CNG HA X HI CH NGHA VIT NAM

QCVN 4-7 : 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM -YU CU K THUT I VI
CHT CHNG TO BT
National technical regulation
on Food Additive - Antifoaming Agent

H NI - 2010

Li ni u
QCVN 4-7:2010/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 24/2010/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 CHNG TO BT
National technical regulation on food additive Antifoaming Agent

I. 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 chng to bt 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 chng to bt 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. Cc cht chng to bt: l ph gia thc phm c s dng vi mc ch
ngn nga v gim thiu s to bt cho cc sn phm 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.

QCVN 4-7 : 2010/BYT

II. YU CU K THUT, PHNG PHP TH V LY MU
1. Yu cu k thut v phng php th i vi cc cht chng to bt c
quy nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
1.1.

Ph lc 1:

Yu cu k thut v phng php th i vi propylen

glycol

1.2.

Ph lc 2:

Yu cu k thut v phng php th i vi polyethylen

glycol

1.3.

Ph lc 3:

Yu cu k thut v phng php th i vi

polyoxyethylen (20) sorbitan monooleat

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 chng to bt 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 chng to bt
Vic kim tra cht lng, v sinh an ton i vi cc cht to bt 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.

QCVN 4-7 : 2010/BYT

2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc cht chng to bt 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.

QCVN 4-7 : 2010/BYT

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

Propanediol, methyl glycol,

INS 1520
ADI= 0-25 mg/kg th trng

2. nh ngha
Tn ha hc

Propan-1,2-diol, 1,2-dihydroxypropan

M s C.A.S.

57-55-6

Cng thc phn t

C3H8O2

Cng thc cu to

OH
H3C

OH

Khi lng phn t

76.10

3. Cm quan

Cht lng snh, trong, khng mu, ht m.

4. Chc nng

Chng to bt, dung mi, cht lm bng, cht lm m.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, ethanol v aceton.

Ph hng ngoi

Ph hng ngoi ca mu phn tn trong kali bromid tng

ng vi ph hng ngoi km theo quy chun ny.

5.2. tinh khit

Nc

Khng c qu 1,0% (Phng php Karl Fischer)

Khong chng ct

Dung dch vi hm lng 99% (tt/tt) c khong chng ct

l 185-189 C.

T trng

d (20,20) = 1,035 1,040.

Tro sulfat

Khng c qu 0,07 %. (Th 5 g mu).

Acid t do

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

Ch

Khng c qu 2,0 mg/kg

5.3. Hm lng C3H8O2

Khng thp hn 99,5 % tnh theo ch phm khan

4

QCVN 4-7 : 2010/BYT

6. Phng php th
6.1. tinh khit
Nc

(Phng php Karl Fischer)

Acid t do

Thm 3 n 6 git dung dch phenol (TS) vo 50 ml

nc, thm dung dch natri hydroxyd 0,1 N cho n khi
dung dch c mu bn vng trong 30 giy. Thm 50 g
mu th c cn chnh xc vo dung dch ny.
Chun bng dung dch natri hydroxyd 0,01 N cho n
khi dung dch tr li mu nh ban u v bn vng
trong 15 giy. Th tch dung dch natri hydroxyd 0,01 N
s dng chun cho 50,0 g mu th Khng c
qu 1,67 ml.

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 ti
JECFA monograph 1 - Vol.4 phn cc phng php
phn tch cng c).

6.2. nh lng
Bm 10 L mu th vo h o sc k kh ph hp, c
trang b detector o dn nhit v ct tch lm bng
thp khng r, 1 m x 1/4 in, nhi Carbowax 20 M 4% trn
Chromosorb T 40/60 mesh, hoc vt liu tng ng.
S dng kh mang l heli vi tc l 75 ml/pht. Nhit
ca cng injector l 240 C, nhit ct t 120 n
200 C, c t chng trnh tng nhit vi tc 5
C/pht, v nhit block l 250 C. Trong cc iu kin
trn, thi gian lu ca propylen glycol l khong 5,7 pht
v thi gian lu ca 3 ng phn ca dipropylen glycol
ln lt l 8,2; 9,0 v 10,2 pht.
o din tch cc pic, tnh phn trm din tch pic ca
propylen glycol trn tng din tch cc pic v quy ra phn
trm khi lng.

QCVN 4-7 : 2010/BYT

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

PEG, Macrogol;
INS 1521
ADI= 0 - 10 mg/kg th trng

2. nh ngha

L cc polymer cng hp ca ethylen oxyd v nc, c

k hiu bng con s tng ng vi trng lng phn t.

Tn ha hc

alpha-Hydro-omega-hydroxypoly (oxy-1,2-ethandiol)

M s C.A.S.

25322-68-3

Cng thc phn t

(C2H4O)n+1H2O

Cng thc cu to

HOCH2 - (CH2 - O - CH2)n - CH2OH

Khi lng phn t

200

3. Cm quan

Cc PEG c khi lng phn t nh hn 700 thng l cc

cht lng trong sut n hi c, khng mu, ht m nh v
c mi nh. Cc PEG c khi lng phn t trong khong t
700 n 900 l cc cht na rn. Cc PEG c khi lng
phn t ln hn 1000 l cht rn dng sp, dng vy, hoc
bt trn chy, mu trng kem.

4. Chc nng

Chng to bt, dung mi, cht lm bng, cht lm m.

9500

5. Yu cu k thut
5.1. nh tnh
tan

Cc Polyethylen glycol c khi lng phn t ln hn hoc

bng 1000 d tan trong nc; cc polyethylen glycol tan
trong nhiu dung mi hu c nh cc keton bo v cc cn
bo, cloroform, glycol ether, ester v cc hydrocarbon thm;
khng tan trong ether v phn ln cc hydrocarbon bo; khi
khi lng phn t tng, tan trong nc v tan trong
cc dung mi hu c gim.

Khi lng phn t

Cc PEG c khi lng phn t di 1000: khng thp hn

95,0% v khng qu 105,0% gi tr cng b.
Cc PEG c khi lng phn t trong khong t 1000 n
7000: khng thp hn 90,0% v khng qu 110,0% gi tr
cng b.
Cc PEG c khi lng phn t ln hn 7000: khng thp
hn 87,5% v khng qu 112,5% gi tr cng b.
Khong nht,theo n v cSt, ca cc PEG nhit
100 0,3 C:

nht

QCVN 4-7 : 2010/BYT

KLPT trung bnh
200
300
400
500
600
700
800
900
1000
1100
1200
1300
1400
1450
1500
1600
1700
1800
1900
2000
2100
2200
2300
2400
2500
2600
2700
2800
2900
3000
3250
3350
3500
3750
4000
4250
4500
4750
5000
5500
6000
6500
7000
7500
8000

Khong nht, cSt

4,1-4,8
5,4-6,4
6,8-8,0
8,3-9,6
9,9-11,3
11,5-13,0
12,5-14,5
15,0-17,0
16,0-19,0
18,0-22,0
20,0-24,5
22,0-27,0
24,0-30,0
25,0-32,0
26,0-33,0
28,0-36,0
31,0-39,0
33,0-42,0
35,0-45,0
38,0-49,0
40,0-53,0
43,0-56,0
46,0-60,0
49-65
51-70
54-74
57-78
60-83
64-88
67-93
73-105
76-110
87-123
99-140
110-158
123-177
140-200
150-228
170-250
206-315
250-390
295-480
350-590
405-735
470-900

Vi cc PEG khng cho trong bng, tnh ton gi tr gii hn

bng cch ni suy.
7

QCVN 4-7 : 2010/BYT

5.2. tinh khit
pH

4,5

7,5 (dung dch 1/20)

Tro sulfat

Khng c qu 0,1 %.
Th 5 g mu

acid

Khng qu 0,05% kl/kl (tnh theo acid acetic).

1,4-Dioxan

Khng c qu 10,0 mg/kg.

Ethylen oxyd

Khng c qu 0,02%

Ethylen glycol v
diethylen glycol

Tng hm lng khng c qu 0,25% (kl/kl) tnh ring

hoc kt hp.

Ch
6. Phng php th

Khng c qu 1,0 mg/kg

6.1. tinh khit

acid

Chuyn 6 g mu th vo bnh nn 250 ml, thm dung dch

phenolphtalein (TS) v 50 ml ethanol trung tnh ri chun
bng dung dch kali hydroxyd 0,1 N trong ethanol ti khi dung
dch chuyn mu hng bn vng trong t nht 15 giy. Th
tch dung dch kali hydroxyd 0,1 N trong ethanol chun
khng c c qu 0,5 ml.

1,4-Dioxan

Tin hnh nh hng dn trong chuyn lun th gii hn

dioxan bng Sc k kh. Xem thm phn phng php sc k
kh khng gian hi trong Phn phng php th Ethylen
oxyd di y.

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 ti JECFA monograph 1
- Vol.4 phn cc phng php phn tch cng c).

6.2. nh tnh
Khi lng phn t

Dung dch Anhydrid phthalic

Cho 49 g anhydrid phthalic vo chai mu nu h phch v
ha tan trong 300 ml pyridin (mi c ct li loi
anhydrid phthalic). Lc mnh chai ha tan hon ton.
yn qua m trc khi s dng.

QCVN 4-7 : 2010/BYT

Chun b mu polyethylen glycol lng
Cn thn thm 25 ml dung dch anhydrid phthalic vo bnh
kh, sch, c p sut chu nhit. Thm vo bnh mt lng
cn chnh xc ca mu th, tng ng vi khi lng
phn t ca n chia cho 160 (v d, vi PEG 200 cn
khong 1,3 g mu th, vi PEG 600 cn khang 3,8g mu
th). ng nt bnh li, gi cn thn trong ti vi.
Chun b mu polyethylen glycols rn
Cn thn thm 25 ml dung dch anhydrid phthalic vo mt
bnh p sut chu nhit sch v kh. Thm vo bnh mt
lng cn chnh xc ca mu th nung chy, tng
ng vi khi lng phn t ca n chia cho 160. Do
tan hn ch ca mu, khng ly nhiu hn 25 g mu th.
Thm vo 25 ml pyridin ( c ct li loi anhydrid
phthalic). Lc u ha tan hon ton, ng nt bnh v gi
cn thn trong ti vi.
Tin hnh
t bnh ng mu vo b nc mc ngang vi vch cht
lng trong bnh v gi nhit trong khong t 96 n 100
C. un bnh trong 30 n 60 pht. Ly bnh ra v lm lnh
n nhit phng. M np bnh cn thn x p sut, ly
bnh ra khi ti vi, thm 5 git dung dch phenolphtalein
trong pyridin 1/100. Chun bng dung dch natri hydroxyd
0,5 N n khi xut hin mu hng bn vng trong 15 giy.
Ghi li th tch cn dng, S, theo ml. Tin hnh lm mu
trng song song vi 25 ml dung dch anhydrid phthalic cng
vi lng pyridin thm vo mu. Ghi li th tch natri
hydroxyd 0,5 N cn dng chun , B, theo ml. Tnh khi
lng phn t ca mu theo cng thc sau:
Khi lng phn t = 2000 W / [(B-S)N]
trong :
W = khi lng mu th, g
B = th tch dung dch NaOH 0,5 N dng chun mu
trng, tnh theo ml
S = th tch dung dch NaOH 0,5 N dng chun mu
th, tnh theo ml
N = chun chnh xc ca NaOH

QCVN 4-7 : 2010/BYT

Phng php d kin khc dng sc k ry kch thc (sc
k gel thm thu)
1. Cc polyethylene glycol c khi lng phn t d on
di 1000
Thit b
Dng sc k lng hiu nng cao HPLC thch hp, c trang
b b phn o khc x vi phn v ct 0,60 m x 7,7 mm
(ng knh trong), nhi gel PL 10 m 50 , dng pha ng
l tetrahydrofuran.
iu kin o
Cc thng s o c th thay i ty thuc vo mi h o
nhng c th dng cc iu kin sau thu c mt sc
hp l:
-Tc pha ng: 1 ml/pht
- p sut: 35 bar
- Th tch mu bm: 20 l dung dch 1% (kl/tt)
- Nhit detector: 25 C 0,1 C
Qui trnh ny cho php nhn bit cc PEG sau khi so snh
vi cht chun v dng kim tra cc hn hp PEG.
2. Cc polyethylene glycol c khi lng phn t d an
ln hn hoc bng 1000
Thc hin cng mt qui trnh nh trn nhng vi pha ng l
Tetrahydrofuran/n-heptan (80/20).
Th tch ra gii d kin ca PEG, ty thuc vo mi h o
v iu kin o, c cho trong bng sau:
KLPT

V ra gii, ml

35 000

21,2

10 000

22,8

6 000

24,2

4 000

25,1

2 000

26,8

1 000

28,4

10

QCVN 4-7 : 2010/BYT

KLPT

nht

V ra gii, ml

35000

21,2

10000

22,8

6000

24,2

4000

25,1

2000

26,8

1000

28,4

Thit b
Nht k Ubbelohde, c minh ha trong hnh v di y,
c th dng xc nh mt cch hiu qu nht ca cc
polyethylen glycol.

Hnh. Nht k Ubbelohde (cc knh thc c cho theo

mm)
xc nh nht trong khong t 300 to 600 centistoke,
dng thit b o nht c 3, c ng knh mao qun l
2,00 0,04 mm. Thit b o nht phi c t trn gi
ph hp vi knh thc ca cc ng tch nh trong hnh
v, v c th gi thit b o nht thng ng. Mi tn
trong bu A ch th tch ti a v ti thiu ca cht lng, s
dng trong cc iu kin ph hp. Th tch ca bu B xp x
5 ml.
Hiu chun thit b o nht
Xc nh hng s nht (C) cho mi thit b o nht bng
cch s dng mt loi du c nht bit. Nghing thit
b khong 30 so vi phng thng ng, bu A nm di
mao qun, v a mt lng mu vo ng 1 mc cht
lng ngang vi vch np di. Vch cht lng khng c
php cao hn vch np trn khi cho thit b o nht quay
v phng thng ng v cho mu th chy ra t ng 1.
11

QCVN 4-7 : 2010/BYT

Np cht lng vo thit b sao cho ng hnh ch U t y
phi hon ton khng c bt kh. Sau khi t thit b o
nht vo bnh iu nhit trong thi gian mu cn bng
nhit, t mt ngn tay ln ng 3 v ht ng 2 cho n khi
cht lng c ht vo n gia bu C. Ngng ht, rt tay ra
khi ng 3, t ln ng 2 cho n khi mu th chy tng git
ra khi u di ca mao qun. Rt tay ra khi ng 2, tnh
khong thi gian (chnh xc n 0,1 giy) cn thit mt
khum ca cht lng chuyn dch t vch T1 n vch T2.
thu c kt qu chnh xc trong mt khong thi gian hp
l, thit b cn phi c iu chnh sao cho khong thi gian
tri l t 80 n 100 giy.
Tnh hng s nht C theo cng thc sau C = cSt/t1 trong
cSt l nht, tnh theo nv centistoke, v t1 l thi gian
chy (efflux), tnh theo giy, ca cht lng chun.
Xc nh nht ca mu th, gi nhit 1000,3 C v
s dng nht k mao qun c thi gian chy t nht l 200
giy (s) i vi PEG cn kim tra. nht phi nm trong
gii hn ch nh trong bng, hoc c ni suy t cc gi tr
cho trong bng.
6.2. tinh khit
Ethylen oxyd

Dung dch Morpholin

Trn 1 phn morpholin c ct li vi 9 phn methanol
khan.
Ch th hn hp
Cn 0,050 g 4,4'bis-(amino-1-naphthylazo-2,2'stilbendisulfonic acid) v 0,010 g vng brilliant vo bnh 65
ml. Dung pipet ly 1,5 ml dung dch natri hydroxyd 0,1 N vo
bnh, trn u. Thm vo 3,5 ml nc, trn u. Chuyn
hn hp trn vo bnh bo qun, trng ra bng 45 ml
methanol, trn u.
Dung dch acid hydrocloric trong methanol chun
Trn 8,5 ml acid hydrocloric v 1000 ml methanol khan.
Chun li nng bng cch ly 9 ml dung dch, chun
bng dung dch NaOH 0,1 N (TS) vi ch th phenolphtalein.
Chun ho li nng nu dng dung dch ny sau 48 gi.
chun b mu th trng, chuyn 25 g mu th c
cn chnh xc vo bnh cu, lc u tan hon ton. Chun
bng dung dch acid hydrocloric trong methanol chun
ha n khi chuyn mu xanh bic.

12

QCVN 4-7 : 2010/BYT

Khi gn ti im kt thc phi thm t t tng lng nh
cht chun.
Thm 50 ml dung dch morpholin vo bnh p sut chu nhit.
To mu thuc th trng bng cch thm mt lng tng
ng Morpholin vo mt bnh tng t khc. Thm vo
bnh th nht 25 g mu th c cn chnh xc, lc u
tan hon ton. Gi cn thn cc bnh ny trong ti vi, t
2 bnh cnh nhau trong b cch thy iu nhit 98 2 C
trong 30 pht, gi mc nc trong b trn mc cht lng
trong bnh mt cht. Ly cc bnh ra, ngui n nhit
phng. Khi cc bnh ngui, ni lng ti vi bc, m np
bnh x p lc v g ti vi bc ra. T t thm 20 ml
anhydrid acetic khan vo mi bnh, lc u tan hon ton.
yn nhit phng trong 15 pht. Nu cc bnh vn
m, ngui n nhit phng. Thm vo mi bnh 4 n
6 git ch th hn hp v chun bng dung dch acid
hydrocloric trong methanol chun n khi chuyn mu xanh
bic. Khi gn ti im kt thc phi thm t t tng lng rt
nh cht chun.
Tnh phn trm ethylen oxyd theo cng thc sau:

trong :
N = chun ca dung dch acid hydrocloric trong methanol
chun
A, B, and C = th tch (ml) tng ng dng chun mu
th, mu thuc th trng v mu th trng,
W1 and W 2 = khi lng (g) tng ng ca mu th ly cho
phn ng v cho mu th trng.
Sc k kh khng gian hi (headspace):
Phng php xut khc xc nh 1,4-Dioxan and
Ethylen oxyd
Nguyn tc:
Sau khi thm nc vo mu, phn tch ethylen oxyd v
1,4-dioxan bng sc k kh khng gian hi (headspace)
Dung dch chun
-

Dung dch gc 1,4-Dioxan

13

QCVN 4-7 : 2010/BYT

-

Dung dch chun ca 1,4-dioxan trong nc c pha

bng cch cn khong 1,00 g 1,4-dioxan trong100 ml
nc ct (dung dch gc) sau pha long nhiu ln.
S dng hai dung dch chun 20 and 100 g 1,4dioxan/ml nc.

Dung dch gc chun Ethylen Oxyd (EO)

Thm 25 ml nc ct vo l bm mu nhiu ln (multidose

injection vial) . ng septum li v cm mt syranh khng d
kh vo. T t a 20 ml kh ethylen oxyd (khong 40 mg)
vo dung dch. Xc nh chnh xc khi lng ethylen oxyd
thm vo bng cch cn l mu trc v sau thi thm kh
(dung dch gc).
Chun b hai dung dch lm vic chun bng cch pha long
2 v 10 g ethylen oxyd trong 1 ml nuc, pha long nhiu
ln.
Thit b
Dng my sc k kh trang b detector ion ha ngn la (FID),
vi ct mao qun 30 m trng dimethylpolysiloxan, ng
knh trong 0,25 mm, dy lp trng l 1,0 m.
iu kin o
iu kin o c th thay i ty thuc vo mi thit b c th,
nhng c th dng nhng iu kin sau thu c sc
ph hp:
t chng trnh ly mu khng gian hi (Headspace
Sampler)
- Thi gian cn bng nhit: 45 pht
- Nhit : 70 C
- Nhit ng truyn: 150 C
- Thi gian t p lc: 30 giy
- Thi gian bm: 6 giy
- Thi gian phn tch: 45 pht
iu kin o sc k kh
Nhit : Ct, 50 C (gi trong 5 pht), tng ln 180 C vi
tc tng nhit 5 C /pht
Detector (FID): 250 C
Kh mang: Heli, 1 ml/pht
p sut kh mang : 0,7 bar
14

QCVN 4-7 : 2010/BYT

T l chia dng: 40 : 1
Hydro v khng kh: cho FID
Chun b mu
Chuyn khong 1 g mu c cn chnh xc n 0,1 mg
vo l mu v thm 1 ml nc ct. ng l mu li v t
vo trong thit b phn tch khng gian hi cn bng trong
45 pht ti 70 C. Chun b 2 l mu trong cng iu kin,
thm vo mi l mu 1 g mu th ( c cn chnh xc ti
0,1 mg) v 1 ml dung dch gc 1,4-dioxan v EO.
Dung dch chun lm vic
Pha hai dung dch chun A v B ( thm chun) nh sau:
A. 1 ml dung dch gc EO c nng xp x 200 mg EO/100
ml + 2 ml dung dch gc 1,4-dioxan c nng xp x 1000
mg dioxan/100 ml + nc n th tch 100 ml. Dung dch
ny s c pha long vi nc theo t l 1 : 10 c nng
khong 2 g EO/ml v 20 g 1,4-dioxan/ml.
B. 1 ml dung dch gc EO c nng xp x 500 mg EO/100
ml + 5 ml dung dch gc 1,4-dioxan c nng xp x 1000
mg dioxan/100 ml + nc n th tch 100 ml. Dung dch ny
s c pha long vi nc theo t l 2 : 10 c nng
khong 10 g EO/ml v 100 g 1,4-dioxan/ml.
Tnh ton
Nng ca cht (i) c th tnh theo cng thc sau:
g cht (i)/g = (W i Ai)/Ais
trong
g cht i/g = khi lng ca 1,4-dioxane hoc EO trong mu
th [g/g]
Wi = khi lng cht i c thm vo, chun li theo 1 g
mu th [g/g]
Ai = Din tch pic ca cht i trong mu th, chun li theo 1 g
mu th
Ais = Din tch pic ca cht i trong mu th c thm
chun, chun li theo 1 g mu th

15

QCVN 4-7 : 2010/BYT

Ethylen glycol v
diethylen glycol

Cc polyethylen glycol c khi lng phn t nh hn 450

Thit b
Dng my sc k kh trang b detector ion ha ngn la hydro
v ct thp khng r 1,5 m x 3 mm (ng knh trong, nhi
sorbitol 12%, theo khi lng, trn t diatomit 60/80 mesh
khng ra acid (Chromosorb W, hoc tng ng).
iu kin o
Cc thng s o c th thay i ty thuc vo tng thit b s
dng, nhng c th thu c mt sc ph hp trong cc
iu kin sau:
Nhit ct: 165 C; Nhit u kh vo: 260 C ; Kh
mang: nit (hoc mt kh tr ph hp); tc kh: 70
ml/pht; My ghi: - 0,5 to 1,05 mV, ton thang, 1 giy, p
ng ton thang; Kh hydro v khng kh vi tc kh vo
u t c ti u ha c nhy ln nht.
Dung dch chun
Chun b dung dch sc k tiu chun bng cch ha tan
trong nc mt lng cn chnh xc ca ethylen glycol
thng mi v diethylen glycol (nu cn th ct tinh khit li).
Khong nng ph hp l t 1 n 6 mg glycol/ml.
Chun b dung dch
Chuyn khong 4 g mu th, c cn chnh xc, vo
bnh nh mc 10 ml, nh mc n vch v lc u.
Tin hnh
Bm 2 l dung dch chun v ghi li sc k . Trong cc
iu kin cho, thi gian ra gii ca ethylen glycol v
diethyl glycol tng ng l khong 2 pht v 6,5 pht. o
chiu cao pic, v ghi li cc ga tr nh sau:
A = chiu cao, tnh theo mm, ca pic ethylen glycol;
B = khi lng, tnh theo mg, ca ethylen glycol trong 1 ml
dung dch chun;
C = chiu cao, mm, ca pic diethylen glycol;
D = khi lng, mg, ca diethylen glycol trong 1 ml dung
dch chun
Tng t, bm 2 l dung dch dung dch mu th v ghi li
sc . o chiu cao pic, E, ca ethylen glycol, v chiu cao
F ca pic diethylen glycol.
16

QCVN 4-7 : 2010/BYT

Tnh ton
Tnh phn trm ca ethylen glycol trong mu theo cng thc
sau: (E x B) / A x khi lng mu th (g).
Tnh phn trm diethylen glycol trong mu theo cng thc:
(F x D) / C x khi lng mu th (g).
Cc polyethylen glycol c khi lng phn t ln hn hoc
bng 450
Chun b mu
Ha tan 50 g mu th vo 75 ml diphenyl ether trong bnh ct
250 ml. Ct chm p sut 1-2 mm Hg v hng vo bnh 100
ml chia vch n 1 ml, cho n khi thu c 25 ml dch ct.
Thm 25 ml nc vo dch ct, lc mnh, yn mt lc
dung dch tch lp. Lm lnh trong lp diphenyl ether
ng rn v d tch loi. Lc lp nc qua giy lc vo ng
ong thy tinh 50 ml chia c nt y. Thm mt th tch
tng ng acetonitril (mi ct tinh khit li) vo dch lc.
Chun b dung dch chun
Chuyn 50 mg diethylen glycol vo bnh nh mc 25 ml, pha
long ti vch bng hn hp 1:1 ca acetonitril (mi ct tinh
khit li) trong nc, trn u.
Tin hnh
Chuyn 10 ml dung dch mu v 10 ml dung dch chun vo
2 bnh 50 ml, ring trong mi bnh cha 15 ml dung dch
ceri IV amoni nitrat (TS), trn u. o hp th quang ca
dung dch bng my o quang trong cuvet 1 cm ti bc
sng 450 nm trong vng 2 n 5 pht. o mu trng c cha
15 ml dung dch ceri IV amoni nitrat (TS) v 10 ml hn hp
1:1 ca acetonitril trong nc . hp th quang ca dung
dch mu th khng c ln hn hp th quang ca
dung dch chun.
Phng php d kin khc xc nh mono and diethylen
glycol
Dung dch th
Cn 5 g mu cn kim tra vo bnh nh mc 100 ml, ha tan
bng aceton v pha long ti vch bng aceton.
Dung dch i chiu
Cn 100 mg monoethylen glycol v 500 mg diethylen glycol
vo bnh nh mc 100 ml. Pha long bng 100 ml aceton.
Pha long 1 ml dung dch ny thnh 10 ml bng aceton.
17

QCVN 4-7 : 2010/BYT

Tin hnh
Tin hnh o sc k kh s dng :
- Ct thy tinh 1,8 m v c ng knh trong 2 mm, nhi
diatomit dng cho sc k kh, c ra sach v silan ha
(Chromosorb G.AW.DMCS 100-125 mesh l ph hp), ngm
tm trong 4 % (kl/kl) polyethylen glycol 20.000 (Carbowax 20
M l ph hp).
- Kh mang Nit, vi tc dng kh l 30 ml/pht,
- Detector ion ha ngn la
Trong trng hp cn thit, luyn ct ti 200
khong 15 gi.

C trong

iu chnh nhit ban u thu c thi gian lu thu

c ca diethylen glycol c gi tr t 14 n 16 pht. H
nhit ct xung 140 C. Bm cc dung dch vo v tng
nhit ct ln 170 C, vi tc tng nhit l 2 C/pht.
Duy tr nhit cng bm v nhit detector 250 C.
Bm 2,0 l dung dch th v 2,0 l dung dch so snh. Kim
tra lp li ca tn hiu sau 5 ln bm.
Tnh ton
o din tch cc pic thu c ca mono v diethyl glycol
trong sc ca dung dch th v dung dch so snh. Tnh
hm lng ca mono v diethylen glycol trong dung dch th
t din tch pic.

18

QCVN 4-7 : 2010/BYT

Ph lc 3
YU CU K THUT V PHNG PHP TH
I VI POLYOXYETYLEN (20) SORBITAN MONOOLEAT
1. Tn khc, ch s

Polysorbat 80;
INS 433
ADI=0-25 mg/kg th trng

2. nh ngha

Hn hp bao gm cc ester mt phn ca sorbitol v cc dn

cht mono- v dianhydrid ca n (c ch s acid di 7,5 v
hm lng nc di 0,2%) vi acid oleic thc phm v c
c vi xp x 20 mol ethylen oxyd cho 1 mol sorbitol v cc
anhydrid ca n.

M s C.A.S.

9005-65-6

Cng thc cu to

Cng thc danh ngha v thnh phn gn ng:

CH2
H
H(OC2H4)xO

O(C2H4O)wH

CH
CH

O(C2H4O)yH
CH2C(C2H4O)2OCR

3. Cm quan

Trong w + x + y + z = ~20 v RCO- l phn acid bo

25oC l dung dch snh mu vng chanh n mu h phch
c mi nh c trng

4. Chc nng

Chng to bt, Cht nh ha, cht phn tn.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, ethanol, methanol, ethyl acetat v toluen;

khng tan trong du khong v ether du ha.

Hp th hng ngoi

Ph hng ngoi ca mu th c trng cho este mt phn ca

acid bo v polyoxyethyl polyol

Phn ng mu

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

Acid bo

Phi c phn ng c trng ca acid bo.

Lin kt khng no

Phi c phn ng c trng ca lin kt khng no.

Gelatin ho

Ti nhit thng hoc thp hn, hn hp mu th trong

nc ct (60/40: v/v) to ra mt khi c.

X phng ha

100 g mu cho khong 23 g acid bo v 75 g polyol.

19

QCVN 4-7 : 2010/BYT

5.2. tinh khit
Nc

Khng c qu 3,0% (phng php Karl-Fischer)

Tro sulfat

Khng c qu 0,25%

Ch s acid

Khng c qu 2,0.

Ch s X phng ha

Khng c thp hn 45 v khng c qu 55.

Ch s Hydroxyl

Khng c thp hn 65 v khng c qu 80.

Ch

Khng c qu 2,0 mg/kg

5.3. Hm lng

Khng thp hn 65,0% v khng c qu 69,5% nhm

oxyethylen tng ng vi khng thp hn 96,5% v khng
c qu 103,5% polyoxyethylen (20) sorbitan monooleat tnh
theo ch phm khan.

6. Phng php th
6.1. nh tnh
Phn ng mu

Thm 10 ml dung dch amoni cobalt (II) thiocyanat v 5 ml

chloroform vo 5 ml dung dch mu th tan trong nc nng
5% (m/v). Lc u v tch lp; lp chloroform s c mu
xanh da tri. (Dung dch amoni cobaltothiocyanat: 37,5 g
cobalt nitrat v 150 g amoni thiocyanat ha tan v chnh th
tch n 100 ml bng nc ct - pha hng ngy trc khi
s dng).

Acid bo

Thm 5 ml dung dch natri hydroxyd (TS) vo 5 ml dung dch

mu th 5% (m/v) trong nc. un si hn hp trong vi pht,
ngui, acid ha hn hp bng acid hydrocloric long. Dung
dch rt c, do acid bo c gii phng.

Lin kt khng no

Nh git dung dch brom (TS) vo dung dch mu th (1/20).

Dung dch brom s mt mu.

Gelatin ho

Ti nhit thng hoc thp hn, hn hp mu th trong

nc ct (60/40: v/v) to thnh mt khi mm c.

6.2. tinh khit

Ch

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

nh bng k thut hp th nguyn t thch hp cho hm
lng quy 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).
20

QCVN 4-7 : 2010/BYT

6.3. nh lng
Xc nh hm lng nhm Oxyethylen (theo hng dn ti
JECFA monograph 1 - Vol.4).

21