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coeus.vn a12.CHẤT-ỔN-ĐINH
coeus.vn a12.CHẤT-ỔN-ĐINH
QCVN 4 13 : 2010/BYT
H NI - 2010
QCVN 4 - 13 : 2010/BYT
Li ni u
QCVN 4-13:2010/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 44/2010/TT-BYT ngy 22 thng 12
nm 2010 ca B trng B Y t.
QCVN 4 - 13 : 2010/BYT
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 n nh 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 n nh 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 n nh: l ph gia thc phm c s dng vi mc ch duy tr s
phn tn ca hai hay nhiu thnh phn nhm to nn s ng nht cho sn 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 MTDI (Maximum tolerable daily intake): Lng n vo hng ngy ti a chu
ng c.
3.7. 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 n nh c quy
nh ti cc ph lc ban hnh km theo Quy chun ny nh sau:
3
QCVN 4 - 13 : 2010/BYT
1.1.
Ph lc 1:
1.2.
Ph lc 2:
1.3.
Ph lc 3:
1.4.
Ph lc 4:
1.5.
Ph lc 5:
1.6.
Ph lc 6:
1.7.
Ph lc 7:
1.8.
Ph lc 8:
1.9
Ph lc 9 :
1.10
Ph
10 :
lc
1.11
Ph
11 :
lc
1.12
Ph
12 :
lc
QCVN 4 - 13 : 2010/BYT
III. YU CU QUN L
1. Cng b hp quy
1.1. Cc cht n nh 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 n nh
Vic kim tra cht lng, v sinh an ton i vi cc cht n nh 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 n nh 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 - 13 : 2010/BYT
Ph lc 1
YU CU K THUT V PHNG PHP TH
I VI POLYVINYLPYROLIDON
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
9003-39-8
(C6H9NO)n
Cng thc cu to
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
To kt ta
Khng c qu 5%.
nht tng i
QCVN 4 - 13 : 2010/BYT
Tro ton phn
Khng c qu 0,02%.
Aldehyd
Hm lng monomer
Hydrazin
Ch
5.3. Hm lng Nitrogen
6. Phng php th
6.1 nh tnh
To kt ta
nht tng i
QCVN 4 - 13 : 2010/BYT
khi dung dch mu th v pipet trong ni cch thy
lm m trong 10 pht, ly dung dch bng cch ht ln rt
nh qua ng mao qun ti khi to thnh mt khum ca cht
lng t 3 ti 4 mm trn vch. Gim t t chn khng, v
khi mt khum ca cht lng t ti vch mc trn, bt u
tnh thi gian chy qua mao qun. Ghi chnh xc thi gian
khi mt khum ca cht lng t n vch mc di, v tnh
thi gian chy chnh xc ti 0,1 giy. Lp li php th ny
t nht 3 ln. Gi tr thu c phi khng lch qu 0,3 giy;
nu khng, xc nh li vi 10 ml dung dch mu th khc
sau khi ra ng o nht bng dung dch ra acid
sulfuric-dicromat. Tnh thi gian chy trung bnh ca dung
dch mu th, v sau , o thi gian chy trung bnh theo
cch tng t ca 10 ml nc lc trn cng ng o
nht. Tnh nht tng i bng cch chia thi gian chy
trung bnh ca dung dch mu th cho thi gian chy trung
bnh ca nc.
Tro ton phn
Aldehyd
Cn 10 g mu th.
Hm lng monomer
Hydrazin
QCVN 4 - 13 : 2010/BYT
ngui, thm 2,0 ml toluen, y np ng ly tm, lc mnh
trong 2 pht, v ly tm. Trn bn mng sc k thch hp,
c ph lp hn hp silica gel dimethylsilan ha dy 0,25
mm, chm 10 L lp toluen trong pha trn trong ng ly tm
v 10 L dung dch chun salicylaldazin trong toluen cha
9,38 g/ml. vt chm kh, v khai trin trong h dung
mi methanol v nc (2:1) ti khi tuyn dung mi i c
ba phn t chiu di ca bn mng. Ly bn mng ra khi
bnh trin khai, nh du tuyn dung mi, v cho dung
mi bay hi. Pht hin vt trn bn mng di nh sng t
ngoi ti bc sng 365 nm: vt salicylaldazin pht quang
c gi tr Rf khong 0,3, v hunh quang ca bt k vt
salicylaldazin ca mu th khng c m hn vt thu
c ca dung dch chun salicylaldazin (hydrazin 1 ppm).
Dung dch chun Salicylaldazin: Ha tan 300 mg hydrazin
sulfat trong 5 ml dung dch salicylaldehyd 20% (tt/tt) trong
alcol isopropyl mi pha, lc u, v yn ti khi xut hin
ta mu vng. Chit hn hp hai ln, mi ln vi 15 ml
methylen clorid. Gp dch chit methylen clorid, v lm kh
trn natri sulfat khan. Gn dung dch methylen clorid, v c
ti kh. Kt tinh li cn salicylaldazin t hn hp toluen v
methanol m (60:40) bng cch lm lnh; lc v lm kh
tinh th trong chn khng. Tinh th c khong chy t
213oC ti 214oC.
Ch
6.3. nh lng
QCVN 4 - 13 : 2010/BYT
Ph lc 2
YU CU K THUT V PHNG PHP TH I VI CALCI LACTAT
1. Tn khc, ch s
INS 327
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
814-80-2
C6H10CaO6.xH2O (x = 0 - 5)
Cng thc cu to
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Lactat
Calci
Khng c qu 30%
pH
acid
Mui magnesi v cc
mui kim
Khng c qu 1 %
Florid
Khng c qu 30 mg/kg
Ch
Khng c qu 2 mg/kg
5.3. Hm lng
C6H10CaO6
10
QCVN 4 - 13 : 2010/BYT
6. Phng php th
6.1 nh tnh
Lactat
Calci
acid
Mui magnesi v cc
mui kim
Florid
Ch
6.3. nh lng
11
QCVN 4 - 13 : 2010/BYT
Ph lc 3
YU CU K THUT V PHNG PHP TH
I VI KALI DIHYDROCITRAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
866-83-1
C6H7KO7
Cng thc cu to
230,21
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Citrat
Kali
Oxalat
Khng c qu 0,04%.
Ch
5.3. Hm lng
C6H7NaO7
6. Phng php th
6.1. nh tnh
Citrat
QCVN 4 - 13 : 2010/BYT
Kali
6.3. nh lng
13
QCVN 4 - 13 : 2010/BYT
Ph lc 4
d
i
2. nh ngha
Tn ha hc
M s C.A.S.
7558-79-4
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Phosphat
Orthophosphat
QCVN 4 - 13 : 2010/BYT
Cc cht khng tan trong
nc
Khng c qu 0,2%.
Florid
Arsen
Ch
Phosphat
Orthophosphat
Arsen
Ch
6.3. nh lng
15
QCVN 4 - 13 : 2010/BYT
Ph lc 5
YU CU K THUT V PHNG PHP TH
I VI DIKALI HYDROGEN PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
7758-11-4
Cng thc ha hc
K2HPO4
174,18
3. M t
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Kali
Phosphat
Orthophosphat
Khng c qu 0,2%.
Fluorid
Arsen
Ch
16
QCVN 4 - 13 : 2010/BYT
5.3. Hm lng K2HPO4
6. Phng php th
6.1. nh tnh
Kali
Phosphat
Orthophosphat
17
QCVN 4 - 13 : 2010/BYT
Arsen
Ch
6.3. nh lng
Cn khong 6,5 g (chnh xc n mg ) mu th, c
lm kh trc, cho vo cc 250 ml. Thm 50 ml dung dch
acid hydrocloric 1 N v 50 ml nc ct, khuy u n khi
mu tan ht. Cho in cc ca pH k thch hp vo dung
dch v chun lng acid d bng dung dch natri
hydroxyd 1 N n im un ti pH~4, ghi li th tch c
trn buret, tnh th tch (A) acid hydrocloric 1 N mu th
s dng. Tip tc chun bng dung dch natri hydroxyd
1 N n im un ti pH~8,8; ghi li th tch trn buret v
tnh th tch dung dch (B) natri hydroxyd 1N s dng
chun gia 2 im un (pH~4 n pH~8,8).
Nu (A) (B), mi ml acid hydrocloric 1 N trong th tch (A)
tng ng vi 174,2 mg K2HPO4.
Nu (A)>(B), mi ml natri hydroxyd 1 N trong hiu th tch
2(B)-(A) tng ng vi 174,2 mg K2HPO4.
18
QCVN 4 - 13 : 2010/BYT
Ph lc 6
YU CU K THUT V PHNG PHP TH
I VI TRICALCI PHOSPHAT
1. Tn khc, ch s
2. nh ngha
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kh tan trong nc, khng tan trong ethanol, tan trong acid
hydrocloric long v acid nitric long.
Calci
Phosphat
Fluorid
Khng c qu 50 mg/kg.
Ch
Khng c qu 4 mg/kg.
5.3. Hm lng
Ca3(PO4)2
6. Phng php th
6.1. nh tnh
Calci
Phosphat
QCVN 4 - 13 : 2010/BYT
hoc III
Ch
6.3. nh lng
Cn 200 mg (chnh xc n 0,1 mg) mu th, ho tan trong
hn hp gm 10ml dung dch acid nitric long (TS) v 25 ml
nc. Lc nu cn, ra kt ta, thm dung dch amoniac
(TS) vo dch lc va to kt ta nh. Sau ha
tan kt ta bng cch thm 1 ml dung dch acid nitric long
(TS). Chnh nhit v 50o, thm 75 ml dung dch amoni
molybdat (TS). Gi nhit ti 50o trong 30 pht, thnh
thong khuy. Gn ra ta 1 hoc hai ln, mi ln vi 30
n 40 ml nc. Chuyn ta sang mt phu lc v ra ta
bng dung dch kali nitrat (1/100) n khi dch ra khng
cn acid khi th bng giy qu. Chuyn ta, giy lc vo
mt bnh kt ta, thm 40 ml natri hydroxyd 1N, lc u n
khi kt ta tan han ton, thm 3 git dung dch
phenolphtalein (TS), sau chun kim d bng acid
sulfuric 1N.
Mi ml dung dch natri hydroxyd 1N tng ng vi 6,743
mg Ca3(PO4)2.
20
QCVN 4 - 13 : 2010/BYT
Ph lc 7
YU CU K THUT V PHNG PHP TH
I VI AMONI POLYPHOSPHAT
1. Tn khc, ch s
INS 452v
MTDI = 70 mg/kg th trng, tnh theo phospho t cc ngun
thc phm
2. nh ngha
Tn ha hc
Amoni polyphosphat
M s C.A.S.
6833-79-9
Cng thc ho hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Amoni
Phosphat
Fluorid
Arsen
Ch
5.3. Hm lng
6. Phng php th
6.1 nh tnh
Amoni
Phosphat
QCVN 4 - 13 : 2010/BYT
Phosphat mch vng
Fluorid
Arsen
Ch
6.3 nh lng
Tin hnh nh ch dn Xc nh photphat tnh theo P2O5 ,
Phng php I, Vol. 4.
22
QCVN 4 - 13 : 2010/BYT
Ph lc 8
YU CU K THUT V PHNG PHP TH
I VI NATRI HYDROGEN CARBONAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
144-55-8
Cng thc ha hc
NaHCO3
84,01
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Natri
Carbonat
Mui amoni
Ch
6. Phng php th
6.1. nh tnh
Natri
Carbonat
23
QCVN 4 - 13 : 2010/BYT
6.2. tinh khit
Cc cht khng tan trong
nc
Mui amoni
Ch
6.3. nh lng
Cn 3 g (chnh xc n mg) mu th sy kh, ha tan
trong nc, thm ch th l dung dch da cam methyl (TS)
v chun bng acid sunfuric 1 N.
Mi ml acid sulfuric 1 N tng ng vi 84,01 mg
NaHCO3.
24
QCVN 4 - 13 : 2010/BYT
Ph lc 9
YU CU K THUT V PHNG PHP TH
I VI KALI CARBONAT
1. Tn khc, ch s
INS 501(i)
ADI khng gii hn
2. nh ngha
Tn ha hc
M s C.A.S.
584-08-7
Cng thc ha hc
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Kali
Carbonat
Ch
6. Phng php th
6.1. nh tnh
Kali
Carbonat
QCVN 4 - 13 : 2010/BYT
cc phng php phn tch cng c.
6.3. nh lng
Cn 1 g (chnh xc n mg) mu th sy kh, ha tan
cn thn trong 50 ml acid sulfuric 1 N, thm ch th l dung
dch da cam methyl (TS) v chun acid d bng dung
dch natri hydroxyd 1N.
Mi ml dung dch acid sulfuric 1 N tng ng vi 69,11
mg K2CO3.
26
QCVN 4 - 13 : 2010/BYT
Ph lc 10
YU CU K THUT V PHNG PHP TH
I VI AMONI HYDROGEN CARBONAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
Amoni hydrogcarbonat
M s C.A.S.
1066-33-7
Cng thc ha hc
CH5NO3
Cng thc cu to
NH4HCO3
79,06
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Carbonat
Amoni
Nhit
Clorid
Sulfat
Ch
6. Phng php th
27
QCVN 4 - 13 : 2010/BYT
6.1. nh tnh
Carbonat
Amoni
6.3. nh lng
Ly 10ml nc vo mt cc cn. Tin hnh xc nh b
(cc v nc). Thm vo cc 2g mu th (cn chnh xc
n mg). Chuyn ton b hn hp trong cc vo mt bnh
nn 250ml. Thm t t, va thm va lc 50ml acid
sulfuric 1N. Sau khi dung dch phn ng xong, trng ra
thnh bnh, thm ch th l dung dch da cam methyl (TS) v
chun acid d bng dung dch natri hydroxyd 1N.
Mi ml acid sulfuric 1N tng ng vi 79,06 mg
NH4HCO3.
28
QCVN 4 - 13 : 2010/BYT
Ph lc 11
YU CU K THUT V PHNG PHP TH
I VI KALI CLORID
1. Tn khc, ch s
Sylvite; Sylvine
INS 508
ADI khng gii hn
2. nh ngha
Tn ha hc
Kali clorid
M s C.A.S.
7447-40-7
Cng thc ha hc
KCl
74,56
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
Clorid
Kali
29
QCVN 4 - 13 : 2010/BYT
Iodid hoc bromid
Natri
Ch
6. Phng php th
6.1. nh tnh
Clorid
Kali
Natri
Ch
6.3. nh lng
Cn khong 250 mg (chnh xc n mg) mu th lm
kh ha tan trong 50 ml nc trong mt bnh thy tinh nt
mi. Thm 50 ml dung dch bc nitrat 0,1 N, 3 ml acid nitric
v 5 ml nitrobenzen, va thm va lc mnh, thm 2 ml st
(III) amoni sulfat (TS). Chun lng bc nitrat d vi
dung dch amoni thiocyanat 0,1 N.
Mi ml dung dch bc nitrat 0,1 N tng ng vi 7,456
mg KCl.
30
QCVN 4 - 13 : 2010/BYT
Ph lc 12
YU CU K THUT V PHNG PHP TH
I VI KALI DIHYDROGEN PHOSPHAT
1. Tn khc, ch s
2. nh ngha
Tn ha hc
M s C.A.S.
7778-77-0
Cng thc ha hc
KH2PO4
136,09
3. Cm quan
4. Chc nng
5. Yu cu k thut
5.1. nh tnh
tan
pH
Kali
Phosphat
Orthophosphat
Khng c qu 0,2%.
Florid
Arsen
Ch
QCVN 4 - 13 : 2010/BYT
6. Phng php th
6.1. nh tnh
Kali
Phosphat
Orthophosphat
Arsen
Ch
QCVN 4 - 13 : 2010/BYT
- Xc nh bng k thut quang ph 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.
6.3. nh lng
Cn khong 5,0 g (chnh xc n mg) mu th c
lm kh trc, cho vo cc 250 ml. Thm 100 ml nc ct
v 5 ml dung dch acid hydrocloric 1 N, khuy u n khi
mu tan ht. Cho in cc ca pH k thch hp vo dung
dch v chun t t (khuy u lin tc) lng acid d
bng dung dch natri hydroxyd 1 N, n im un ti pH~4.
Ghi li th tch c trn buret, tnh th tch (A) acid
hydrocloric 1 N s dng (nu cn). Tip tc chun
bng dung dch natri hydroxyd 1 N n im un ti
pH~8,8; ghi li th tch trn buret v tnh th tch dung dch
(B) natri hydroxyd 1N tiu tn chun gia 2 im
un (pH~4 n pH~8,8).
Mi ml natri hydroxyd 1 N ca hiu th tch (B)-(A) tng
ng vi 136,1 mg KH2PO4.
33