cu phi ch tr v ng Isomalt ............................................... 49
4.3.4. Quy trnh ch bin tr t l du tm.......................................................... 50
Phn 5. KT LUN V KIN NGH ............................................................ 52
5.1. Kt lun ........................................................................................................ 52
5.2 Kin ngh ....................................................................................................... 52
TI LIU THAM KHO ................................................................................ 53

DANH MC BNG
Bng 2.1. Din tch du tm chia theo vng sinh thi .......................................... 6
Bng 2. 2. Thnh phn ha hc chnh ca l du (% cht kh) ............................ 8
Bng 2.3. Thnh phn cc cht alkaloid c trong l du tm ............................. 10
Bng 2.4. Thnh phn dc tnh ca l du ........................................................ 14
Bng 4.1. nh hng ca gi thu hi n hm lng alkaloid TS trong l du Qu ...... 32
Bng 4.2. S bin i hm lng alkaloid ca l du ti v l du kh trong 10
ngy theo di ....................................................................................................... 32
Bng 4.3. nh hng ca cc phng php trch ly n hm lng alkaloid c
trong l du .......................................................................................................... 35
Bng 4.4. nh hng ca loi v nng dung mi n hm lng alkaloid TS
v DNJ thu c trong l du ............................................................................. 37
Bng 4.5. nh hng ca nhit chit xut n hm lng alkaloid TS v DNJ
thu c trong l du........................................................................................... 39
Bng 4.6. nh hng ca t l dung mi n hm lng alkaloid TS v DNJ thu
c t l du ...................................................................................................... 40
Bng 4.7. nh hng thi gian chit n hm lng alkaloid TS v DNJ thu
c trong l du ................................................................................................. 41
Bng 4.8. nh hng s ln trch ly n hm lng alkaloid TS v DNJ thu
c trong l du ................................................................................................. 42
Bng 4.9. Kt qu cm quan khi phi ch bt l du kh v bt chit l du .... 48
Bng 4.10. Kt qu cm quan khi phi ch tr v ng Isomalt ...................... 49

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DANH MC HNH
Hnh2.1. Cy du tm ............................................................................................ 3
Hnh 2.2. Cu trc ha hc ca hp cht DNJ .................................................... 11
Hnh 2.3. Mt s sn phm cho ngi bnh tiu ng ..................................... 20
Hnh 4.1. thi s bin i hm lng alkaloid TS qua 1 thng theo di ca l
du kh ................................................................................................................ 34
Hnh 4.2. th biu din nh hng ca cht mang v nng cht mang ti
hm lng DNJ c trong bt sy phun ............................................................... 44
Hnh 4.3. th biu din nh hng ca nhit khng kh u vo n hiu
sut thu hi DNJ ca qu trnh sy phun ............................................................ 45
Hnh 4.4. th biu din nh hng ca nhit khng kh u vo n m
sn phm .............................................................................................................. 45
Hnh 4.5. th biu din nh hng ca lu lng nhp liu n hiu sut thu
hi DNJ................................................................................................................ 46
Hnh 4.6. th biu din nh hng ca lu lng nhp liu n m sn
phm .................................................................................................................... 47

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