CNG HO X HI CH NGHA VIT NAM

QCVN 4 - 16: 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT N
National technical regulation on Food Additive Bulking agents

H NI - 2010

QCVN 4 - 16: 2010/BYT

Li ni u
QCVN 4-16:2010/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 - 16: 2010/BYT

QUY CHUN K THUT QUC GIA

V PH GIA THC PHM - CHT N
National technical regulation on Food Additive Bulking agents

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 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 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: l ph gia thc phm c b sung vo thnh phn chnh ca
thc phm vi gi tr nng lng khng ng k.
3.2. JECFA monograph 1 - Vol. 4 (JECFA monographs 1 - Combined
compendium of food additive 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 - 16: 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 n 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 celulose vi

tinh th

1.2.

Ph lc 2:

Yu cu k thut v phng php th i vi sp

carnauba

1.3.

Ph lc 3:

Yu cu k thut v phng php th i vi natri

alginat

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 c gi tr 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 n 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
Vic kim tra cht lng, v sinh an ton i vi cc cht n 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.
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QCVN 4 - 16: 2010/BYT

2. T chc, c nhn ch c nhp khu, xut khu, sn xut, bun bn v s dng
cc cht n 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 - 16: 2010/BYT

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

Mycrocrystalline cellulose; Cellulose gel;

INS 460
ADI khng gii hn.

2. nh ngha

Celulose tinh khit, c ct mch mt phn bng cch x

l alpha-celulose, thu c nh mt khi bt nho t cc
nguyn liu thc vt dng si x l vi cc acid v c.
polyme ha thng nh hn 400. Khng qu 10% tiu
phn c ng knh nh hn 5 m.

Tn ha hc

Celulose

M s C.A.S.

9004-34-6

Cng thc ha hc

(C6H10O5)n

3. Cm quan

Bt tinh th trn chy, mn, mu trng hoc gn nh trng,

khng mi.

4. Chc nng

Cht n, cht nh ha, cht n nh, cht chng ng

vn, tc nhn phn tn.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, ethanol, ether v cc acid v c

long. t tan trong dung dch natri hydroxyd.

Hp th hng ngoi

Ph hp th hng ngoi ca mu th phn tn trong kali

bromid phi tng ng vi ph hng ngoi di y.

To huyn ph

Phi c phn ng to huyn ph c trng

5.2. tinh khit

Gim khi lng khi lm
kh

Khng c qu 7,0 %. (sy ti 105 C, trong 3 gi).

pH

5,0 - 7,5

Cc cht tan trong nc

Tro sulfat

Khng c qu 0,24 %.

Tinh bt

Khng c qu 0,05 %.
Khng pht hin.

QCVN 4 - 16: 2010/BYT

Ch

Khng c qu 2,0 mg/kg.

5.3. Hm lng

Khng thp hn 97% carbohydrat, tnh theo celulose trn

ch phm kh.

6. Phng php th
6.1. nh tnh
To huyn ph

Trn 30 g mu th vi 270 ml nc trong my trn tc

cao (18.000 vng/pht) trong 5 pht. Chuyn 100 ml hn
hp vo ng ong chia dung tch 100 ml, yn trong 3
gi. Thu c mt huyn ph trng, c, khng c bt,
huyn ph ny sau phn lp .

6.2. tinh khit

pH

Lc 5 g mu th vi 40 ml nc trong 20 pht v em ly
tm. Xc nh pH ca phn dung dch pha trn.

Cc cht tan trong nc

Lc 5 g mu th vi khong 80 ml nc trong 10 pht, lc

qua giy lc Whatman No.42 hoc giy lc tng ung,
thu dch lc vo bnh cn b, ra phn cn li trn giy
lc bng 20 ml nc v un cch thy n kh. Sy kh
nhit 105 C trong 1 gi, lm ngui, cn v tnh % khi
lng.

Tro sulfat

Th theo JECFA monograph 1 - Vol.4 - Phng php 1,

(cn 10 g mu).

Tinh bt

Ch

Thm vi git dung dch iod (TS) vo 20 ml huyn ph thu

c t php th nh tnh tinh bt, trn u. Khng c
php xut hin mu tm xanh hoc mu xanh.
- Th theo JECFA monograph 1 - Vol.4.
- 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 125 mg (chnh xc n mg) mu th, chuyn
vo bnh nn 300 ml bng khong 25 ml nc. Thm 50,0
ml kali dicromat 0,5 N vo v trn u. Cn thn thm 100
ml acid sulfuric v un n si. Ly dung dch ra, nhit
phng trong 15 pht v lm mt bng cch ngm trong
b iu nhit. Chuyn dung dch thu c vo bnh nh
mc 250 ml. Ra bnh nn bng nc ct, gp dch ra
vo bnh nh mc v pha long gn ti vch bng nc.
i nhit ca bnh nh mc t ti nhit phng
(25 C), sau nh mc ti vch bng nc v lc u.
Chun 50 ml dung dch thu c vi dung dch st (II)
amoni sulfat 0,1N, s dng 2 n 3 git dung dch orthophenanthrolin (TS) lm ch th v ghi li th tch s dng
7

QCVN 4 - 16: 2010/BYT

(S) ml. Tin lm mu trng song song v ghi li th tch
dung dch st (II) amoni sulfat tiu tn (B) ml. Tnh phn
trm celulose trong mu th theo cng thc sau:

Ph hng ngoi

trong :
W l khi lng mu th, mg, c hiu chnh khi
lng sau khi lm kh.
Celulose vi tinh th

QCVN 4 - 16: 2010/BYT

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

INS 903
ADI = 0-7 mg/kg

2. nh ngha

Sp tinh luyn thu c t l ca cy c nhit i Brazil

Copernicia cerifera (Arruda) Mart. [syn. C. purnifera (Muell.)];
l hn hp ca mt s hp cht hoias hc, ch yu l cc
ester, v d nh:
- Cc ester mch thng (Ester gia cc acid mch thng c
mch carbon chn t C24 n C28 v cc ru mch thng
c mch carbon chn t C30 n C34).
- Cc ester alpha-hydroxy (Ester gia cc hydroxyl acid
mch thng c mch carbon chn t C22 n C28, cc acid
mch thng c mch carbon chn t C24 n C28, v cc
ru n chc mch thng c mch carbon chn t C24 n
C34 v ru diol mch thng c mch carbon chn t C24
n C34 ).
- Cc Diester cinnamic aliphatic (Ester gia acid p-methoxy
cinnamic v cc ru diol mch thng c mch carbon chn
t C24 n C34 ).
Ngoi ra ch phm cng cha cc acid t do (cc acid mch
thng c mch carbon chn t C22 n C28), cc ru t do
(cc ru mch thng c mch carbon chn t C30 n C34),
cc hydrocarbon (mch thng c mch carbon l t C27 n
C31) v nha.

M s C.A.S.

8015-86-9

3. Cm quan

Dng rn, cng, rn mu vng nht n nu sng, c vt

nt trong.

4. Chc nng

Cht lm bng, cht n, cht iu chnh acid, cht

mang.

5. Yu cu k thut
5.1. nh tnh
tan

Khng tan trong nc, t tan trong ethanol si v tan trong

ether.

Khong nng chy

80oC - 86oC

5.2. tinh khit

Ch s acid

T 2 n 7.

Ch s x phng ha

T 78 n 95.

Ch s ester

T 71 n 93.
Ch s ester thu c khi ly gi tr ch s x phng ha tr
9

QCVN 4 - 16: 2010/BYT

i gi tr ch s acid.

10

QCVN 4 - 16: 2010/BYT

Tro sulfat

Khng c qu 0,25 % (kl/kl).

Cc cht khng x
phng ha

T 50% n 55%.

Ch

Khng c qu 2,0 mg/kg.

6. Phng php th
6.1. tinh khit
Tro sulfat

Cc cht khng x
phng ha

Cn 2 g mu th vo mt chn s hoc a platin xc

nh trng lng b, un trn la n khi hi bay ra khng
cn mi hng. Nung theo hng dn ti huyn lun xc nh
tro sulfat, phng php I - JECFA monograph 1 - Vol.4).
Cn 5 g mu th, chnh xc n mg, cho vo bnh dung tch
250 ml thm vo cc dung dch gm 2g kali hydroxyd trong
40 ml ethanol, un hi lu (si nh) trong khong 1 gi hoc
n khi qu trnh x phng ha xy ra hon ton. Sau khi kt
thc un hi lu, chuyn hn hp trong bnh v mt phu
chit c nt thy tinh di khong 30 cm, ng kinh 3,5 cm
v c chia vch th tch ( 40,80 v 130 ml). Trng bnh ct
bng cn, gp dch trng vo phu chit, sao cho 40 ml;
tip tc trng bnh bng nc ct nng, nc ct lnh, gp
dch trng vo phu chit sao cho t khong 80 ml; cui
cng trng bnh ct bng vi ml ether du ha, gp dch
trng vo phu chit, lm mt phu chit v dch trong phu
v nhit phng, thm 50 ml ether du ha. y nt phu
chit v lc u trong t nht 1 pht, tch lp hn hp
n khi hn hp trong phu chit tch thnh 2 lp, trong.
Gn ly lp ether pha trn vo phu chit 500 ml (ch
khng ln lp dch pha di). Lp li 6 ln qu trnh
chit nh trn vi lp dch nc, mi ln vi 50 ml ether du
ha, gp cc dch chit ether du ha vo phu chit 500 ml.
Ra dch chit ether du ha trong phu chit 500 ml nhiu
ln, mi ln vi 25 ml ethanol 10%, lc u, ra cho n khi
dch ra cn trung tnh vi phenolphtalein, loi b dch ra
cn. Cho dch ether du ha ra vo cc xc nh
trng lng b, ra phu chit bng 10 ml ether, gp dch
ra ny vo cc ng dch ether du ha. Cho bay hi hn
hp trong cc n kh trn hi nc ca b cch thy. Sy
kh cn n khi lng khng i ti 75oC n 80oC trong
chn khng khng qu 200 mmHg hoc ti 100oC trong 30
pht. ngui trong trong bnh ht m, cn khi lng cn
cn li (cc cht khng x phng ha).
Ha tan cn trong 50 ml ethanol trung tnh m v chun
vi natri hydroxyd 0,02N, s dng ch th l phenolphtalein.
Mi ml natri hydroxyd 0,02N tng ng vi 5,659 mg acid
bo, tnh theo acid oleic.
Hiu chnh kt qu: Ly khi lng cn thu c tr i khi
lng acid bo thu c khi lng chnh xc cc cht
khng x phng ha trong mu th.
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QCVN 4 - 16: 2010/BYT

Ch

- Th theo JECFA monograph 1 - Vol.4.

- 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.

12

QCVN 4 - 16: 2010/BYT

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

INS 401
ADI khng gii hn

2. nh ngha

Mui natri ca acid alginic

M s C.A.S.

9005-38-3

Cng thc ha hc

(C6H7NaO6)n

Cng thc cu to

Cng thc cu to do Phillips, Wedlock and Williams cng

b trong Gums and Stabilizers for the Food Industry 5
(1990), nh xut bn Oxford University Press.

Khi lng phn t

S lng v trnh t ca cc phn mannuronat v gluconat

c th thay i trong alginat t nhin. Cng thc trn cha
th hin s kt hp vi nc.
n v cu trc : 198,11 (l thuyt); 222 (trung bnh trn thc
t).
i phn t: 10000-600000 (trung bnh thng thng)

3. Cm quan

Dng ht, bt hoc si mnh mu trng n vng nu.

4. Chc nng

Cht n, cht n nh, cht lm dy, cht to gel, cht nh

ha

5. Yu cu k thut
5.1. nh tnh
tan

Tan chm trong nc, to ra dung dch nht. Khng tan

trong ethanol v ether.

To kt ta vi calci
clorid

Phi c phn ng kt ta c trng vi calci clorid.

To kt ta vi amoni
sulfat

Phi c phn ng kt ta c trng vi amoni sulfat.

Alginat

Phi c phn ng c trng ca alginat.

Natri

Phi c phn ng c trng ca natri.

5.2. tinh khit

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QCVN 4 - 16: 2010/BYT

Gim khi lng khi sy
kh

Khng c qu 15% (Sy ti 105oC trong 4 gi).

Cht khng tan trong

nc

Khng c qu 2% tnh theo ch phm kh.

Arsen

Khng c qu 3,0 mg/kg.

Ch

Khng c qu 5,0 mg/kg.

5.3. Yu cu v vi sinh vt
Tng s vi sinh vt hiu
kh

Khng c qu 5000 khun lc/g.

Tng s bo t nm
men-mc

Khng c qu 500 khun lc/g

Coliforms

m tnh

Salmonella

m tnh

5.3. Hm lng
(C6H7NaO6)n

Ch phm khan cha khng thp hn 18,0% v khng c

qu 21,0% CO2 tng ng vi khng thp hn 90,8% v
khng c qu 106,0% natri alginat (C6H7NaO6)n.

6. Phng php th
6.1. nh tnh
To kt ta vi calci
clorid

Thm dung dch calci clorid 2,5% vo dch th l dung dch

mu th 0,5% trong dung dch natri hydroxyd (TS), vi th
tch bng 1/5 th tch dch th. Xut hin ta khi ln dng
keo. Php th ny phn bit calci alginat vi gm arabic,
natri carboxymethyl celulose, carragenan, gelatin, gm
ghatti, gm karaya, gm carob bean, methyl celulose, gm
tragacanth.

To kt ta vi amoni
sulfat

Thm dung dch amoni sulfat bo ha vo dch th l dung

dch mu th 0,5% trong dung dch natri hydroxyd (TS), vi
th tch bng 1/2 th tch dch th. Khng c xut hin
ta. Php th ny phn bit calci alginat vi thch, natri
carboxymethyl celulose, carragenan, pectin de-este ha,
gelatin, gm carob bean, methyl celulose v tinh bt.

Alginat

Th theo JECFA monograph 1 - Vol.4.

Natri

Th theo JECFA monograph 1 - Vol.4.

6.2. tinh khit

Cht khng tan trong
nc

Cn 2 g (chnh xc n 0,1 mg) mu, ha vo 800 ml nc

trong bnh 2000 ml. Trung ha ti pH 7 bng dung dch natri
hydroxyd (TS) v thm d 3 ml. Thm 40 ml dung dch hydro
peroxyd 30% (kl/kl), y bnh v un trong khong 1 gi,
khuy thng xuyn. Lc nng qua mt chn lc Gooch c
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QCVN 4 - 16: 2010/BYT

Arsen
Ch

mng lc bng x thy tinh cn b (2,4 cm, No 934 AH,

Reeve Angel & Co, Clifton, N.Y., USA hoc tng ng).
Nu qu trnh lc b chm do dung dch mu c nht cao,
un si n khi nht gim n mc c th lc c. Ra
k chn lc bng nc nng, sy chn lc v phn cht
khng tan ti 105o trong 1 gi, ngui v cn. Tnh hm
lng % ca phn cht khng tan sy kh.
Th theo JECFA monograph 1 - Vol.4. phng php II.
- Th theo JECFA monograph 1 - Vol.4.
- 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. Cc yu cu v
VSV
Tng s vi sinh vt hiu
kh

Ban u chun b m pha long gc 10-1 bng cch

thm 50g mu vo 450ml dung dch pha long m
phosphat Butterfield v ng nht mu bng my trn tc
cao.

6.2. nh lng
Tin hnh theo hng dn trong chuyn lun Xc nh
carbon dioxyd bng phng php decarboxyl ha ti JECFA
monograph 1 - Vol.4.
Mi ml natri hydroxyd 0,25 N s dng tng ng vi 5,5
mg carbon dioxyd hoc 27,75 mg natri alginat (tng ng
khi lng 222).

15