CNG HA X HI CH NGHA VIT NAM

QCVN 4-8 : 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT NGT TNG HP
National technical regulation
on Food additives Artificial sweeteners

H NI - 2010

Li ni u
QCVN 4-8:2010/BYT do Ban son tho quy chun k thut
quc gia v Ph gia thc phm v cc cht h tr ch bin
bin son, Cc An ton v sinh thc phm trnh duyt v
c ban hnh theo Thng t s 25/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT NGT TNG HP
National technical regulation on Food additives Sweeteners

1. QUY NH CHUNG
1. Phm vi iu chnh
Quy chun k thut quc gia (sau y gi tt l Quy chun) ny quy nh cc yu cu
k thut v qun l v cht lng, v sinh an ton i vi cc cht ngt tng hp c s
dng vi mc ch lm ph gia thc phm.
2. i tng p dng
Quy chun ny p dng i vi:
2.1. T chc, c nhn nhp khu, xut khu, sn xut, bun bn v s dng cc
cht ngt tng hp lm ph gia thc phm (sau y gi tt l t chc, c nhn).
2.2. C quan qun l nh nc c lin quan.
3. Gii thch t ng v ch vit tt:
3.1. Cht ngt tng hp: l ph gia thc phm khng phi l ng c ngun
gc t nhin c s dng vi mc ch to v ngt cho thc phm.
3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food addiditive specifications; Joint FAO/WHO expert committee on
food additives; Volume 4 - Analytical methods, test procedures and laboratory
solutions used by and referenced in the food additive specifications; FAO, 2006): Cc
yu cu k thut i vi ph gia thc phm, Tp 4 Cc phng php phn tch, quy
trnh th nghim, dung dch th nghim c s dng (hoc tham chiu) trong yu
cu k thut i vi ph gia thc phm; JECFA bin son; FAO ban hnh nm 2006.
3.3. M s C.A.S (Chemical Abstracts Service): M s ng k ha cht ca
Hip hi Ha cht Hoa K.
3.4. TS (test solution): Dung dch thuc th.
3.5. ADI (Acceptable daily intake): Lng n vo hng ngy chp nhn c.
3.6. INS (International numbering system): H thng m s quc t v ph gia
thc phm.

II. YU CU K THUT, PHNG PHP TH V LY MU

1. Yu cu k thut v phng php th i vi cc cht ngt tng hp c
quy nh ti cc ph lc ban hnh km theo ca Quy chun ny nh sau:
1.1. Ph lc 1: Yu cu k thut v phng php th i vi Mannitol.
1.2. Ph lc 2: Yu cu k thut v phng php th i vi Acesulfam kali.
1.3. Ph lc 3: Yu cu k thut v phng php th i vi Isomalt.
1.4. Ph lc 4: Yu cu k thut v phng php th i vi Saccarin.
1.5. Ph lc 5: Yu cu k thut v phng php th i vi Sorbitol.
2. Cc yu cu k thut quy nh trong Quy chun ny c th theo JECFA
monograph 1 - Vol. 4, ngoi tr mt s php th ring c m t trong cc ph lc.
Cc phng php th c hng dn trong Quy chun ny khng bt buc phi
p dng, c th s dng cc phng php th khc tng ng.
3. Ly mu theo hng dn ti Thng t 16/2009/TT-BKHCN ngy 02 thng
6 nm 2009 ca B Khoa hc v Cng ngh v hng dn kim tra nh nc v
cht lng hng ha lu thng trn th trng v cc quy nh khc ca php lut
c lin quan.
III. YU CU QUN L
1. Cng b hp quy
1.1. Cc cht ngt tng hp phi c cng b ph hp vi cc quy nh ti
Quy chun ny.
1.2. Phng thc, trnh t, th tc cng b hp quy c thc hin theo Quy
nh v chng nhn hp chun, chng nhn hp quy v cng b hp chun, cng
b hp quy ban hnh km theo Quyt nh s 24/2007/Q-BKHCN ngy 28 thng 9
nm 2007 ca B trng B Khoa hc v Cng ngh v cc quy nh ca php lut.
2. Kim tra i vi cht ngt tng hp
Vic kim tra cht lng, v sinh an ton i vi cc cht ngt tng hp phi
thc hin theo cc quy nh ca php lut.
IV. TRCH NHIM CA T CHC, C NHN
1. T chc, c nhn phi cng b hp quy ph hp vi cc quy nh k
thut ti Quy chun ny, ng k bn cng b hp quy ti Cc An ton v sinh thc
phm v bo m cht lng, v sinh an ton theo ng ni dung cng b.

2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng

cc cht ngt tng hp sau khi hon tt ng k bn cng b hp quy v bo m cht
lng, v sinh an ton, ghi nhn ph hp vi cc quy nh ca php lut.
V. T CHC THC HIN
1. Giao Cc An ton v sinh thc phm ch tr, phi hp vi cc c quan chc
nng c lin quan hng dn trin khai v t chc vic thc hin Quy chun ny.
2. Cn c vo yu cu qun l, Cc An ton v sinh thc phm c trch nhim
kin ngh B Y t sa i, b sung Quy chun ny.
3. Trng hp hng dn ca quc t v phng php th v cc quy nh
ca php lut vin dn trong Quy chun ny c sa i, b sung hoc thay th th
p dng theo vn bn mi.

Ph lc 1
YU CU K THUT V PHNG PHP TH I VI MANNITOL
1. Tn khc, ch s

D-Mannitol, manit, Mannitol

INS 421
ADI khng gii hn

2. nh ngha
Tn ha hc

D-Mannitol

M s C.A.S.

69-65-8

Cng thc ha hc

C6H14O6

Cng thc cu to

CH2OH
HO C

HO C

H C OH
H C OH
CH2OH

Khi lng phn t

182,17

3. Cm quan

Bt kt tinh trng, khng mi

4. Chc nng

Cht ngt tng hp, cht gi m, cht to kt cu, cht n

nh, cht n.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, tan rt t trong ethanol, thc t khng tan

trong ether.

Khong nng chy

164 - 169oC.

Sc k lp mng

t yu cu.
(Tin hnh theo ch dn phn Sc k lp mng ca cc
Polyol ti JECFA monograph 1 - Vol.4)
S dng nh sau:
Dung dch chun
Ha tan 50 mg Mannitol chun i chiu (USP) trong 20 ml
nc.
Dung dch th
Ha tan 50 mg mu th trong 20 ml nc

5.2. tinh khit

Gim khi lng khi lm Khng c qu 0,3%. (sy 105C trong 4 gi)
kh

Nng sut quay cc

[]20,D: trong khong +23 v +25o.

pH

Trong khong 5 - 8

Tro sulfat

Khng c qu 0,1%

Clorid

Khng c qu 70,0 mg/kg

Sulfat

Khng c qu 100,0 mg/kg

Nickel

Khng c qu 2,0 mg/kg

ng kh

Khng c qu 0,3%

ng tng s

Khng c qu 1,0% (tnh theo glucose)

Ch

Khng c qu 1,0 mg/kg

5.3.
Hm
C6H14O6

lng Khng c nh hn 96,0% v khng ln hn 102,0% tnh

theo ch phm kh.

6. Phng php th
6.1 tinh khit
Nng sut quay cc

Th theo hng dn ti JECFA monograph 1 - Vol.4- Cn

chnh xc v ha tan 2,0 g mu th v 2,6 g dinatri
tetraborat trong khong 20 ml nc c lm nng
trc ti khong 30 oC, lc lin tc trong 15-30 pht, khng
lm nng thm. Pha long dung dch trong ny ti 25 ml vi
nc.

pH

Th theo hng dn ti JECFA monograph 1 - Vol.4-Thm

0,5 ml dung dch kali clorid bo ha vo 10 ml dung dch
mu th 10% (kl/tt), sau o pH.

Tro sulfat

Th theo hng dn ti JECFA monograph 1 - Vol.4Phng php I-Th trn 2 g mu th

Clorid

Th theo hng dn ti JECFA monograph 1 - Vol.4-Th

trn 10 g mu th bng Php th gii hn clorid, dng 2,0
ml acid hydrocloric 0,01 N lm dung dch i chng.

Sulfat

Th theo hng dn ti JECFA monograph 1 - Vol.4-Th

trn 10 g mu th bng Php th gii hn sulfat, dng 2,0
ml acid sulfuric 0,01 N lm dung dch i chng.

Nickel

Th theo hng dn ti JECFA monograph 1 - Vol.4-Tin

hnh theo ch dn phn Nickel trong Polyol

ng kh

Th theo hng dn ti JECFA monograph 1 - Vol.4-Tin

hnh theo ch dn phn Cc cht kh (tnh theo glucose),
Phng php II. Khi lng ca ng (I) oxyd phi khng
vt qu 50 mg.

ng tng s

Th theo hng dn ti JECFA monograph 1 - Vol.4-Cho

2,1 g mu th vo bnh 250 ml lp kht vi mt ng ni thy
tinh mi, thm 40 ml acid hydrocloric 0,1 N, lp sinh hn
hi lu, v un hi lu trong 4 gi. Chuyn dung dch ny
sang cc 400 ml, ra sch bnh vi khong 10 ml nc,
trung tnh bng natri hydroxyd 6 N v tin hnh nh ch dn
trong phn Phng php chung cho cc cht kh (tnh
theo glucose), Phng php II. Khi lng ca ng (I)
oxyd phi khng vt qu 50 mg

Ch

Th theo hng dn ti JECFA monograph 1 - Vol.4. S

dng k thut hp th nguyn t thch hp cho hm lng
quy nh xc nh. La chn c mu th v phng
php chun b mu da trn nguyn tc ca phng php
m t trong JECFA monograph 1 - Vol.4 phn cc phng
php phn tch cng c.

6.2. nh lng
S dng sc k lng xc nh hm lng Mannitol ca
mu th (xem JECFA monograph 1 - Vol.4)
Thit b
Sc k lng (HPLC)
Pht hin: detector o khc x duy tr nhit khng
i
My ghi tch phn
Ct: AMINEX HPX 87 C (nha dng calci), di 30 cm,
ng knh trong 9 mm
Dung mi ra gii: nc ct hai ln c loi kh (lc qua
mng lc Millipore 0,45 m)
iu kin sc k
Nhit ct: 850,5 oC
Lu lng dng: 0,5 ml /pht
Dung dch chun
Ha tan mt lng cn chnh xc Mannitol chun i chiu
trong nc thu c dung dch c nng khong 10,0
mg Mannitol trong 1 ml.
Dung dch th
Cho khong 1 g mu th c cn chnh xc vo bnh nh
mc 50 ml, pha long bng nc n vch v lc u.
Tin hnh
Tim ring bit cng th tch (khong 20 L) dung dch th
v dung dch chun vo h thng sc k. Ghi sc v o
p ng ca pic Mannitol. Tnh khi lng ca Mannitol
(n v mg) trong phn mu th ly nh lng theo cng
thc sau:

50 C

At
Ac

Trong :
C = nng , mg/ml, Mannitol trong dung dch chun
At = p ng ca pic Mannitol ca dung dch th
Ac = p ng ca pic Mannitol ca dung dch chun.

Ph lc 2
YU CU K THUT V PHNG PHP TH I VI ACESULFAM KALI
1. Tn khc, ch s

Acesulfame potassium; Acesulfame K;

INS 950
ADI = 0 - 15 mg/kg th trng

2. nh ngha
Tn ha hc

Mui kali ca 6-methyl-1,2,3-oxathiazin-4(3H)-1-2,2-dioxid;

mui kali ca 3,4-dihydro-6-methyl-1,2,3-oxathiazin-4-on2,2-dioxid

M s C.A.S.

55589-62-3

Cng thc ha hc

C4H4KNO4S

Cng thc cu to

H3C

SO2
NK

Khi lng phn t

201,24

3. Cm quan

Bt kt tinh trng, khng mi

4. Chc nng

Cht ngt tng hp, cht iu hng

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, rt t tan trong cn.

Quang ph

Ha tan 10 mg ch phm th trong 1000 ml nc. Dung

dch ny c cc i hp th ti 227 2 nm

Kali

Phi c phn ng c trng ca kali.

(Tin hnh th vi cn thu c khi t 2 g mu th).

To kt ta

Thm vi git dung dch natri cobaltinitrit 10% vo dung

dch 0,2 g ch phm th trong 2 ml dung dch acid acetic
(TS) v 2 ml nc. Trong dung dch c kt ta mu vng.

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 1,0% (105oC; 2 gi).

pH

5,5 7,5 (dung dch 1%).

Tp cht hu c

t i vi 20 mg/kg thnh phn p ng vi UV.

Xem m t trong phn phng php th

Florid

Khng c qu 3,0 mg/kg.

(Phng php III; s dng c mu th thch hp v th
tch dung dch chun ph hp thit lp ng chun)

Ch

Khng c qu 1,0 mg/kg.

5.3. Hm lng
C4H4KNO4S

Khng c nh hn 99,0% v khng ln hn 101,0% tnh

theo ch phm lm kh.

6. Phng php th
6.1. tinh khit
Tp cht hu c

Tin hnh theo ch dn trong phn phng php sc k

(Sc k lng hiu nng cao, FNP 5) theo iu kin sau v
s dng acid 4-hydroxybenzoic ethyl ester lm cht i
chiu:
Ct: thp khng g 25 cm 4,6 mm
Pha tnh: Pha ngc (C18 silica gel, 3 - 5 m)
Ra gii: ng dng
Pha ng: Acetonitril/ tetrabutyl amoni hydrosulfat (TBAHS)
0,01 mol/L trong nc (40:60)
Tc dng: Khong 1 ml/pht
Detector: UV hoc Diod array, 227 nm
Th tch tim: 20 l dung dch ch phm th 10 g/L trong
nc kh ion
H thng sc k phi c kh nng tch kali acesulfam v
acid 4-hydroxybenzoic ethyl esther vi phn gii bng 2.
Nu pic khc ngoi kali acesulfam xut hin trong khong 3
ln thi gian ra gii ca kali acesulfam, tin hnh phn
tch ln th hai vi 20 l dung dch ch phm th 0,2 mg/L.
Tng din tch tt c cc pic c ra gii trong ln phn
tch th nht vi thi gian chy gp 3 ln thi gian ra gii
ca kali acesulfam, tr pic ca kali acesulfam khng c
ln hn din tch pic ca kali acesulfam trong ln phn tch
th hai.

Ch

Th theo hng dn ti JECFA monograph 1 - Vol.4 . S

dng k thut hp th nguyn t thch hp xc nh.
La chn c mu th v phng php chun b mu da
trn nguyn tc ca phng php m t trong JECFA
monograph 1 - Vol.4 phn cc phng php phn tch
cng c.

6.2. nh lng

Cn khong 0,15 g (chnh xc n mg) mu th kh, ha

tan trong 50,0 ml acid acetic bng (qu trnh ha tan c th
chm) v chun bng acid percloric 0,1 N, xc nh
im kt thc chun bng o th hoc s dng ch th l
hai git dung dch tm tinh th (TS) v chun bng acid
percloric 0,1 N ti khi chuyn sang mu lam lc bn trong t
nht 30 giy. Tin hnh lm mt mu trng song song v
hiu chnh nu cn.
Mi ml acid percloric 0,1 N tng ng vi 20,12 mg
C4H4KNO4S.

Ph lc 3
YU CU K THUT V PHNG PHP TH I VI ISOMALT
1. Tn khc, ch s

Isomaltulose hydro ha
INS 953
ADI Khng gii hn

2. nh ngha

L hn hp ca cc mono v disaccharid hydro ha m

thnh phn chnh l cc disaccharid sau:

Tn ha hc

6-O- -D-Glucopyranosyl-D-sorbitol (1,6-GPS) v

1-O- -D-Glucopyranosyl-D-mannitol dihydrat (1,1-GPM)

M s C.A.S.

64519-82-0

Cng thc ha hc

6-O- -D-Glucopyranosyl-D-sorbitol: C12H24O11

1-O- -D-Glucopyranosyl-D-mannitol dihydrat: C12H24O11.H2O

Cng thc cu to

CH2 OH

CH2OH
HO C H
CH2OH
H
OH

H C OH

CH2

OH

1,6-GPS
Khi lng phn t

H
H
OH

H C OH

OH
H

CH2 OH

HO C H
O H

H C OH
HO C H
O H

H C OH

H C OH
O

OH
H

CH2

OH

1,1-GPM (khng c nc trong

tinh th)

6-O- -D-Glucopyranosyl-D-sorbitol: 344,32

1-O- -D-Glucopyranosyl-D-mannitol dihydrat: 380,32

3. Cm quan

Tinh th trng hoc khng mu, ht m nh.

4. Chc nng

Cht ngt tng hp, cht n, cht chng ng vn, cht lm

bng.

5. Yu cu k thut
5.1. nh tnh
tan

D tan trong nc, rt t tan trong cn.

Sc k lp mng

t yu cu (m t trong phn Phng php th).

5.2. tinh khit

Nc

Khng c qu 7,0% (phng php Karl-Fischer)

Tro sulfat

Khng c qu 0,05%. (Cn 5 g mu th).

D-mannitol

Khng c qu 3,0%.

D-sorbitol

Khng c qu 6,0%.

ng kh

Khng c qu 0,3%.

Nickel

Khng c qu 2,0 mg/kg.

Ch

Khng c qu 1,0 mg/kg.

5.3. Hm lng

Khng c nh hn 98,0% mono- v di-saccarid hydro ha

v khng nh hn 86,0% hn hp ca 6-O-alpha-Dglucopyranosyl-D-sorbitol v 1-O-alpha-D-glucopyranosyl-Dmannitol tnh theo ch phm khan.

6. Phng php th
6.1. nh tnh
Sc k lp mng

Bn mng sc k
Bn mng sc k l bn nhm hoc knh di ~ 12 cm ph lp
pha tnh l Kieselgel 60 F254, (Art. 5554, Merck hoc tng
ng) dy ~ 0,2 mm.
Dung dch chun:
Ha tan 500 mg mi loi ng sau y trong 100 ml nc:
Sorbitol, mannitol, lactilol, 6-O- -D-Glucopyranosyl-D-sorbitol
(1,6 GPS), 1-O- -D-Glucopyranosyl-D-mannitol (1,1 GPM)
Dung dch th:
Ho tan 500 mg mu trong 100 ml nc.
Dung mi A:
Isopropanol/n-butanol/dung dch acid boric (25 mg/ml)/acid
acetic/acid propionic (50/30/20/2/16 - tt/tt/tt/tt/tt).
Dung mi B:
Ethyl acetat/pyridin/nc/acid : acid acetic : acid propionic
(50/50/10/5/5 - tt/tt/tt/tt/tt).
Dung dch thuc th hin mu:
S I: Dung dch natri metaperiodat 0,1% (kl/kl).
S II: ethanol/acid sulfuric/anisaldehyd/acid acetic (90/5/1/1 tt/tt/tt/tt).
Tin hnh
Chm ~ 0,3 L mi dung dch chun v dung dch th ln
vch xut pht ca bn mng. Sy kh vt chm trong khng
kh nng. Tin hnh khai trin sc k trong bung khai trin
bo ha h dung mi A hoc B, n khi chiu cao tuyn dung
mi t ~ 10 cm. bn mng kh trong khng kh nng, sau
ngm bn mng trong dung dch thuc th hin mu s I
trong 3 giy.
Ly bn mng ra, kh trong khng kh nng. Ch : bn
mng phi kh c 2 mt. ngm bn mng trong dung dch
thuc th hin mu s II trong 3 giy. Ly bn mng ra,
kh trong khng kh nng n khi c th quan st c mu
ca vt. C th iu chnh tng phn vi mu nn trong
dng khng kh m.
Gi tr Rf gn ng v mu ca vt trn bn mng c trng
ring cho tng cht nh sau:

Hp cht

mu

Rf (trong
Rf (trong
DM A)
DM B)
Mannitol
Hi
0,36
0,40
Sorbitol
nu
0,36
0,36
GPM
Xm-xanh lam
0,28
0,16
GPS
Xm-xanh lam
0,25
0,13
Maltitol
Xanh lc
0,26
0,22
Lactilol
Xanh olive
0,23
0,14
Gi tr Rf c th thay i cht t khi s dng bn mng silicagel
t cc ngun khc nhau.
Vt chnh trn sc k dung dch th isomalt phi tng ng
v Rf v mu sc ca vt GPM v GPS.
6.2. tinh khit
ng kh

Th theo hng dn ti JECFA monograph 1 - Vol.4 - Tin

hnh theo hng dn trong chuyn lun th gii hn cc hp
cht kh (tnh theo glucose) phng php II. Khi lng ng
(I) oxyd khng c qu 50 mg.

Nickel

Dung dch th:

Ha tan 20,0 g mu th trong hn hp gm dung dch acid
acetic long (TS) v nc, trn ng th tch, sau nh
mc n 100 ml bng hn hp dung mi ny. Thm 2,0 ml
dung dch amoni pyrrolidin-dithiocarbamat 1% (kl/tt) v 10 ml
methyl isobutyl keton. Trn u v yn tch lp, ly lp
methyl isobutyl keton tin hnh th nghim tip theo.
Dung dch chun:
Chun b 3 dung dch chun (theo hng dn chun b dung
dch th) nhng thay v cho 20,0 g mu th th cho 0,5 ml; 1,0
ml; 1,5 ml dung dch chun cha 10 mg Ni/L.
Tin hnh:
Chnh thit b v 0 bng cch o dung dch methyl isobutyl
keton (c chun b nh chun b dung dch th nhng
khng cho mu th). o hp th ca dch methyl isobutyl
keton chit ra ti 232,0 nm, s dng n cathod rng Nickel
lm ngun bc x v ngn la acetylen/khng kh.

Ch

Th theo hng dn ti JECFA monograph 1 - Vol.4 . S

dng k thut hp th nguyn t thch hp xc nh. La
chn c mu th v phng php chun b mu da trn
nguyn tc ca phng php m t trong JECFA monograph
1 - Vol.4 phn cc phng php phn tch cng c.

6.3. nh lng

Dung dch chun ni

Ha tan lng va phenyl- -D-glucopyranosid v mannitol
trong nc sao cho thu c dung dch c nng 1 mg
phenyl- -D-glucopyranosid/1g nc v 50 mg mannitol/1 g
nc.

Dung dch chun

Cn chnh xc lng 6-O- -D-Glucopyranosyl-D-sorbitol (1,6
GPS), 1-O- -D-Glucopyranosyl-D-mannitol (1,1 GPM) tnh
theo ch phm lm kh, ho tan ring r trong nc thnh
2 dung dch chun c nng 50 mg/g. ng thi pha mt
dung dch c thnh phn gn ng gm 1 mg mannitol/g v 1
mg sorbitol/g.
Dung dch mu th
Cn khong 1 g mu th (chnh xc n mg) ha tan trong
nc va thu c nng khong 10 g/100 g.
Tin hnh
Ht 100,0 mg dung dch chun v dung dch mu th vo cc
ng nghim c nt, thm vo mi ng 100,0 mg dung dch
chun ni. Loi nc bng cch ng kh v ho tan phn
cn li trong 1,0 ml pyridin Thm vo mi ng 4 mg O-benzylhydroxylamin hydroclorid, y nt v yn ti nhit phng
trong 12 gi. Sau thm 1 ml N-methyl-N-trimethylsilyltrifluoroacetamid (MSTFA) v un nng ti 80 oC trong 12 gi,
trong khi un thnh thong lc, sau ngui. Bm 1 L mi
dung dch ny trc tip vo my sc k kh di iu kin hot
ng nh sau:
Kh mang He (dng ban u ~ 1 ml/pht ti 80 oC v 1 atm,
chia dng 25 ml/pht);
Ct Fused silica HT-8 (25 m x 0,22 mm x 0,25 m) hoc
tng ng;
Bm mu: chng trnh nhit bay hi 30 oC; 270o/pht n
300o (49 pht);
Detector: ion ha ngn la FID; 360 oC;
Chng trnh nhit : 80o (3 pht); 10o/pht n 210o; 5o/pht
n 300o (6 pht).
Thi gian lu gn ng nh sau:
Cc monosaccharid hydro ha:
Mannitol 19,5 pht
Sorbitol 19,6 pht
Chun ni:
Phenyl--D-glucopyranosid 26,8 pht
Maltitol 33,5 pht
Cc disaccharid hydro ha (32 - 36 pht)
1,1-GPS 33,9 pht
1,1-GPM 34,5 pht
1,6-GPS 34,6 pht
Tnh hm lng (%) ca tng thnh phn trong mu (wI) theo
cng thc sau:

Trong
aI = din tch pic ca cu t I (Vs)
aS = din tch pic ca chun ni (Vs)
mS = Khi lng ca chun ni dng dn xut ha (mg
d.s.)
mISOMALT = Khi lng mu th tham gia dn xut ha (mg
d.s.)
FI = H s tng quan p ng fI/fS
fI = H s p ng ca cu t I : fI =(aI/mI) x (100/% tinh
khit)
fS = H s p ng ca chun ni: fS =(aS/mS) x (100/% tinh
khit)
mI, mS = Khi lng cu t I hoc chun ni dng cho qu
trnh dn xut ha mu th (mg d.s.).
Ch : S dng maltitol lm chun ni khi tnh hm lng cc
disaccharid hydro ha (VD 1,1-GPM; 1,6-GPS) v phenyl- -Dglucopyranosid lm chun ni khi tnh hm lng cc
monosaccharid hydro ha (mannitol, sorbitol). tnh tng
saccharid khc (hydro ha hoc khng hydro ha) ly 100%
tr i tng hm lng 1,1-GPM; 1,6-GPS; mannitol; sorbitol.

Ph lc 4
YU CU K THUT V PHNG PHP TH I VI SACCARIN
1. Tn khc, ch s

INS 954
ADI = 0 - 5 mg/kg th trng

2. nh ngha
Tn ha hc

1,2-Benzisothiazol-3(2H)-on-1,1-dioxid;
3-oxo-2,3-dihydrobenzo[d]isothiazol-1,1-dioxid

M s C.A.S.

81-07-2

Cng thc ha hc

C7H5NO3S

Cng thc cu to

SO2
NH
O
Khi lng phn t

183,18

3. Cm quan

Tinh th hoc bt tinh th trng, khng mi hoc c mi

thm nh.

4. Chc nng

Cht ngt tng hp

5. Yu cu k thut
5.1. nh tnh
tan

t tan trong nc; tan trong dung dch kim, t tan trong
ethanol.

Tnh acid

Dung dch mu th bo ha c tnh acid.

Dn xut ha thnh acid t yu cu (m t trong phn Phng php th).

salicylic
Dn xut ha thnh hp t yu cu (m t trong phn Phng php th)
cht c hunh quang
5.2. tinh khit
o
Gim khi lng khi lm Khng c qu 1,0% (105 C; 2 gi)
kh

Khong nng chy

226 - 230oC.

Tro sulfat

Khng c qu 0,2% (Cn 2 g mu th).

Acid benzoic
salicylic

acid t yu cu (m t trong phn Phng php th).

Cc hp cht d b than t yu cu (m t trong phn Phng php th).

ha
Toluensulfonamid

Khng c qu 25,0 mg/kg.

Selen

Khng c qu 30,0 mg/kg.

Ch

Khng c qu 1,0 mg/kg.

5.3. Hm lng
C7H5NO3S

Khng c nh hn 99,0% v khng ln hn 101,0% tnh

theo ch phm lm kh.

6. Phng php th
6.1 nh tnh
Dn xut ha thnh acid Ha tan 0,1 g mu th trong 5 ml natri hydroxyd 5%. Cho
bay hi n kh v nung nh cn trn ngn la nh n khi
salicylic
khng cn mi amoniac thot ra. Sau khi ngui, ha tan
cn trong 20 ml nc, trung ha dung dch bng dung dch
acid hydrocloric long (TS) v lc. Thm 1 git dung dch
st (III) clorid (TS) vo dch lc, dung dch c mu tm.
Dn xut ha thnh hp Trn 20 mg mu th vi 40 mg resorcinol, thm 10 git
acid sulfuric, un cch du hn hp ti 200 oC trong 3 pht,
cht c hunh quang
sau khi lm mt, thm 10 ml nc v lng d dung dch
natri hydroxyd (TS). Dung dch ny c hunh quang xanh
lc.
6.2 tinh khit
Acid benzoic
salicylic

acid Thm nh git dng dch st (III) clorid (TS) vo dung dch
mu th bo ha. Khng c xut hin kt ta mu tm.

Cc hp cht d b than Ha tan 0,2 g mu th trong 5 ml dung dch acid sulfuric

(TS). Gi ti nhit 48 - 50oC trong 10 pht. Mu ca
ha
dung dch khng c m hn mu vng nu nht ca
dung dch i chng A (Matching Fluid A).
Selen

Th theo hng dn ti JECFA monograph 1 - Vol.4 - Tin

hnh theo hng dn trong chuyn lun th gii hn selen,
phng php I, cn 0,2 g mu th.

Ch

Th theo hng dn ti JECFA monograph 1 - Vol.4 . S

dng k thut hp th nguyn t thch hp xc nh.
La chn c mu th v phng php chun b mu da
trn nguyn tc ca phng php m t trong JECFA
monograph 1 - Vol.4 phn cc phng php phn tch
cng c.

6.3. nh lng

Cn khong 0,5 g (chnh xc n mg) mu th c

lm kh, ha tan trong 75 ml nc nng. Lm ngui nhanh
v thm dung dch phenolphtalein (TS), chun vi dung
dch natri hydroxyd 0,1 N.
Mi ml natri hydroxyd 0,1 N tng ng vi 18,32 mg
C7H5NO3S.

Ph lc 5
YU CU K THUT V PHNG PHP TH I VI SORBITOL
1. Tn khc, ch s

D-Glucitol, D-Sorbitol, Sorbol

INS 420
ADI khng gii hn

2. nh ngha
Tn ha hc

D-Sorbitol

M s C.A.S.

50-70-4

Cng thc ha hc

C6H14O6

Cng thc cu to

CH2OH
H C OH
HO C

H C OH
H C OH
CH2OH

Khi lng phn t

182,17

3. Cm quan

Bt trng ho nc, bt tinh th, dng vy hoc ht

4. Chc nng

Cht ngt tng hp, cht gi m, cht to kt cu, cht n

nh, cht n.

5. Yu cu k thut
5.1. nh tnh
tan

Rt d tan trong nc, t tan trong ethanol.

Khong nng chy

88 102 oC.

Sc k lp mng

t yu cu (m t trong phn Phng php th)

5.2. tinh khit

Gim khi lng khi lm Khng c qu 1%. (phng php Karl Fisher)
kh
Tro sulfat
Clorid

Khng c qu 0,1%
Khng c qu 50 mg/kg

Sulfat

Khng c qu 100 mg/kg

Nickel

Khng c qu 2 mg/kg

ng kh

Khng c qu 0,3%

ng tng s

Khng c qu 1,0% (tnh theo glucose)

Ch

Khng c qu 1 mg/kg

5.3. Hm lng

Khng c thp hn 97,0% C6H14O6 trong tng cc

glycitol v khng c thp hn 91,0% sorbitol tnh theo
ch phm kh. Thut ng glycitol ch cc hp cht c cng
thc CH2OH-(CHOH)n-CH2OH, n 4.

6. Phng php th
6.1. nh tnh
Sc k lp mng

Tin hnh theo ch dn phn Sc k lp mng ca cc

Polyol ti JECFA monograph 1 - Vol.4.
S dng nh sau:
Dung dch chun
Ha tan 50 mg sorbitol chun i chiu USP trong 20 ml
nc
Dung dch th
Ha tan 50 mg mu th trong 20 ml nc

6.2. tinh khit

Tro sulfat

Th theo hng dn ti JECFA monograph 1 - Vol.4Phng php I-Th trn 2 g mu th.

Clorid

Th theo hng dn ti JECFA monograph 1 - Vol.4-Th

trn 10 g mu th bng Php th gii hn clorid, dng 1,5
ml acid hydrocloric 0,01 N lm dung dch i chng.

Sulfat

Th theo hng dn ti JECFA monograph 1 - Vol.4-Th

trn 10 g mu th bng Php th gii hn sulfat, dng 2,0
ml acid sulfuric 0,01 N lm dung dch i chng.

ng kh

Th theo hng dn ti JECFA monograph 1 - Vol.4 - phn

Cc cht kh (tnh theo glucose), Phng php II. Khi
lng ca ng (I) oxyd phi khng vt qu 50 mg.

ng tng s

Th theo hng dn ti JECFA monograph 1 - Vol.4-Cho

2,1 g mu th vo bnh 250 ml lp kht vi mt ng ni thy
tinh mi, thm 40 ml acid hydrocloric 0,1 N, lp sinh hn
hi lu, v un hi lu trong 4 gi. Chuyn dung dch ny
sang cc 400 ml, ra sch bnh vi khong 10 ml nc,
trung tnh bng natri hydroxyd 6 N v tin hnh nh ch dn
trong phn cc cht kh (tnh theo glucose), Phng php
II. Khi lng ca ng (I) oxyd phi khng vt qu 50
mg.

Ch

Th theo hng dn ti JECFA monograph 1 - Vol.4. S

dng k thut hp th nguyn t thch hp cho hm lng
quy nh xc nh. La chn c mu th v phng
php chun b mu da trn nguyn tc ca phng php
m t trong JECFA monograph 1 - Vol.4 phn cc phng
php phn tch cng c.

6.3. nh lng

S dng sc k lng xc nh hm lng Sorbitol ca

mu th (xem JECFA monograph 1 - Vol.4)
Thit b
Sc k lng (HPLC)
Pht hin: detector o khc x duy tr nhit khng
i
My ghi tch phn
Ct: AMINEX HPX 87 C (nha dng calci), di 30 cm,
ng knh trong 9 mm
Dung mi ra gii: nc ct hai ln c loi kh (lc qua
mng lc Millipore 0,45 m)
iu kin sc k
Nhit ct: 850,5oC
Lu lng dng: 0,5 ml /pht
Dung dch chun
Ha tan mt lng cn chnh xc Sorbitol chun i chiu
trong nc thu c dung dch c nng khong 10,0
mg/ml.
Dung dch th
Cho khong 1 g mu th cn chnh xc vo bnh nh mc
50 ml, pha long bng nc n vch v lc u.
Tin hnh
Tim ring bit cng th tch (khong 20 L) dung dch th
v dung dch chun vo h thng sc k. Ghi sc v o
p ng ca pic Sorbitol. Tnh khi lng (mg) ca Sorbitol
trong phn mu th ly nh lng theo cng thc sau:
At
50 C
Ac
Trong :
C = nng , mg/ml, Sorbitol trong dung dch chun
At = p ng ca pic Sorbitol ca dung dch th
Ac = p ng ca pic Sorbitol ca dung dch chun.