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QCVN 4-18:2011/BYT
H NI - 2011
Li ni u
QCVN 4-18:2011/BYT do Ban son tho quy chun k thut quc gia v Ph gia thc phm v cht h
tr ch bin bin son, Cc An ton v sinh thc phm trnh duyt v c ban hnh theo Thng t s
01/2011/TT-BYT ngy 13 thng 01 nm 2011 ca B trng B Y t.
PH LC
YU CU K THUT V PHNG PHP TH I VI CH PHM TINH BT
1. Tn khc, ch s
M s C.A.S.
Tinh bt acetat :
9045-28-7
68130-14-3
Tinh bt hydroxypropyl:
9049-76-7
53124-00-8
68187-08-6
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Cu trc hin vi
Nhum mu iod
Kh ng
Ch
- Xem ct 3 bng 1
- Xem m t trong phn Phng php th
6. Phng php th
6.1. nh tnh
Soi knh hin vi
Nhum mu iod
Kh ng
Phm vi p dng:
Phng php ny c p dng, vi mt vi thay i nh, i vi mu
cht lng hoc rn thm ch c s c mt ca cc hp cht cha lu
hunh d bay hi khc.
Nguyn tc:
SO2 c gii phng ra t mu trong mi trng acid un si v tch kh
SO2 ra bng dng kh CO2. Kh tch ra c dn vo dung dch
hydrogen peroxid long ni n b oxy ha thnh H 2SO4 v c chun
bng dung dch kim tiu chun. Mt cch khc, H2SO4 c th c
nh lng bng BaSO4.
Dng c:
B dng c Monier-Williams nh lng acid sulfur, c cu to
bng cc kt ni thu tinh thon tiu chun, c th mua c cc ca
hng bn dng c thu tinh phc v nghin cu khoa hc ng tin cy.
Tuy nhin, dng c ny thng c t lp t cc dng c thu tinh th
nghim tiu chun c cc kt ni c np (xem Hnh 1).
Hnh 1
B dng c gm bnh un hai c trn dung tch 1.000 ml ni vi mt ng
kh vo, mt phu nh git dung tch 60 ml c van kho kch thc l 2
mm, sinh hn ngc nghing Allihn. Mt ng dn ni vi phn trn cng
ca sinh hn ti y ca bnh nhn hnh nn dung tch 250 ml, bnh ny
dc ni ng Peligot.
Trong qu trnh vn hnh, lng kh CO2 thot ra c dn qua bnh by
v to thnh bt khi cho qua hn hp phn ng nng, dn SO 2 qua bnh
ngng v vo cc bnh nhn, ni n c ht nh lng.
Chun b dung dch:
Tm lc phng
php
Yu cu k thut i
vi sn phm cui
cng
X l nhit kh vi
acid HCl hoc acid
ortho-H3PO4
pH = 2,5 7,0
Tinh bt x l bng
acid
pH = 4,8 7,0
Tinh bt x l bng
kim
X l bng NaOH
hoc KOH
pH = 5,0 7,5
Tinh bt ty mu
X l bng acid
peracetic v hoc
hydrogen peroxid,
hoc natri hypochlorit,
Tinh bt x l bng
enzym
Tinh bt oxy ho
X l bng natri
hypochlorit
Cc nhm carboxyl
khng c qu
1,1%; D lng SO2
khng c qu 50
mg/kg
Monostarch phosphat
Hm lng phosphat
tnh theo phosphor
khng c qu 0,5%
i vi tinh bt khoai
ty hoc bt m, v
khng c qu 0,4%
i vi tinh bt khc.
Distarch phosphat
Hm lng phosphat
tnh theo phosphor
khng c qu 0,5%
i vi tinh bt khoai
ty hoc bt m, v
khng c qu 0,4%
i vi tinh bt khc.
Distarch phosphat
phosphat ho
Kt hp cc x l i
vi Monostarch
phosphat v Distarch
phosphat
Hm lng phosphat
tnh theo phosphor
khng c qu 0,5%
i vi tinh bt khoai
ty hoc bt m, v
khng c qu 0,4%
i vi tinh bt khc.
Distarch phosphat
acetylat
Cc nhm acetyl
khng c qu
2,5%; hm lng
phosphat tnh theo
phosphor khng c
qu 0,14% i vi tinh
bt khoai ty hoc bt
m, v khng c
qu 0,04% i vi tinh
bt khc; v vinyl
acetat khng c
qu 0,1 mg/kg
Tinh bt acetat
Ester ho bng
anhydrid acetic hoc
vinyl acetat
Cc nhm acetyl
khng c qu 2,5%
Distarch adipat
Ester ho bng
Cc nhm acetyl
Ch
acetylat
anhydrid acetic v
anhydrid adipic
khng c qu 2,5%
v cc nhm adipat
khng c qu
0,135%
Tinh bt hydroxypropyl
Ester ho bng
propylen oxyd
Cc nhm
hydroxypropyl khng
c qu 7,0%;
propylen chlorohydrin
khng c qu 1
mg/kg
Distarch phosphat
hydroxypropyl
Cc nhm
hydroxypropyl khng
c qu 7,0%;
propylen chlorohydrin
khng c qu 1
mg/kg v d lng
phosphat tnh theo
phosphor khng c
qu 0,14% i vi tinh
bt khoai ty hoc bt
m, v khng c
qu 0,04% i vi tinh
bt khc
Tinh bt natri
octenylsuccinat
Ester ho bng
anhydrid
octenylsuccinic
Cc nhm
octenylsuccinyl khng
c qu 3%; v d
lng acid
octenylsuccinic khng
c qu 0,3%
Tinh bt oxy ho
acetylat
X l bng natri
hypochlorit sau
ester ho bng
anhydrid acetic
Cc nhm acetyl
khng c qu 2,5%
v cc nhm carboxyl
khng c qu 1,3%
pH
- c m t trong Ct 3 ca Bng 1.
- Ha 20 g mu vi 80 ml nc. Khuy lin tc tc trung bnh trong 5
pht (Trong trng hp mu l tinh bt keo ha s b, cn 3 g ha vi
97 ml nc).
Nhm carboxyl
c m t trong Ct 3 ca Bng 1.
Nguyn tc:
Tinh bt c cha carboxyl c cn bng vi acid v c chuyn cc
mui carboxyl thnh dng acid. Cc cation v acid d c loi b bng
cch ra vi nc. Mu ra c ho tan trong nc v c chun
bng dung dch kim chun.
Ch : Cc nhm phosphat t nhin c mt trong tinh bt
khoai ty lm tng chun c tm thy trong phng
Ch v phng nga:
Lng mu khng nn vt qu 5,0 g i vi tinh bt oxy ho trung bnh
hoc nh hn 0,15 g i vi tinh bt thng mi oxy ho cao.
Thm 1 ml dung dch AgNO 3 1% pha trong nc vo 5 ml dch lc. Xut hin
kt ta hoc c trong vng 1 pht nu c mt ca clorid.
Khng nn gia nhit trn a nng hoc trn n t Bunsen. S qu nhit
hoc qu nng i vi lng mu nh s lm phn hy mu v kt qu
carboxyl cao gi to.
H ha mu trit to iu kin chun nhanh chng v pht hin im
kt thc chnh xc.
Chun mu trng c tin hnh trn mu c ra bng nc
hiu chnh cc thnh phn acid khng c a vo oxy ho hoc
chuyn ho. Cc acid bo t do kt hp vi amylose trong tinh bt ng
thng l nhng cht c ng gp chnh i vi chun mu trng.
c m t trong Ct 3 Bng 1
Thit b:
Thit b quang ph hp th nguyn t vi n cathod rng mangan
Chun b dung dch:
Dung dch chun: Chun b dung dch 0,5 mg mangan/lt.
Dung dch mu th: Chuyn 10 g mu vo bnh nh mc Kohlrausch dung
tch 200 ml trc c ra bng dung dch HCl 0,5N, thm 140 ml dung
dch HCl 0,5N v lc mnh trong 15 pht, thch hp nht dng my lc. Pha
ti th tch 200 ml bng dung dch HCl 0,5N v lc. Li tm khong 100 ml
hn hp trong ng ly tm c thnh dy hoc l tc 650 xg trong 5 pht
v ly dung dch lng trn b mt. Dung dch ny l dung dch mu th.
Cch tin hnh:
Thc hin theo hng dn ca nh sn xut cho vn hnh ca thit b
quang ph hp th nguyn t v ht nc ct thng qua n kh acetylen
trong 5 pht c mt ng nn ti bc sng 279,5 nm. Trong cng
mt cch, ht mt phn ca dung dch chun v lu kt qu. Cui cng,
ht dung dch mu v so snh kt qu vi kt qu ca dung dch chun,
v nhn gi tr ny vi 20 c c nng tnh bng mg mangan/kg mu
ban u c ly phn tch.
Phosphor
c m t trong Ct 3 ca Bng 1.
Ho cht, thuc th:
Dung dch amoni molybdat 5%: Ho 50 g amoni molybdat tetrahydrat,
(NH4)6Mo7O244H2O, trong 900 ml nc m, lm ngui ti nhit phng,
pha long ti 1000 ml bng nc v lc u.
Dung dch amoni Vanadat 0,25%: Ho 2,5 g amoni metavanadat, NH 4VO3,
trong 600 ml nc si, lm ngui ti 60 70 0C v thm vo 20 ml dung dch
acid nitric. Lm ngui ti nhit phng, pha long ti 1000 ml bng nc
v lc u.
Dung dch km acetat 10%: Ho 120 g km acetat dihydrat,
Zn(C2H3O2)2,H2O, trong 880 ml nc v lc qua giy lc Whatman s 2V
hoc giy lc tng ng trc khi s dng.
Dung dch acid nitric 29%: Thm 300 ml dung dch acid nitric (t trng 1,42)
vo 600 ml nc v lc u.
Dung dch phosphor chun (100 g P/ml): Ho 438,7 mg KH2PO4 trong
nc trong bnh nh mc 1000 ml, pha ti 1000 ml bng nc v lc u.
ng chun:
Dng pipet ht 5; 10 v 15 ml dung dch phosphor chun cho vo cc bnh
nh mc ring bit dung tch 100 ml. Thm vo mi bnh v bnh mu trng
th t ln lt theo th t 10 ml dung dch acid nitric, 10 ml dung dch
amoni Vanadat v 10 ml dung dch amoni molybdat, lc mnh sau mi khi
thm. Pha ti th tch 100 ml bng nc, lc u v yn trong 10 pht.
Trong :
W: Khi lng mu th (g)
Cc nhm acetyl
c m t trong Ct 3 ca Bng 1.
Cn chnh xc 5 g mu v cho vo bnh nn dung tch 250 ml. To hn dch
trong 50 ml nc, thm vo vi git phenolphthalein TS v chun bng
dung dch NaOH 0,1N n khi xut hin mu hng nht. Thm 25 ml dung
dch NaOH 0,45N, y np bnh v lc mnh trong 30 pht, thch hp nht l
lc bng my. (Ch : Nhit khng c qu 30 0C, nu khng mt vi
loi tinh bt c th b h ha). Tho np y, ra np v thnh bnh bng
mt vi ml nc v chun kim d bng dung dch HCl 0,2N cho n khi
mt mu hng. Ghi li th tch dung dch HCl 0,2N dng chun (S ml).
Thc hin chun mu trng trn 25 ml dung dch NaOH 0,45N v ghi li
th tch ca dung dch HCl 0,2N (B ml)
(B S) x N x 0,043 x 100
% cc nhm acetyl = ------------------------------------------W
Trong :
N: Nng ng lng ca dung dch HCl
W: Khi lng mu (g)
Vinyl acetat
Cc nhm adipat
c m t trong Ct 3 ca Bng 1.
Ho cht v dung dch:
N,N-Bis-trimethylsilyltrifluoroacetamid (BSTFA): ca Macherey-Nagel, D
5160 Dueren, c hoc tng ng.
Dung dch acid glutaric: Ho tan 1 g acid glutaric (ca Merck hoc tng
ng) trong nc v pha ti 1.000 ml.
Dung dch acid adipic: Ho tan 1 g acid adipic (UCB, Brussels, B hoc
tng ng) trong 900 ml nc m, lm ngui n nhit phng, pha
ti 1.000 ml v lc u.
Dng c, thit b:
Thit b sc k kh Hewlett-Packard Model 7620A hoc tng ng c
trang b detector ion ho ngn la v Thit b phn tch Model 3370A.
Cc thng s ct: lm bng thp khng r c chiu di 2 m, ng knh
trong 1,83 mm, c nhi bng OV-17 5% trn Chromosorb GAW-DMCS 80
- 100 mesh (Alltech Europe, Inc,. B 9731 Eke, B); luyn ct 350 0C trong
24 gi vi tc kh mang nitrogen 40 ml/pht. Cc tc dng kh hot
ng (ml/pht): kh mang nitrogen l 30, hydrogen l 40, khng kh l 400.
Nhit : bung bm mu 280 0C, detector 2500C, ct 1400C. Cc thi gian
lu (pht): acid glutaric l 2,83; acid adipic l 4,5.
Hiu chun:
Cn v cho vo 4 bnh bnh tam gic dung tch 250 ml (1 g tinh bt ng dng
sp/bnh). Thm vo mi bnh 50 ml nc v 1 ml dung dch nc cha 1
mg acid glutaric/ml. Thm vo bnh mt 0,25 ml dung dch nc cha 1 mg
acid adipic/ml, thm vo 3 bnh cn li ln lt 0,5; 0,75 v 1 ml. Mi bnh
sau cha 1 mg acid glutaric v ln lt l 0,25; 0,5; 0,75 v 1 mg acid
adipic. Lc mnh cc bnh bng tay phn tn hon ton tinh bt v thm
50 ml dung dch NaOH 4N. Tip tc lc mnh trong 5 pht, mi bnh trong
chu nc nhit mi trng v thm cn thn 20 ml dung dch HCl
12N cho mi bnh. Khi mi bnh ngui, chuyn ton lng hn hp trong
bnh vo phu chit dung tch 250 ml. Chit vi 100 ml ethyl acetat tinh
khit. Rt lp nc di vo mt cc vi ; tp trung lp dung mi hu c
pha trn vo mt bnh bnh tam gic dung tch 500 ml cha 20 g Na 2SO4
khan. Chuyn phn tan trong nc quay tr li phu chit v lp li chit
bng ethyl acetat hai ln na. Lc cc bnh nh k trong 10 pht v sau
lc qua giy lc Whatman s 1 vo trong cc bnh y trn dung tch 1 lt.
Ra cc bnh v cc cn khng ho tan c lc 2 ln bng 50 ml ethyl
acetat. C ton b phn chit hu c v nc ra ca mi bnh nhit
khng qu 400C, p sut chn khng (50 mgHg) cho n khi kh hon ton.
C ethyl acetat nn c thc hin cng nhanh cng tt bi v d xy ra cc
phn ng thu phn trong qu trnh thc hin. Cc sn phm thu phn lm
gim phn gii ca acid adipic trong phn tch sc k.
Thm ln lt 2 ml pyridin v 1 ml N,N-Bis-trimethylsilyltrifluoroacetamid vo
cc thnh phn kh. y np tng bnh y trn v ra b mt bn trong
tht k bng cch lc xoy. yn cc bnh trong 1 gi sau chuyn
khong 2 ml t mi bnh vo cc l thu tinh nh v y kn ngay lp tc.
Bm 4 l vo thit b sc k kh.
Tnh kt qu:
Xc nh cc thi gian lu i vi mi acid v xc nh chiu cao pic i vi
acid glutaric v i vi mi nng acid adipic. V th biu din quan h
tuyn tnh gia t l chiu cao pic ca acid adipic/chiu cao pic ca acid
Trong :
Hs v Hl: Cc chiu cao ln lt ca ca acid adipic chun v acid glutaric;
Ws: Khi lng acid adipic chun
RF nn c kim tra mi tun mt ln.
Adipat tng s:
Cn chnh xc 1 g mu cho vo bnh bnh tam gic dung tch 250 ml, thm
vo 50 ml nc v 1 ml dung dch tan trong nc c 1 mg acid glutaric/ml.
Tin hnh nh trong phn Hiu chun, bt u Lc cc bnh bng tay....
Acid adipic t do:
Cn chnh xc 5 g mu cho bnh bnh tam gic dung tch 250 ml, thm vo
100 ml nc v 1 ml dung dch acid glutaric. Lc mnh trong 1 gi, lc qua
dng c lc Milipore 0,45 m, thm 1 ml dung dch HCl m c vo phn
lc c v chuyn ton lng vo phu chit dung tch 250 ml. Tin hnh
nh trong phn Hiu chun, bt u Chit vi 100 ml....
Tnh kt qu:
i vi c hai php nh lng (Hm lng adipat tng v Hm lng
acid adipic t do) ghi chiu cao cc pic i vi acid adipic v acid glutaric
(ni chun). Tnh hm lng ln lt adipat tng s v acid adipic t do c
trong mu theo cng thc sau:
Trong :
A: Hm lng adipat tng s hoc acid adipic t do (%)
HX: Chiu cao pic ca acid adipic trong dung dch mu thc
HIX: Chiu cao pic ca acid glutaric trong dung dch mu thc
RF: H s p ng i vi acid adipic
S: Khi lng mu trong dung dch mu thc (g)
Cc nhm adipat (%) = Hm lng adipat tng s (%) hm lng acid
adipic t do (%)
Cc nhm hydroxypropyl
c m t trong Ct 3 ca Bng 1.
Thuc th Ninhydrin:
Dung dch 3% tinh th 1,2,3,-triketohydrinden trong dung dch natri bisulfit
5% trong nc.
Cch tin hnh:
Cn chnh xc 50 100 mg mu cho vo trong bnh nh mc dung tch 100
ml v thm 25 ml dung dch H2SO4 1N. Chun b mt mu tinh bt cha bin
tnh c cng ngun gc (tc l ng hoc khoai ty) trong cng cch thc
hin. t cc bnh trong cch thy si v gia nhit cho n khi cc mu to
thnh dung dch. Lm ngui v pha ti th tch 100 ml bng nc. Nu cn
thit pha long mu hn m bo khng c qu 4 mg nhm
hydroxypropyl/100 ml, sau pha mu trng tinh bt tng ng. Dng pipet
ly 1 ml cc dung dch cho vo cc ng th nh mc 25 ml c cc np thu
tinh c ngm trong nc lnh, thm tng git 8 ml dung dch H 2SO4 m
c vo mi ng. Lc u v t cc ng trong cch thy si chnh xc 3
pht. Chuyn ngay lp tc cc ng vo chu cho n khi dung dch lnh.
Thm 0,6 ml ninhydrin, cn thn cho thuc th chy xung theo thnh
ca cc ng th. Lc u ngay lp tc v t cc ng trong chu nc 25 0C
trong 100 pht. iu chnh th tch trong mi ng ti 25 ml bng acid H 2SO4
v lc ngc cc ng vi ln. (Khng c lc). Ngay lp tc chuyn cc
phn ca cc dung dch vo cc cng o 1 cm v sau chnh xc 5 pht o
hp th (A) bc sng 590 nm, s dng mu trng tinh bt nh l mu
i chng. Chun b ng chun bng cc phn 1 ml ca cc dung dch
chun tan trong nc c 10, 20, 30, 40 v 50 g propylen glycol/ml.
Tnh kt qu:
C x 0,7763 x 10 F
Cc nhm hydroxypropyl (%) =----------------------------W
Trong :
C: Hm lng propylen glycol trong dung dch mu tnh c da vo
ng chun (g/ml)
F: H s pha long (nu cn mt pha long hn)
W: Khi lng mu (mg)
Propylen clorhydrin
c m t trong Ct 3 ca Bng 1.
Thit b sc k kh:
S dng thit b Hewlett-Packard Model 5750 hoc tng ng. Mt thit
b ct kp c trang b detector ion ho ngn la. Mt thit b tch phn l
mt phn ca h thng ghi.
Ct sc k kh: S dng ct thp khng r, di 3 m, ng knh ngoi 3,2
mm, c nhi 10% Carbowax 20M trn 80/100 mesh Gas Chrom 2, hoc
tng ng. Sau khi nhi, trc khi s dng, luyn ct qua m trong iu
kin nhit 2000C, s dng dng kh heli vi tc 25 ml/pht.
Dng c c c: S dng dng c c c Kuderna-Danish c mt bnh dung
tch 500 ml, c sn ca Cng ty Kontes Glass,.. Vineland, N.J., M, (Catalog
s K-57000), hoc tng ng.
Cc bnh p lc: S dng cc bnh p lc dung tch 200 ml, c giong
Neoprene, np y thu tinh v gn vi mt ci kp kim loi, c sn ca
Cng ty Fisher Scientific, Pittsburgh, PA, M. (Vitro 400, catalog s 3 100).
Trong :
C: Nng (mg/kg) ca cc propylen chlorohydrin (tng ca cc ng phn)
trong mu i chng
a: Tng din tch tn hiu c to ra bi cc ng phn propylen
chlorohydrin trong mu th
A: Tng din tch tn hiu c to ra bi cc ng phn propylen
chlorohydrin trong i chng
ester ha ca natri
octenyl succinat
tinh bt
Nguyn tc:
ester ha c xc nh bi lng kim tiu th sau khi acid ho v ra
k monoester ca acid octenylsuccinic vi tinh bt.
Cch tin hnh:
Cn v cho 5 g mu vo cc dung tch 150 ml. Lm m bng mt vi ml
isopropyl alcol tinh khit. Dng pipet thm vo 25 ml dung dch HCl 2,5N
trong isopropanol, dng acid ra mu bm trn thnh cc. Khuy trong
30 pht bng my khuy t. Thm vo 100 ml isopropanol 90% t ng ong
chia . Khuy trong 10 pht. Lc mu qua phu Buchner v ra bnh lc
bng isopropanol 90% cho n khi dch lc thu c khng cn ion clorid.
S dng AgNO3 0,1N kim tra cc ion clorid. Chuyn bnh lc vo cc
dung tch 600 ml v ra nh phu Buchner ra tinh bt trong cc. Thm
nc ct vo cho n th tch 300 ml. t trong cch thy si c khuy
trong 10 pht. Chun trong khi cn nng bng dung dch NaOH 0,1N cho
n im kt thc c pht hin bng phenolphthalein.
Kt qu:
0,162 x A
ester ha (DS) = ------------------------1 0,210 x A
Trong :
A: s mili ng lng ca NaOH s dng/g octenyl succinat tinh bt