CNG HA X HI CH NGHA VIT NAM

QCVN 3-4 : 2010/BYT

QUY CHUN K THUT QUC GIA

V CC CHT C S DNG B SUNG CALCI
VO THC PHM
National technical regulation
on substances may be added for calcium fortification in food

H NI - 2010

Li ni u
QCVN 3-4:2010/BYT do Ban son tho quy chun k
thut quc gia v Thc phm b sung vi cht dinh dng
bin son, Cc An ton v sinh thc phm trnh duyt v
c ban hnh theo Thng t s 17/2010/TT-BYT
ngy 20 thng 5 nm 2010 ca B trng B Y t.

QUY CHUN K THUT QUC GIA

V CC CHT C S DNG B SUNG CALCI
VO THC PHM

National technical regulation

on substances may be added for calcium fortification in food

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 c s dng vi mc
ch b sung calci vo 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 b sung calci vo 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 b sung calci vo thc phm: l cc cht c ch ng cho vo
thc phm vi mc ch b sung calci.
3.2. JECFA monograph 1 - Vol. 4: JECFA monographs 1 - Combined
compendium - 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 i vi 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 b sung calci vo
thc phm 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 Calci

carbonat.

1.2.

Ph lc 2:

Yu cu k thut v phng php th i vi Calci

gluconat.

1.3.

Ph lc 3:

Yu cu k thut v phng php th i vi Calci

dihydro phosphat.

1.4.

Ph lc 4:

Yu cu k thut v phng php th i vi Calci

dihydro diphosphat.

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;
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 Tt c cc cht b sung calci vo thc phm 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 b sung calci vo thc phm
Vic kim tra cht lng, v sinh an ton i vi cc cht b sung calci vo
thc phm phi c 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 yu cu 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 b sung calci vo thc phm 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 CALCI CARBONAT
1. Tn khc, ch s

Calcium carbonate, phn

INS 170i
ADI Khng gii hn

2. nh ngha
Tn ha hc

Calci carbonat; mui Calci ca acid carbonic

M s C.A.S.

471-43-1

Cng thc ha hc

CaCO3

Khi lng phn t

100,09

3. Cm quan

Bt tinh th nh mu trng, khng mi

4. Chc nng

- Cht dinh dng b sung: b sung calci

- Ph gia thc phm: chng ng vn

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc v ethanol.

Calci

Phi c phn ng c trng ca calci.

Carbonat

Phi c phn ng c trng ca carbonat.

5.2. tinh khit

Gim khi lng khi sy

Khng c qu 2,0% (sy 200 oC trong 4 gi).

Cc cht khng tan trong

acid

Khng qu 0,2%.

Bari

Khng c qu 0,03%.

Florid

Khng c qu 50,0 mg/kg.

Kim t do

Khng c qu 0,05%.

Mui magnesi v mui

kim

Khng c qu 1,0%.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 3,0 mg/kg.

5.3. Hm lng

Khng c thp hn 98,0% sau khi sy kh.

6. Phng php th
6.1. tinh khit
Cc cht khng tan trong Cn 5 g (chnh xc n mg) mu th, cho phn tn vo
25 ml nc. Thm cn thn 25 ml dung dch acid
acid
hydrocloric (1 trong 2), va thm va khuy, thm nc
v nh mc n 200 ml. un si hn hp, y kn bnh
ng, ngm trong b cch thu trong 1 gi, ngui v
lc. Ra kt ta thu c bng nc cho n khi dch
ra khng cn clorid khi th vi dung dch bc nitrat
(TS). Nung kt ta, ngui, cn v tnh kt qu (%).
Khi lng cn thu c khng c qu 10 mg.
Bari

Cn 1 g (chnh xc n mg) mu th, trn ln vi 10 ml

nc. Thm 15 ml dung dch acid hydrocloric long (TS),
pha long tip n 30 ml bng nc v lc. Ly 20 ml
dch lc, thm 2 g natri acetat, 1 ml dung dch acid acetic
long (TS), 0,5 ml dung dch kali cromat (TS) v yn
trong 15 pht. Dung dch thu c khng c c hn
dung dch kim chng c cha 1 mg bari / ml. chun
b dung dch kim chng, thm 20 ml nc ct vo 0,3
ml dung dch chun bari (1,799 g bari clorid / 1 l), sau
thm 2 g natri acetat, 1 ml dung dch acid acetic long
(TS), 0,5 ml dung dch kali cromat (TS).

Florid

- Mu th: 1 g (chnh xc n mg).

- Th theo JECFA monograph 1 - Vol. 4 (chuyn lun
th gii hn florid - phng php III).

Kim t do

Cn 3 g mu th, cho vo 30 ml nc mi c un si
v ngui, khuy trong 3 pht v lc. Thm 2 git dung
dch phenolphtalein (TS) vo 20 ml dch lc. Dung dch
chuyn mu v b mt mu khi cho thm 0,2 ml acid
hydrocloric 0,1 N.

Mui magnesi v mui

kim

Trn 1 g mu th vi 40 ml nc, thm cn thn 5 ml

acid hydrocloric, lc u hn hp v un si trong 1
pht. Thm tht nhanh 40 ml dung dch acid oxalic (TS),
khuy mnh cho n khi to thnh kt ta. Thm ngay 2
git dung dch methyl (TS), sau thm tng git
dung dch amoniac (TS), cho n khi dung dch bt u
c tnh kim, ngui dung dch. Chuyn hn hp vo
ng ong 100 ml, pha long bng nc n 100 ml,
yn trong 4 gi hoc qua m, sau gn ly phn
dung dch trong pha trn lc qua giy lc kh. Ly 50
ml dch lc vo mt a platin, thm 0,5 ml acid sulfuric,
c cn hn hp trn bp cch thy cho n khi cn mt
t dung dch. Cn thn c phn dung dch cn li trn
ngn la n kh v tip tc un nng cho n khi cc
mui amoni b ph hy v bay hi hon ton. Cui cng,
nung cn cn li n khi lng khng i. ngui,
cn v tnh kt qu. (Khi lng cn thu c khng
c qu 5 mg).

Arsen

Th theo JECFA monograph 1 - Vol. 4 (chuyn lun th

gii hn arsen - phng php II).

Ch

Th theo JECFA monograph 1 - Vol. 4. Xc nh bng

k thut hp th nguyn t thch hp vi hm lng qui
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 200 mg (chnh xc n 0,1 mg) mu th c

sy kh, chuyn vo cc 400 ml, thm 10 ml nc v
khuy to thnh mt hn hp st. y cc bng mt
mt knh ng h v dng pipet (pipet c t gia
mp cc v g ca knh ng h) thm 2 ml dung dch
acid hydrocloric long (TS). Lc cc ha tan mu th.
Trng ra thnh cc, mt ngoi ca pipet v mt knh
ng h, pha long n 100 ml bng nc ct. Trong khi
khuy, (tt nht l dng my khuy t) thm 30 ml
dinatri ethylendiamintetraacetat 0,05 M, sau thm 15
ml dung dch natri hydroxyd (TS) v 300 mg ch th xanh
hydroxynaphthol v tip tc chun n khi dung dch
c mu xanh da tri.
Mi ml dinatri ethylendiamintetraacetat 0,05 M tng
ng vi 5,004 mg CaCO3.

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

Calcium gluconate
INS 578
ADI Khng gii hn

2. nh ngha
Tn ha hc

Calci di-D-gluconat monohydrat

M s C.A.S.

299-28-5

Cng thc phn t

C12H22CaO14.H2O

Cng thc cu to

OH OH H

OH

OH

HOH2C

COO

Ca

2+

Khi lng phn t

448,39

3. Cm quan

Dng ht hoc bt tinh th mu trng, khng mi, bn

trong khng kh.

4. Chc nng

- Cht dinh dng b sung: b sung calci.

- Ph gia thc phm: iu chnh acid, lm rn chc,
to phc kim loi.

5. Yu cu k thut
5.1. nh tnh
tan

Tan trong nc, khng tan trong ethanol.

Calci

Phi c phn ng trng ca calci.

Gluconat

Phi c phn ng trng ca gluconat.

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 2,0%. (sy ti 105 oC, trong 16 gi).

Cc hp cht kh

Khng c qu 1,0% tnh theo D-glucose.

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng

Khng thp hn 98,0% v khng c qu 102,0% tnh

theo ch phm lm kh.

6. Phng php th
6.1. tinh khit
Cc hp cht kh

Th theo JECFA monograph 1 - Vol. 4 (chuyn lun xc

nh cc hp cht kh - phng php I).

Ch

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

6.2. nh lng

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

trong 5 ml dung dch acid hydrocloric long. Thm 50 ml
nc, 25 ml dung dch natri hydroxyd (TS) v khong
0,1 g acid 2-hydroxy-1-(2'-hydroxy-4'sulfo-1'-naphtylazo)3-naphthoic. Chun ngay vi dung dch EDTA 0,05 M
n khi mu ca dung dch chuyn t mu sang mu
xanh.
Mi ml dung dch EDTA 0,05 M tng ng vi 22,42
mg C12H22CaO14.H2O.

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

Calcium dihydrogen phosphate; Monobasic calcium

phosphate; Monocalcium orthophosphate, Monocalcium
phosphate; Calcium biphosphate; Acid calcium phosphate;
INS 341i
MTDI=70mg/kg th trng tnh theo Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Calci dihydrogen phosphat

M s C.A.S.

Dng khan: 7758-23-8

Dng monohydrat: 10031-30-8

Cng thc ha hc

Dng khan: Ca(H2PO4)2

Dng monohydrat: Ca(H2PO4)2.H2O

Khi lng phn t

Dng khan: 234,05

Dng monohydrat: 252,07

3. Cm quan

Dng tinh th hoc ht mu trng, d ht m hoc dng ht

mn.

4. Chc nng

- Cht dinh dng: B sung calci.

- Ph gia thc phm: m, cht lm rn chc, cht to
phc kim loi, bt n, cht iu ho dng nho, cht to
kt cu, thc phm cho men.

5. Yu cu k thut
5.1. nh tnh
tan

t tan trong nc, khng tan trong ethanol.

Calci

Phi c phn ng c trng ca calci.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit

Gim khi lng khi sy
kh

Dng monohydrat: Khng c qu 1,0% (60 oC trong 3

gi).

o
Gim khi lng khi nung Dng khan: gia 14,0 v 15,5% (800 C trong 30 pht).

Florid

Khng c qu 50,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg.

5.3. Hm lng

Dng khan: Khng c thp hn 16,8% v khng c

qu 18,3% tnh theo Ca.
Dng monohydrat: Khng c thp hn 15,9% v khng
c qu 17,7% tnh theo Ca.

6. Phng php th
6.1. tinh khit
Florid

Th theo JECFA monograph 1 - Vol. 4. Dng khan: tin

hnh xc nh theo Phng php II; Dng monohydrat: tin
hnh xc nh theo phng php IV.

Arsen

Th theo JECFA monograph 1 - Vol. 4 , phng php II.

Ch

Th theo 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.

6.2. nh lng

Cn mu th (chnh xc n mg) khi lng tng ng

vi khong 475 mg mui khan, ho tan trong 10 ml dung
dch acid hydrocloric (TS). Thm vi git dung dch da cam
methyl (TS) v un si trong 5 pht, duy tr lin tc th tch
v pH ca dung dch trong qu trnh un si bng cch cho
thm dung dch acid hydrocloric hoc nc ct nu cn
thit. Thm 2 git dung dch methyl (TS) v 30 ml dung
dch amoni oxalat (TS), sau thm tng git (va thm
va khuy) hn hp ng th tch dung dch amoniac 6 N
v nc n khi dung dch bt u c mu hng.
hn hp trong b cch thy nc si trong 30 pht, lm
ngui ti nhit phng v ch kt ta lng xung, lc b
phn dch qua phu lc thy tinh xp, ht chn khng nh
nu cn. Ra ta trong cc vi khong 30 ml dung dch ra
lnh (di 20 oC), c pha bng cch ly 10 ml dung dch
amoni oxalat (TS) pha long vi nc n 1000 ml.
kt tu lng xung, gn phn dch pha trn qua phu lc,
lm nh vy 3 ln. Dng dch ra, chuyn ton b phn kt
ta vo phu lc, ra cc v thnh phu bng nc lnh
(di 20 oC) 2 ln, mi ln vi 10 ml. t phu lc thy tinh
xp ln trn cc, thm 100 ml nc v 50 ml dung dch
acid sulfuric long lnh (1 trong 6). Dng buret cho 35 ml
kali permanganat 0,1 N vo dung dch. Khuy u n khi
dung dch mt mu. un nng n khong 70 oC v chun
tip bng dung dch kali permanganat 0,1 N.
Mi ml dung dch kali permanganat 0,1 N tng ng vi
2,004 mg Ca.

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

Monocalcium dihydrogen pyrophosphate

INS 450vii
MTDI=70mg/kg th trng tnh cho Phospho t cc ngun
thc phm

2. nh ngha
Tn ha hc

Monocalci dihydro di-phosphat

M s C.A.S.

14866-19-4

Cng thc ha hc

CaH2P2O7

Khi lng phn t

215,97

3. Cm quan

Tinh th trng hoc bt trng.

4. Chc nng

- Cht dinh dng: B sung calci

- Ph gia thc phm: cht n nh, bt ni, cht nh ha.

5. Yu cu k thut
5.1. nh tnh
Calci

Phi c phn ng c trng ca calci.

Phosphat

Phi c phn ng c trng ca phosphat.

5.2. tinh khit

Gim khi lng khi sy
kh

Khng c qu 1,0% (105 oC trong 4 gi).

Cc cht khng tan trong

acid

Khng c qu 0,4%.

Florid

Khng c qu 30,0 mg/kg.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 4,0 mg/kg.

5.3. Hm lng

Khng c qu 64,0% quy ra P2O5 tnh theo ch phm

kh.

6. Phng php th
6.1. tinh khit
Florid

Th JECFA monograph 1 - Vol.4, phng php III; s

dng c mu v th tch dung dch chun xy dng
ng chun ph hp.

Arsen

Th theo JECFA monograph 1 - Vol. 4, phng php II.

Ch

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

6.2. nh lng

Cn khong 200 mg (chnh xc n mg) mu th, ha tan

trong 25 ml nc v 10 ml dung dch acid nitric long (TS),
un si trong 30 pht. Lc nu cn v ra kt ta, sau
ha tan ta bng cch thm 1 ml dung dch acid nitric long
(TS). un nng n 50 oC, thm 75 ml dung dch amoni
molybdat (TS) v gi 50 oC trong 30 pht, thnh thong
khuy. yn 16 gi hoc qua m nhit d phng. Gn
phn dch pha trn qua giy lc, ra ta bng nc 1 hoc
2 ln, mi ln 30-40 ml, gn b dch ra ln giy lc nu
trn, Cho kt ta vo giy lc va gn dch ra, ra ton
b bng dung dch kali nitrat (1/100) n khi dch ra khng
cn acid khi th vi qu tm. Cho giy lc cha ta vo
bnh kt ta, thm 50ml dung dch natri hydroxyd 1N, lc
n khi ta tan hon ton, thm 3 git dung dch
phenolphtalein (TS) v chun lng natri hydroxyd d
bng acid sulfuric 1N.
Mi ml dung dch natri hydroxyd 1N tng ng vi 3,088
mg P2O5.