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MINISTRY OF
HEALTH
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SOCIALIST REPUBLIC
OF VIETNAM
Independence – Freedom – Happiness
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No.:
01/2011/TT-BYT
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Hanoi, January
13, 2011
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CIRCULAR
PROMULGATION
OF NATIONAL TECHNICAL REGULATIONS ON FOOD ADDITIVE
MINISTER OF HEALTH
Pursuant to the Law on technical standards and
regulations dated June 29, 2006 and the Government's Decree No. 127/2007/ND-CP
dated August 01, 2007 detailing the implementation of a number of articles of
the Law on Technical regulations and standards;
Pursuant to the Ordinance on food hygiene and
safety dated August 07, 2003 and the Government's Decree No. 163/2004/ND-CP
dated September 07, 2004 detailing the implementation of a number of articles
of the Ordinance on food hygiene and safety;
Pursuant to the Government's Decree No.
188/2007/ND-CP dated December 27, 2007 defining the functions, tasks, powers
and organizational structure of Ministry of Health;
At the request of Directors of Vietnam Food
Administration, the Science and Education Department and the Legal Department,
STIPULATES:
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1. QCVN 4-18:2011/BYT National technical regulation
on Food Additive – Modified starches;
2. QCVN 4-19:2011/BYT National technical regulation
on Food Additive – Enzyme;
3. QCVN 4-20:2011/BYT National technical regulation
on Food Additive – Glazing agent;
4. QCVN 4-21:2011/BYT National technical regulation
on Food Additive – Thickener;
5. QCVN 4-22:2011/BYT National technical regulation
on Food Additive – Emulsifier;
6. QCVN 4-23:2011/BYT National technical regulation
on Food Additive – Foaming agent.
Article 2. This Circular takes effect as of August 01, 2011.
Article 3. Director of Vietnam Food Administration, heads of Ministry
of Health’s departments and affiliates, directors of departments of health of
central-affiliated cities or provinces and relevant organizations and
individuals shall implement this Circular./.
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PP MINISTER
VICE-MINISTER
Trinh Quan Huan
NATIONAL TECHNICAL REGULATION
QCVN 4-18:2011/BYT
NATIONAL TECHNICAL REGULATION ON FOOD ADDITIVE – MODIFIED
STARCHES
Foreword
QCVN 4- :2010/BYT is developed by the Drafting Board for
National technical regulation on Food Additives and Food Processing Aids,
submitted by the Vietnam Food Administration for approval and promulgated
together with the Circular No. 01/2011/TT-BYT dated January 13, 2011 of the
Minister of Health.
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1.
Scope
This National technical regulation
(hereinafter referred to as “the Regulation”) provides for specifications and
regulatory requirements for quality, hygiene and safety of modified starches
used as food additives.
2.
Regulated entities
This Regulation applies to:
2.1. Importers, exporters, producers,
traders and users of modified starches used as food additives (hereinafter
referred to as “entities”).
2.2. Relevant regulatory bodies
3. Interpretation of
terms and acronyms:
3.1. 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) is developed by JECFA and was published by FAO in
2006.
3.2. “C.A.S number”
(Chemical Abstracts Service) refers to registry numbers of chemical substances
identified by the American Chemical Society.
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3.4. “ADI” stands for acceptable daily
intake.
3.5. “INS” stands for international
numbering system.
II.
SPECIFICATIONS, TESTS AND SAMPLING
1. Specifications and tests for:
-
Dextrin roasted starch
- Acid
treated starch
-
Alkaline treated starch
-
Bleached starch
- Oxidized
starch
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-
Monostarch phosphate
-
Distarch phosphate
-
Phosphated distarch phosphate
-
Acetylated distarch phosphate
-
Starch acetate
-
Acetylated distarch adipate
-
Hydroxypropyl starch
-
Hydroxypropyl distarch phosphate
- Starch sodium octenylsuccinate
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2. Specifications specified in this Regulation are tested under
JECFA monograph 1 - Vol. 4, except for some specific tests described in the
Annex. The tests provided in this Regulation are optional. Other equivalent
tests may be used.
3. Sampling adheres to the guidelines in the Circular No.
16/2009/TT-BKHCN dated June 02, 2009 by the Ministry of Science and Technology
and relevant regulations of law.
III. REGULATORY
REQUIREMENTS
1. Declaration
of conformity
1.1.
Modified starches shall be declared in accordance with the regulations set out
in this Regulation.
1.2.
Methods and procedures for declaration of conformity shall comply with the
Regulation on certification and declaration of conformity with regulations and
standards under the Decision No. 24/2007/QD-BKHCN dated September 28, 2007 of
the Minister of Science and Technology and regulations of laws.
2.
Inspection of modified starches
The quality, hygiene and safety of modified starches must
be inspected in accordance with the regulations of law.
IV.
RESPONSIBILITIES OF ENTITIES
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2. Entities are only
entitled to import, export, produce, sell and use propellants as declared after
their completion of registration of declarations of conformity and their
compliance with regulations of law on quality, hygiene, safety and labeling.
V.
IMPLEMENTATION
1. The Vietnam Food
Administration shall preside over and cooperate with competent authorities
concerned to provide guidance on and organize the implementation of this
Regulation.
2. The Vietnam Food
Administration shall, according to its managerial duties, suggest amendments to
this Regulation to the Ministry of Health.
3. In the cases where
any of the international guidelines for tests and regulations of law referred
to in this Regulation is amended or replaced, the newest one shall apply.
ANNEX
SPECIFICATIONS AND TESTS FOR MODIFIED STARCHES
1. Synonyms
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Acid treated starch: INS 1401
Alkaline treated starch: INS 1402
Bleached starch: INS 1403
Oxidized starch: INS 1404
Enzyme-treated starch: INS 1405
Monostarch phosphate: INS 1410
Distarch phosphate: INS 1412
Phosphated distarch phosphate: INS 1413
Acetylated distarch phosphate: INS 1414
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Acetylated distarch adipate: INS 1422
Hydroxypropyl starch: INS 1440
Hydroxypropyl distarch phosphate: INS 1442
Starch sodium octenylsuccinate: INS 1450
2. Definition
Food starches which have one or more of their original
characteristics altered by treatment in accordance with good manufacturing
practice by several certain procedures
Starch acetate:
9045-28-7
Acetylated distarch adipate: 68130-14-3
Hydroxypropyl starch: 9049-76-7
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Acetylated oxidised starch: 68187-08-6
3. Description
Most modified starches are white or off-white, odourless
powders. According to the drying method these powders can consist of whole
granules having the appearance of the original native starch, or aggregates
consisting of a number of granules (pearl starch, starch-grits) or, if
pregelatinized, of flakes, amorphous powder or coarse particles.
4. Functional uses
Modified starch, thickener,
stabilizer, binder, emulsifier
5. Specifications
5.1. Identification
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Insoluble in cold water (if not pregelatinized); forming
typical colloidal solutions with viscous properties in hot water; insoluble
in ethanol.
Microscopy
See description under Tests
Iodine stain
Passes test.
Copper reduction
Passes test.
Differentiation test
Passes test for type of starch.
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- Hypochlorite oxydised starch
- Specific reaction for acetyl groups
- Positive test for ester groups
Sulfur dioxide (SO2)
- Not more than 50 mg/kg for modified cereal starches
- Not more than 10 mg/kg for other modified starches
unless otherwise specified in Table 1
(See description under Tests)
Lead
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- Tested according to JECFA monograph 1 - Vol.4.
- Determine using a method appropriate to the specified
level. The selection of sample size and method of sample preparation may be
based on principles of methods described in JECFA monograph 1 - Volume 4,
Instrumental Methods.
Additional purity specifications for individual modified
starches
- See column 3 of Table 1
- See description under Tests
6.1. Identification
Microscopy
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Iodine stain
Add a few drops of 0.1 N potassium tri-iodide
to an aqueous suspension of the sample. These starches stain with iodine in
the same way as native starches. The colour can range from dark blue to red.
Copper reduction
Place about 2.5 g of the sample previously washed with
water, in a boiling flask, add 10 ml of dilute hydrochloric acid (3%) and 70
ml of water, mix, reflux for about three hours and cool. Add 0.5 ml of the
resulting solution to 5 ml of hot alkaline cupric tartrate TS. A copious red
precipitate is produced.
Differentiation test
To differentiate between various treated starches perform
the following tests:
- Test for hypochlorite-oxidized starch (not for slightly
oxidized potato starch)
Principle:
Because of the carboxyl group content,
hypochlorite-oxidized starch has anionic properties. It can be dyed with
positively charged dyes such as methylene blue.
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50 mg of the sample are kept in suspension for 5-10 min
in 25 ml of a 1% aqueous dye solution and stirred occasionally. After
decantation of the excess solution, the starch is washed with distilled
water. Microscopic inspection clearly shows colouring, if the sample is
hypochlorite-oxidized starch. By this test hypochlorite-oxidized starch is
distinguished from native and acid modified starch of the same botanical
origin.
- Specific reaction of acetyl groups:
Principle: Acetate
is liberated upon saponification of acetylated starch. After concentration
the acetate is converted to acetone by heating with calcium hydroxide. The
acetone thus produced stains blue with o-nitrobenzaldehyde.
Procedure: About 10
g of the sample is suspended in 25 ml water to which is added 20 ml of 0.4 N
NaOH. After shaking for 1 h the starch is filtered off and the filtrate
evaporated in an oven at 110°C. The residue is dissolved in a few drops of
water and transferred to the test tube. Calcium hydroxide is added and if the
sample is an acetylated starch, the tube heated thereby gives off acetone
vapours. These produce a blue colour on a paper strip soaked in a fresh
saturated solution of o-nitrobenzaldehyde in 2 N NaOH. The blue colour is
more distinct when the original yellow colour of the reagents is removed with
1 drop of a 1 in 10 solution of hydrochloric acid.
- Positive test for ester groups :
The infrared spectrum of a thin film gives a typical
absorption band at about 1720 cm-1 which is an indication for
ester groups. The limit of detection is about 0.5% acetyl, adipyl or succinyl
groups in the product.
Sulfur dioxide
Scope:
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Principle:
SO2 is released from the sample in a boiling
acid medium and is removed by a stream of CO2. The separated gas
is collected in dilute hydrogen peroxide where it is oxidized to H2SO4
and titrated with standard alkali. Alternatively, H2SO4
may be determined gravimetrically with BaSO4.
Apparatus:
"Monier-Williams" apparatus for the
determination of sulfurous acid, constructed with standard-taper glass
connections, can be obtained from any reliable scientific glass apparatus
store. It is customary, however, to construct the apparatus with regular
laboratory glassware using stopper connections (see Figure 1).
Figure 1
The assembly consists of a 1000-ml two-neck round-bottom
boiling flask to which a gas-inlet tube, a 60-ml dropping funnel having a
2-mm bore stopcock, and a sloping Allihn reflux condenser are attached. A
delivery tube connects the upper end of the condenser to the bottom of a
250-ml conical receiving flask, which is followed by a Peligot tube.
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Preparation of solutions:
Sodium carbonate solution: Dissolve approximately 15 g of
Na2CO3 or 40 g of Na2CO3.10H2O
in distilled water, and dilute to 100 ml.
Hydrogen peroxide, 3%: Dilute 10 ml of C.P. (Chemical
Purity) neutral 30% hydrogen peroxide (H2O2) with
distilled water to 100 ml.
Procedure:
Pass CO2 to remove chlorine, thence into the
gas-inlet tube of the boiling flask. Place 15 ml of the 3% hydrogen peroxide
in the receiving flask and 5 ml in the Peligot tube. Connect the apparatus
and introduce into the boiling flask, by means of the dropping funnel, 300 ml
of distilled water and 20 ml of concentrated hydrochloric acid. Boil the
contents approximately 10 min in a current of CO2. Weigh, to the
nearest g, 100 g of the sample and disperse in approximately 300 ml of
recently-boiled distilled water. Transfer the slurry to the boiling flask by
means of dropping funnel, regulating the sample addition rate and the gas
flow rate through the apparatus to prevent drawback of hydrogen peroxide,
inclusion of air, or burning of sample. Boil the mixture gently for 1 h in a
slow current of CO2. Stop
the flow of water in the condenser just before the end of the distillation.
When the delivery tube just above the receiving flask becomes hot, remove the
tube from the condenser immediately. Wash the delivery tube and the Peligot
tube contents into the receiving flask, and titrate with 0.1 N sodium
hydroxide, using bromphenol blue indicator (see Note).
Perform a blank determination on the reagents, and
correct results accordingly.
(S – B) x 0.0032 x 100
% SO2 =
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in which:
S: ml of 0.1 N
sodium hydroxide used for the sample
B: ml of 0.1 N sodium hydroxide used for the blank
W: the weight (in
grams) of the sample.
Note: A gravimetric determination may be made after
titration. Acidify with HCl, precipitate with BaCl2, settle,
filter, wash, ignite, and weigh as BaSO4.
Table 1. Additional purity specifications for
individual chemically modified starches
Modification
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End-product specifications
Dextrin roasted starch
Dry heat treatment with hydrochloric acid or
ortho-phosphoric acid- H3PO4
pH = 2.5-7.0
Acid treated starch
Treatment with hydrochloric acid or
ortho-phosphoric acid- H3PO4 or H2SO4
pH = 4.8-7.0
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Alkaline treated starch
Treatment with NaOH or KOH
pH = 5.0-7.5
Bleached starch
Treatment with peracetic acid and/or hydrogen
peroxide, or sodium hypochlorite or sodium chlorite, or sulfur dioxide or alternative permitted
forms of sulfites, or potassium
permanganate or ammonium persulfate
Added carbonyl group not more than 0.1%; No
residual reagent; Residual sulfur dioxide not more than 50 mg/kg; Residual
manganese not more than 50 mg/kg.
Enzyme-treated starch
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Residual sulfur dioxide not more than 50
mg/kg
Oxidized starch
Treatment with sodium hypochlorite
Carboxyl groups not more than 1.1%; Residual
sulfur dioxide not more than 50 mg/kg
Monostarch phosphate
Esterification with ortho-phosphoric acid, or
sodium or potassium ortho-phosphate, or sodium tripolyphosphate
Phosphate calculated as phosphorus not more
than 0.5% for potato or wheat, and not more than 0.4% for other starches
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Distarch phosphate
Esterification with sodium trimetaphosphate
or phosphorus oxychloride
Phosphate calculated as phosphorus not more
than 0.5% for potato or wheat, and not more than 0.4% for other starches
Phosphated distarch phosphate
Combination of treatments for Monostarch
phosphate and Distarch phosphate
Phosphate calculated as phosphorus not more
than 0.5% for potato or wheat, and not more than 0.4% for other starches
Acetylated distarch phosphate
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Acetyl groups not more than 2.5%; phosphate
calculated as phosphorus not more than 0.14% for potato and wheat, and 0.04%
for other starches; and vinyl acetate not more than 0.1 mg/kg
Starch acetate
Esterification with acetic anhydride or vinyl
acetate
Acetyl groups not more than 2.5%
Acetylated distarch adipate
Esterification with acetic anhydride and
adipic anhydride
Acetyl groups not more than 2.5% and adipate
groups not more than 0.135%
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Hydroxypropyl starch
Esterification with propylene oxide
Hydroxypropyl groups not more than 7.0%;
propylene chlorohydrin not more than 1 mg/kg
Hydroxypropyl distarch phosphate
Esterification by sodium trimetaphosphate or
phosphorus oxychloride combined with etherification by propylene oxide
Hydroxypropyl groups not more than 7.0%;
propylene chlorohydrin not more than 1 mg/kg; and residual phosphate calculated
as phosphorus not more than 0.14% for potato and wheat, and not more than
0.04% for other starches
Starch sodium octenylsuccinate
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Octenylsuccinyl groups not more than 3%; and
residual octenylsuccinic acid not more than 0.3%
Acetylated oxidised starch
Treatment with sodium hypochlorite, then
esterification with acetic anhydride
Acetyl groups not more than 2.5% and carboxyl
groups not more than 1.3%
Lead
-
Tested according to JECFA monograph 1 - Vol.4.
-
Determine using a method appropriate to the specified level. The selection of
sample size and method of sample preparation may be based on principles of
methods described in JECFA monograph 1 - Volume 4, Instrumental Methods.
pH
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-
Mix 20 g of the sample with 80 ml of water, and agitate continuously at a
moderate rate for 5 min (In the case of pregelatinized starches, 3 g should
be suspended in 97 ml of water).
Carboxy
groups
As
specified in Column 3 of Table 1.
Principle:
The
carboxyl containing starch is leached with mineral acid to convert carboxyl
salts to the acid form. Cations and excess acid are removed by washing with
water. The washed sample is gelatinized in water and titrated with standard
alkali.
Note:
Native phosphate groups present in potato starch increase the titre found in
this method (See note 6).Reagents:
Hydrochloric
Acid Solution, 0.10 N: Standardization unnecessary
Sodium
Hydroxide Solution, 0.10 N: Standardized
Phenolphthalein
Indicator, 1%
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If
necessary, grind sample completely through a laboratory cutting mill to 20
mesh or finer, taking precautions to prevent any significant change in
moisture, and mix thoroughly.
Weigh
accurately a sample containing not more than 0.25 milli-equivalent of
carboxyl (Note 1), and transfer quantitatively to a 150-ml beaker. Add 25 ml
of 0.1 N hydrochloric acid and stir occasionally over a period of 30 min.
Vacuum filter the slurry through a medium porosity fritted-glass crucible or
small funnel, using a fine stream of water from a wash bottle to aid
quantitative transfer of the sample. Wash the sample with distilled water
(300 ml usually sufficient) until the filtrate is free from chloride
determined by silver nitrate test (Note 2).
Transfer
the demineralized sample quantitatively to a 600 ml beaker with the aid of
distilled water, and slurry the sample in 300 ml of distilled water. Heat
sample dispersion in a steam bath or boiling water bath (Note 3), stirring
continuously until the starch gelatinizes, and continue heating for 15 min to
ensure complete gelatinization (Note 4).
Remove
sample from bath and titrate while hot with standard 0.10 N sodium hydroxide
solution to a phenolphthalein end-point. The end-point may be detected
electrometrically at pH 8.3. A blank determination is run on the original
sample to correct for native acid substances (Note 5). Weigh the same
quantity of starch as taken for carboxyl titration, and slurry in 10 ml of
distilled water. Stir at about 5-min intervals for 30 min. Vacuum filter the
slurry quantitatively through a medium porosity fritted-glass crucible or
small funnel, and wash sample with 200 ml of distilled water. Transfer,
gelatinize, and titrate the sample with standard 0.10 N sodium hydroxide in
the same manner as the demineralized sample.
Calculation:
(ml NaOH – blank) x 0.0045 x 100
Carboxyl groups (%) =
----------------------------------------------------------
Sample weight (g)
Notes
and Precautions:
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Add
1 ml of 1% aqueous silver nitrate solution to 5 ml of filtrate. Turbidity or precipitation
occurs within 1 min if chloride is present.
Heating
on a hot plate or over a Bunsen burner is not recommended. Over-heating or
scorching in amounts too small to be visible will cause sample decomposition
and apparent high carboxyl results.
Thorough
gelatinization facilitates rapid titration and accurate end-point detection.
A
blank titration is run on a water washed sample to correct for acidic
components which are not introduced by oxidation or derivatization. Free
fatty acids complexed with amylose in common corn starch are the principal
contributors to the blank titer.
A
correction for phosphate content in potato starch (deduction) should be made
after determining the phosphorus content of the sample being examined.
The
deduction is calculated:
where:
P = phosphorus content (%)
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As
specified in Column 3 of Table 1
Instrumentation:
Atomic
absorption spectrophotometer with manganese hollow cathode lamp
Preparation
of solutions:
Standard
solution: Prepare a solution containing 0.5 mg/l of manganese.
Sample
solution: Transfer 10.000 g of the sample into a 200-ml Kohlrausch volumetric
flask, previously rinsed with 0.5 N hydrochloric acid, add 140 ml of 0.5 N
hydrochloric acid, and shake vigorously for 15 min, preferably with a mechanical
shaker. Dilute to volume with 0.5 N hydrochloric acid, and shake. Centrifuge
approximately 100 ml of the mixture in a heavy-walled centrifuge tube or
bottle at 650xg for 5 min, and collect the supernatant liquid. This
supernatant comprises the “sample solution”.
Procedure:
Follow
manufacturer's instructions for operating the atomic absorption
spectrophotometer and aspirate distilled water through the air-acetylene
burner for 5 min to obtain a base-line reading at 279.5 nm. In the same
manner aspirate a portion of the "Standard solution" and note the
reading. Finally, aspirate the "Sample solution" and compare the
reading with the reading for the "Standard solution", and multiply
this value by 20 to obtain mg per kg of manganese in the original sample taken
for analysis.
Phosphorus
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Reagents:
Ammonium
Molybdate Solution (5%): Dissolve 50 g of ammonium molybdate tetrahydrate,
(NH4)6Mo7O24·4H2O, in
900 ml of warm water, cool to room temperature, dilute to 1000 ml with water,
and mix.
Ammonium
Vanadate Solution (0.25%): Dissolve 2.5 g of ammonium metavanadate, NH4VO3,
in 600 ml of boiling water, cool to 60 - 70oC, and add 20 ml of
nitric acid. Cool to room temperature, dilute to 1000 ml with water, and mix.
Zinc
Acetate Solution (10%): Dissolve 120 g of zinc acetate dihydrate, Zn(C2H3O2)2,H2O,
in 880 ml of water, and filter through Whatman No. 2V or equivalent filter
paper before use.
Nitric
Acid Solution (29%): Add 300 ml of nitric acid (sp. gr 1.42) to 600 ml of
water, and mix.
Standard
Phosphorus Solution: (100 µg P in 1 ml): Dissolve 438.7 mg of monobasic
potassium phosphate, KH2PO4, in water in a 1000-ml
volumetric flask, dilute to volume with water, and mix.
Standard
Curve:
Pipet
5.0, 10.0, and 15.0 ml of the Standard Phosphorus Solution into separate
100-ml volumetric flasks. To each of these flasks, and to a fourth blank
flask, add in the order stated 10 ml of Nitric Acid Solution, 10 ml of
Ammonium Vanadate Solution, and 10 ml of Ammonium Molybdate Solution, mixing
thoroughly after each addition. Dilute to volume with water, mix, and allow
to stand for 10 min. Determine the absorbance of each standard solution in a
1 cm cell at 460 nm, with a suitable spectrophotometer, using the blank to
set the instrument at zero. Prepare a standard curve by plotting the absorbance of
each solution versus its concentration, in mg P per 100 ml.
Sample
pre-treatment:
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Sample
preparation:
Transfer
about 10 g of the Treated Sample, calculated on the dry-substance and
accurately weighed, into a Vycor dish, and add 10 ml of Zinc Acetate Solution
in a fine stream, distributing the solution uniformly in the sample.
Carefully evaporate to dryness on a hot plate, then increase the heat, and
carbonize the sample on the hot plate or over a gas flame. Ignite in a muffle
furnace at 550°C until the ash is free from carbon (about 1 to 2 h), and
cool. Wet the ash with 15 ml of water and wash slowly down the sides of the
dish with 5 ml of Nitric Acid Solution. Heat to boiling, cool, and
quantitatively transfer the mixture into a 200-ml volumetric flask, rinsing
the dish with three 20-ml portions of water and adding the rinsings to the
flask. Dilute to volume with water, and mix. Transfer an accurately measured
aliquot (V, in ml) of this solution, containing not more than 1.5 mg of
phosphorus, into a 100-ml volumetric flask and add 10 ml of Nitric Acid
Solution, 10 ml of Ammonium Vanadate Solution, and 10 ml of Ammonium
Molybdate Solution, mixing thoroughly after each addition. Dilute to volume
with water, mix, and allow to stand for 10 min.
Procedure:
Determine
the absorbance of the Sample Preparation in a 1 cm cell at 460 nm, with a
suitable spectrophotometer, using the blank to set the instrument at zero. From the Standard
Curve, determine the mg of phosphorus in the aliquot taken, recording this
value as a. Calculate the amount in mg/kg of Phosphorus (P) in the original
sample by the formula:
Where:
W is
the weight of the sample taken, in g.
As
specified in Column 3 of Table 1.
Accurately
weigh about 5 g of the sample and transfer into a 250 ml conical flask.
Suspend in 50 ml of water, add a few drops of phenolphthalein TS, and titrate
with 0.1 N sodium hydroxide to a permanent pink end-point. Add 25.0 ml of
0.45 N sodium hydroxide, stopper the flask, and shake vigorously for 30 min,
preferably with a mechanical shaker. (NOTE: the temperature should not exceed
30oC or some starches may gelatinize). Remove the stopper, wash
the stopper and sides of the flask with a few ml of water, and titrate the
excess alkali with 0.2 N hydrochloric acid to the disappearance of the pink
colour. Record the volume, in ml of 0.2 N hydrochloric acid required as S.
Perform a blank titration on 25.0 ml of 0.45 N sodium hydroxide, and record
the volume, in ml, of 0.2 N hydrochloric acid required as B.
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Acetyl groups (%) =
-------------------------------------------
W
Where:
N is
the normality of hydrochloric acid solution; and
W is
the weight of sample in grams.
Headspace
Gas Chromatographic method.
Use
a gas chromatograph equipped with a 2 m x 2 mm (i.d.) glass column containing
Porapak Q, 80-100 mesh (or equivalent) fitted with a flame ionization
detector, under the following conditions:
-
Carrier gas flow (nitrogen): 20 ml/min
-
injection port temperature: 200°C
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-
detector temperature: 200°C
Standard
preparation: Accurately
weigh 150 mg vinyl acetate (reagent grade) into a 100 ml volumetric flask.
Dissolve and make up to volume with distilled water. Place 1 ml of this
solution in a 10-ml volumetric flask and make up to volume with distilled
water. Add 1 ml of this dilute solution to 30 g unmodified starch of the same
botanical origin as the test substance in a 100-ml flask with a septum-liner.
Seal the flask immediately with the septum-liner. This provides a standard
starch preparation with a vinyl acetate content of 5 mg/kg.
Procedure:
Weigh
30 g of the test substance into a 100-ml flask with a septum-liner. Seal the
flask. Place the flask containing the test substance and the flask containing
the standard preparation in a constant temperature water bath at 70°C for 30
min. Withdraw 2.0 ml from the headspace volume of the flask containing the
standard preparation using a gas-tight syringe, inject directly into the
injection port of the gas chromatograph and record the peak height of the
chromatogram. Similarly inject 2.0 ml of the headspace volume from the flask
containing the test substance into the chromatograph. Calculate the content
of vinyl acetate in the test substance from a comparison of the peak heights
of the two chromatograms.
Adipate
groups
As
specified in Column 3 of Table 1.
Reagents
and Solutions:
N,N-Bis-trimethylsilyltrifluoroacetamide
(BSTFA): Macherey-Nagel, D 5160 Dueren, Germany or equivalent.
Glutaric
acid solution: Dissolve 1.00 g of glutaric acid (Merck or equivalent) in
water and dilute to 1000 ml.
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Apparatus:
Chromatograph:
Hewlett-Packard Model 7620A gas chromatograph or equivalent equipped with
flame ionization detector and Model 3370A integrator.
Column
parameters: 2-m stainless steel, 1.83 mm id, packed with 5% OV17 on 80-100
mesh Chromosorb GAW-DMCS (Alltech Europe, Inc., B 9731 Eke, Belgium);
precondition column 24 h at 350° with nitrogen carrier gas at 40 ml/min.
Operating gas flow rates (ml/min): nitrogen carrier 30, hydrogen 40, air 400. Temperature: injection
280°, detector 250°, column 140°. Retention times (min): glutaric acid 2.83,
adipic acid 4.50.
Calibration:
Weigh
1.0 g waxy corn starch into each of four 250-ml Erlenmeyer flasks. To each
flask add 50 ml water and 1.0 ml of an aqueous solution containing 1.0 mg
glutaric acid/ml. Add, to one flask, 0.25 ml of an aqueous solution
containing 1.0 mg adipic acid per ml; to the other three, add 0.50 ml, 0.75
ml, and 1.0 ml, respectively. Each flask then contains 1.0 mg glutaric acid
and, respectively, 0.25, 0.50, 0.75 and 1.0 mg adipic acid. Agitate flasks
manually to disperse the starch fully and add 50 ml 4N sodium hydroxide.
Continue agitation another 5 min, place each flask in water bath at ambient
temperature, and carefully add 20 ml 12 N hydrochloric acid to each. When
each flask is cool quantitatively transfer contents to 250 ml separatory
funnel. Extract with 100 ml reagent grade ethyl acetate. Drain bottom aqueous
layer into beaker and collect upper organic layer in 500-ml Erlenmeyer flask
containing 20 g anhydrous sodium sulphate. Transfer aqueous portion back to
separatory funnel and repeat ethyl acetate extraction twice more. Shake
flasks periodically during 10 min and then filter contents through Whatman
No. 1 paper into 1-litre round-bottom flasks. Rinse flasks and insoluble
residues in filters twice with 50 ml of ethyl acetate. Under vacuum, (50 mm
Hg) at temperature not exceeding 40°, evaporate total organic extraction and
washings of each flask until completely dry.
The
evaporation of ethyl acetate should be effected as quickly as possible
because some hydrolysis takes place on standing. The products of hydrolysis
cause deterioration in the resolution of adipic acid in the chromatographic
separation.
Successively
add 2 ml pyridine and 1 ml N,N-bis-trimethylsilyltrifluoroacetamide to the
dry contents. Close each of the round-bottom flasks with stopper and rinse
internal surfaces thoroughly by swirling. Let flasks stand 1 h; then transfer
ca 2 ml from each to small glass vials and immediately seal. Inject 4 µl into
gas chromatograph.
Calculations
Establish
retention times for each acid and determine peak height for glutaric acid and
for each level of adipic acid represented. A plot of peak height ratio of
adipic acid to glutaric acid against amount of adipic acid is linear. This
calibration curve may be used, but it is simpler to use a response factor
(RF):
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Hs
and Hl is the peak heights of the standard adipic acid and
glutaric acid, respectively; and
Ws
is the weight of the standard adipic acid.
RF
should be verified weekly.
Total
adipate:
Accurately
weigh about 1.0 g of the sample into a 250 ml Erlenmeyer flask, and add 50 ml
water and 1.0 ml of an aqueous solution containing 1.0 mg glutaric acid/ml.
Proceed as in Calibration, beginning “Agitate flasks manually...”.
Free
adipic acid:
Accurately
weigh about 5.0 g of the sample into a 250 ml Erlenmeyer flask, add 100 ml
water and 1.0 ml of the glutaric acid solution. Agitate for 1 h, filter
through a 0.45 µm Millipore filter, add 1 ml concentrated hydrochloric acid
to the filtrate and transfer it quantitatively to a 250-ml separating funnel.
Proceed as in Calibration, beginning “Extract with 100 ml...”.
Calculation:
For
both preparations (“Total adipate content” and “Free adipic acid content”)
record peak heights for adipic acid and glutaric acid (internal standard).
Calculate the amounts of total adipate and free adipic acid, respectively,
contained in the sample as follows:
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Where:
A is
the content of total adipate or free adipic acid respectively (%);
HX
is the peak height of adipic acid in the actual sample preparation;
HIX is the peak height of glutaric acid in the
actual sample preparation;
RF
is the response factor for adipic acid; and
S is
the weight of sample in the actual preparation (g).
Adipate groups (%) = content of total adipate (%) -
content of free adipic acid (%)
Hydroxypropyl
groups
As
specified in Column 3 of Table 1.
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A 3%
solution of 1,2,3,-triketohydrindene crystals in 5% aqueous sodium bisulfite
solution.
Procedure:
Accurately
weigh about 5 g of the sample and transfer into a 250 ml conical flask. Prepare a sample of
unmodified starch of the same source (i.e. corn or potato) in the same
manner. Place the flasks in a boiling water bath and heat until the samples
are in solution. Cool and dilute the contents to 100 ml with water. If
necessary, dilute the sample further to assure the presence of no more than 4
mg of hydroxypropyl group per 100 ml, and then dilute the blank starch in the same proportion. Pipet
1 ml of the solutions into 25-ml graduated test tubes with glass stoppers
and, with the tubes immersed in cold water, add dropwise 8 ml of concentrated
sulfuric acid to each. Mix well and place the tubes in a boiling water bath
for exactly 3 min. Immediately transfer the tubes to an ice bath until the
solution is chilled. Add 0.6 ml of ninhydrin reagent, carefully allowing the
reagent to run down the walls of the test tubes. Immediately shake well, and
place the tubes in a 25° water bath for 100 min. Adjust the volume in each
tube to 25 ml with concentrated sulfuric acid and mix by inverting the tubes
several times. (Do not shake). Immediately transfer portions of the solutions
to 1-cm cells and after exactly 5 min, measure the absorption (A) at 590 nm,
using the starch blank as the reference. Prepare a calibration curve with
1-ml aliquots of standard aqueous solutions, containing 10, 20, 30, 40 and 50
µg of propylene glycol per ml.
Calculation:
C x
0.7763 x 10 F
Hydroxypropyl groups (%) =-----------------------------
W
Where:
C is
the amount of propylene glycol in the sample solution read from the
calibration curve (µg/ml);
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W is
the weight of sample (mg).
Propylene
chlorhydrin
As
specified in Column 3 of Table 1.
Gas
Chromatographic system:
Use
a Hewlett-Packard Model 5750 or equivalent. A dual-column instrument equipped
with a flame-ionization detector is recommended. An integrator should be part
of the recording system.
Gas
Chromatography column: Use a stainless steel column, 3 m x 3.2 mm (o.d.), packed
with 10% Carbowax 20 M on 80/100-mesh Gas Chrom 2, or equivalent. After
packing and prior to use, condition the column overnight at 200°C, using a
helium flow of 25 ml per min.
Concentrator:
Use a Kuderna-Danish concentrator having a 500-ml flask, available from
Kontes Glass Co., Vineland, N.J., USA, (Catalogue No. K57000), or equivalent.
Pressure
Bottles: Use 200-ml pressure bottles, with a Neoprene washer, glass stopper,
and attached wire clamp, available from Fisher Scientific Co., Pittsburgh,
PA, USA (Vitro 400, Catalogue No. 3-100), or equivalent.
Reagents:
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Florisil:
Use 60/100 mesh material, available from Floridin Co., 3 Penn Center,
Pittsburgh, PA 15235, USA, or an equivalent product.
Propylene
chlorohydrins: Use Eastman No. P1325 1-Chloro-2-propanol Practical,
containing 25% 2-chloro-1-propanol, available from Eastman Kodak Co.,
Rochester, N.Y. 14650, USA or equivalent.
Standard
preparation: Draw 25 µl of mixed propylene chlorohydrin isomers containing
75% of 1-chloro-2-propanol and 25% of 2-chloro-1-propanol) into a 50-µl
syringe. Accurately weigh the syringe and discharge the contents into a
500-ml volumetric flask partially filled with water. Reweigh the syringe, and
record the weight of the chlorohydrins taken. Dilute to the volume with
water, and mix. This solution contains about 27.5 mg of mixed chlorohydrins,
or about 55 µg per ml. Prepare this solution fresh on the day of use.
Sample
preparation:
Transfer
a blended representative 50.0 g sample into a Pressure Bottle, and add 125 ml
of 2 N sulfuric acid. Clamp the top in place, and swirl the contents until
the sample is completely dispersed. Place the bottle in a boiling water bath,
heat for 10 min, then swirl the bottle to mix the contents, and heat in the
bath for an additional 15 min. Cool in air to room temperature, then
neutralize the hydrolyzed sample to pH 7 with 25% sodium hydroxide solution,
and filter through Whatman No. 1 paper, or equivalent, in a Buchner funnel,
using suction. Wash the bottle and filter paper with 25 ml of water, and
combine the washings with the filtrate. Add 30 g of anhydrous sodium sulfate,
and stir with a magnetic stirring bar for 5 to 10 min, or until the sodium sulfate
is completely dissolved. Transfer the solution into a 500-ml separator
equipped with a teflon plug, rinse the flask with 25 ml of water, and combine
the washings with the sample solution. Extract with five 50 ml portions of
diethyl ether, allowing at least 5 min in each extraction for adequate phase
separation. Transfer the combined ether extracts in a Concentrator, place the
graduated receiver of the concentrator in a water bath maintained at 50 -
55°, and concentrate the extract to a volume of 4 ml.
(NOTE:
Ether extracts of samples may contain foreign residues that interfere with
the analysis and/or the interpretation of the chromatograms. These residues
are believed to be degradation products arising during the hydrolysis
treatment. Analytical problems created by their presence can be avoided
through application of a clean-up treatment performed as follows: Concentrate
the ether extract to about 8 ml, instead of 4 ml specified above. Add 10 g of
Florisil, previously heated to 130° for 16 h just before use, to a
chromatographic tube of suitable size, then tap gently, and add 1 g of
anhydrous sodium sulfate to the top of the column. Wet the column with 25 ml
of diethyl ether, and quantitatively transfer the concentrated extract to the
column with the aid of small portions of the ether. Elute with three 25-ml
portions of the ether, collect all of the eluate, transfer it to a
concentrator, and concentrate to a volume of 4 ml).
Cool
the extract to room temperature, transfer it quantitatively to a 5.0-ml volumetric
flask with the aid of small portions of diethyl ether, dilute to volume with
the ether, and mix.
Control
Preparations:
Transfer
50.0 g portions of unmodified (underivatized) waxy corn starch into five
separate pressure bottles, and add 125 ml of 2 N sulfuric acid to each
bottle. Add 0.0, 0.5, 1.0, 2.0, and 5.0 ml of the Standard Preparation to the
bottles, respectively, giving propylene chlorohydrin concentrations, on the
starch basis, of 0, 0.5, 1.0, 2.0, and 5.0 mg/kg, respectively. Calculate the
exact concentration in each bottle from the weight of propylene chlorohydrins
used in making the Standard Preparation. Clamp the tops in place, swirl until
the contents of each bottle are completely dissolved, and proceed with the hydrolysis,
neutralization, filtration, extraction, extract concentration, and final
dilution as directed under Sample Preparation.
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The
operating conditions may be varied, depending upon the particular instrument
used, but a suitable chromatogram is obtained with the Hewlett-Packard Model
5750 using a column oven temperature of 1100C, isothermal;
injection port temperature of 210°C; detector temperature of 240°C; and
hydrogen (30 ml per min), helium (25 ml per min), or air (350 ml per min) as
the carrier gas. A 1.0 mV full-scale recorder is recommended; range,
attenuation, and chart speed should be selected to optimize signal
characteristics. Inject 2.0 µl aliquots of each of the concentrated extracts,
prepared as directed under Control Preparation, allowing sufficient time
between injections for signal peaks corresponding to the two chlorohydrin
isomers to be recorded (and integrated) and for the column to be purged.
Record and sum the signal areas (integrator outputs) from the two
chlorohydrin isomers for each of the controls. Using identical operating
conditions, inject a 2.0 µl aliquot of the concentrated extract prepared as
directed under Sample Preparation, and record and sum the signal areas
(integrator outputs) from the sample.
Calculation:
Prepare
a calibration plot on linear coordinate graph paper by plotting the summed
signal areas for each of the controls against the calculated propylene
chlorohydrin concentrations, in mg/kg, derived from the actual weight of
chlorohydrin isomers used. Using the summed signal areas corresponding to the
1-chloro-2-propanol and 2-chloro-1-propanol from the sample, determine the
concentration of mixed propylene chlorohydrins, in mg/kg, in the sample by
reference to the calibration plot derived from the control samples. After
gaining experience with the procedure and demonstrating that the calibration
plot derived from the control samples is linear and reproducible, the number
of controls can be reduced to one containing about 5 mg/kg of mixed propylene
chlorohydrin isomers. The propylene chlorohydrin level in the sample can then
be calculated as follows:
Where:
C is the concentration,
in mg/kg, of propylene chlorohydrins (sum of isomers) in the control;
a is
the sum of signal areas produced by the propylene chlorohydrin isomers in the
sample; and
A is
the sum of the signal areas produced by the propylene chlorohydrin isomers in
the control.
Degree
of substitution of starch sodium octenyl succinate
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The
degree of substitution is determined by alkali consumed after acidification
and thorough washing of the starch half ester.
Procedure:
Weigh
out 5.0 g of sample in a 150-ml beaker. Wet out with a few ml of reagent
grade isopropyl alcohol. Add, by pipette 25 ml of 2.5 N hydrochloric acid in
isopropanol, allowing the acid to wash down any sample on the sides of the
beaker. Stir for 30 min on a magnetic stir plate. Add 100 ml of 90%
isopropanol from a graduated cylinder. Stir for 10 min. Filter the sample
through a Buchner funnel and wash the filter cake with 90% isopropanol until
the filtrate is negative for chloride ions. Use 0.1 N AgNO3 to check for
chloride ions. Transfer the filter cake to a 600-ml beaker and rinse the
Buchner funnel to wash any starch into the beaker. Bring to a 300-ml volume
with distilled water. Place for 10 min in a boiling water bath with stirring.
Titrate while hot with 0.1 N NaOH to the phenolphthalein end-point.
Calculation:
0.162 x A
Degree of substitution (DS) = -------------------------
1 – 0.210 x
A
Where:
A is milliequivalents
of sodium hydroxide required per 1g of starch octenyl succinate.
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Extraction and
preparation of sample solution:
Extract about 500 mg of
starch with 15 ml of methanol overnight under constant shaking (weigh starch
accurately). Filter the extraction mixture. Wash the starch on the filter
with 7 ml of methanol. Repeat three times. Combine all filtrates (about 80%
of the residuals are extracted by this procedure). Add 1 ml of 0.16 N
methanolic KOH to the extracts. Dry the extracts with a flash evaporator at
30°. Dissolve the residue in 2 ml methanol. Dry the extract using a flash
evaporator at 30°C and dissolve the residue in 2 ml of methanol. Take 0.5 ml
of residue solution to the reaction vial. Add 0.5 ml derivative reagent (2.8
g of 2-p-dibromoacetophenone and 0.28 g 18-Crown-6 in 50 ml CH3CN)
to the reaction vial. Add 2 ml CH3CN to the reaction vial. Cap the
reaction vial and heat it at 80° for 30 min. Cool the reaction solution to
room temperature (use within 24h).
Liquid Chromatography
Analysis:
- Column:
Micro-Bondapark C18 (Waters) or equivalent
-
Mobile Phase: Gradient elution of 70% to 80% methanol in water in 5 min.
Curve 6 (Waters 660 solvent programmer).
Flow
Rate: 1.5 ml/min
Detector:
UV at 254 nm, attenuation 0.16 AUFS
Injection
volume: 5 ml
Preparation
of Calibration Curve:
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for
Solution C1 0.2375 mg
for
Solution C2 0.4750 mg
for
Solution C3 0.9500 mg
Plot
peak height from Liquid Chromatograph Chart versus m g of residuals
per 5 ml of solution.
Calculation:
Prepare
a calibration curve according to the procedure. Using the peak height of the
unknown sample from the Liquid Cromato-graph Chart, determine the level of
residuals (calculated as octenyl succinic acid) in the injected volume from
the calibration curve.
300 x value from
graph
% Residual starch = -------------------------------------------
Weight of starch
(mg)
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QCVN 4-19:2011/BYT
NATIONAL
TECHNICAL REGULATION ON FOOD ADDITIVE – ENZYME
Preface
QCVN 4-19:201/BYT is compiled by
the Drafting Board of national technical regulations on food additive and
processing aids, submitted for approval by Vietnam Food Administration and
promulgated under Circular No. 01/2011/TT-BYT dated January 13, 2011 by
Minister of Health.
NATIONAL
TECHNICAL REGULATION ON FOOD ADDITIVE – ENZYME
I. GENERAL PROVISIONS
1. Scope
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2. Regulated entities
This Regulation applies to:
2.1. Importers, exporters, producers, traders and
users of enzymes as food additive (hereinafter referred to as entities).
2.2. Relevant regulatory agencies.
3. Interpretation of terms and acronyms:
3.1. JECFA monograph 1 - Vol. 4 refers to 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 ( or referenced) in the food additive
specifications; compiled by JECFA; issued by FAO in 2006.
3.2. C.A.S (Chemical Abstracts
Service) number refers to registry numbers of chemical substances identified by
the American Chemical Society.
3.3. TS (test solution) means reagent liquid.
3.4. ADI stands for acceptable daily intake.
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II. SPECIFICATIONS, METHODS OF
ASSAY AND SAMPLING
1. Specifications and methods of assay for
enzymes are defined in annexes to this Regulation:
1.1.
Annex 1 :
Specifications and methods of assay
for amylase
1.2.
Annex 2 :
Specifications and methods of assay
for protease
1.3.
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Specifications and methods of assay
for papain
1.4.
Annex 4 :
Specifications and methods of assay
for bromelain
1.5.
Annex 5 :
Specifications and methods of assay
for glucose oxidase and catalase
2.
Specifications in this Regulation are tested according to JECFA monograph 1 -
Vol. 4, except for certain specific methods of assay prescribed in annexes
herein. Methods of assay as prescribed in this Regulation are not mandatory.
Different methods of assay with equivalent degree of precision may be employed.
3.
Sampling adheres to the guidelines in the Circular
No. 16/2009/TT-BKHCN dated June 02, 2009 by the Ministry of Science
and Technology on regulations for state inspection of the quality of goods in
circulation and relevant laws.
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1. Declaration of conformity
1.1. The conformity of enzymes must
be declared according to this Regulation.
1.2. The method and procedure for
declaration of conformity shall be governed by regulations on certification and
declaration of conformity enclosed to Decision No. 24/2007/QD-BKHCN dated
September 28, 2007 by Minister of Science and Technology and by relevant laws.
2. Inspection of enzymes
The quality,
hygiene and safety of enzymes must be inspected in accordance with the law
regulations.
IV.
RESPONSIBILITIES OF ENTITIES
1. Entities
must declare their conformity with this Regulation, register their declaration
of conformity at Vietnam Food Administration and ensure the quality, hygiene
and safety of enzymes as declared.
2. Entities shall only be permitted to import, export, produce, sell and
use enzymes upon their completion of registration of declaration of conformity
and their fulfillment of law regulations on quality, hygiene, safety and
labeling.
V. IMPLEMENTATION
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2. Vietnam Food Administration, according to its administrative devoirs,
shall be responsible for proposing to the Ministry of Health the amendments and
supplements to this Regulation.
3. If international guidelines for methods of assay and laws referred to
in this Regulation are amended, supplemented or replaced, revised documents
shall prevail.
ANNEX 1
SPECIFICATIONS AND METHODS OF ASSAY
FOR α-AMYLASE AND GLUCOAMYLASE
INS 1100
Produced by the controlled
fermentation of non-toxicogenic and nonpathogenic strains of Aspergillus
oryzae and isolated from the growth medium
alpha-Amylase
(synonyms: diastase, ptyalin, glycogenase)
Glucan
1,4-alpha-glucosidase (synonyms: amyloglucosidase, acid maltase, lysosomal
alpha-glucosidase, exo-1,4-alpha-glucosidase)
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EC 3.2.1.1
alpha-Amylase hydrolyzes
1,4-alpha-glucosidic linkages in polysaccharides yielding dextrins, oligosaccharides
and glucose
Glucoamylase hydrolyzes
1,4-alpha- and 1,6-alpha-glucosidic linkages in polysaccharides yielding
glucose
Lipase (EC
3.1.1.3)
Tannase (EC
3.1.1.20)
Cellulase (EC
3.2.1.4)
Endo-1,3-beta-glucanase
(EC 3.2.1.6)
Pectinase (EC
3.2.1.15)
Maltase (EC
3.2.1.20)
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Endo-1,4-beta-mannanase
(EC 3.2.1.78)
Protease
Tan amorphous powders or tan
to dark-brown liquids that may be dispersed in diluents (purely used in food)
and may contain stabilizers and preservatives; soluble in water and
practically insoluble in ethanol and ether
Enzyme preparation.
Used in the hydrolysis of
cereals and starch; in the preparation of fruit and vegetable products,
beverages, sugar, confectionery and bakery products and in honey.
Must
conform to the general specifications for enzyme preparations used in food
processing
Reactions are
required to show typical alpha-amylase activity (from Aspergillus
oryzae, var ) (adop methods of assay in JECFA monograph 1 -
Vol.4)
Reaction shows typical glucoamilase
activity (from Aspergillus oryzae, var ) (use
methods of assay in JECFA monograph 1 - Vol.4)
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ANNEX 2
SPECIFICATIONS AND METHODS OF ASSAY
FOR PROTEASE (FROM FUNGAL)
INS 1101(i)
Produced by the controlled
fermentation of non-toxicogenic and nonpathogenic strains of Aspergillus
oryzae and isolated from the growth medium
Endo- and
exopeptidases
1. Aminopeptidases (EC
3.4.11)
2. Serine
endopeptidases (EC 3.4.21)
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1. Hydrolysis of proteins at
the N-terminal, liberating amino acids
2. Hydrolysis of proteins
containing serine peptide bonds
3. Hydrolysis of proteins
containing aspartic acid bonds
alpha-amylase
(EC 3.2.1.1)
Off-white to tan amorphous powders
dispersed in dispersion medium or carriers (purely used in food); may contain
stabilizers and preservatives; soluble in water and practically insoluble in
ethanol and ether
Enzyme preparation.
Used in the preparation of
meat and fish products, beverages, soup and broths, dairy and bakery
products.
Must
conform to the general specifications for enzyme preparations used in food
processing (see instructions)
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Reaction shows
typical proteolytic activity (Use method of assay for proteolytic, Fungal
(HUT))
SPECIFICATIONS AND METHODS OF ASSAY
FOR PAPAIN
INS 1101(ii)
Purified proteolytic
substances derived from the fruit of Carica papaya (L) (Fam. Caricaceae)
1. Papain (papaya
peptidase I, cystein proteinase)
2. Chymopapain (cystein
proteinase)
1. None
(EC 3.4.22.2)
2. None
(EC 3.4.22.6)
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White to light tan amorphous
powder or liquids; soluble in water, the solutions being colourless to light
yellow and somewhat opalescent; practically insoluble in alcohol, chloroform
and ether
Enzyme preparation.
Used in
the processing and preparation of beef, processing of meat, preparation of
cereals, and production of protein hydrolysates
Must
conform to the general specifications for enzyme preparations used in food
processing (see instructions)
Reaction shows
typical plant proteolytic activity
SPECIFICATIONS AND METHODS OF ASSAY
FOR BROMELAIN
INS 1101(iii)
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Bromelain (crystein
proteinase)
None (EC
3.4.22.4)
The enzyme hydrolyzes polypeptides, amides and esters, especially at
linkages involving basic amino acids, or leucine or glycine, yielding
peptides of lower molecular weight.
White to
light tan amorphous powder; soluble in water, the solutions being colourless
to light yellow and somewhat opalescent; practically insoluble in alcohol,
chloroform and ether
Enzyme preparation.
Used in
the processing of beef, processing of meat, preparation of cereals, and
production of protein hydrolysates
Must
conform to the general specifications for enzyme preparations used in food
processing
Reaction shows
typical plant proteolytic activity (see Proteolytic activity, plant)
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SPECIFICATIONS AND METHODS OF ASSAY
FOR GLUCOSE OXIDASE AND CATALASE FROM ASPERGILLUS NIGER var.
Glucose
oxyhydrase, glucose aerodehydrogenase, notatin, aero-glucose dehydrogenase;
INS 1102
Commercial enzyme preparations
are produced by the controlled fermentation of Aspergillus niger va r.
1. Glucose oxidase
2. Catalase
1. ß-D-glucose: oxygen
1-oxidoreductase (EC 1.1.3.4)
2. Hydrogen-peroxide:
hydrogen-peroxide oxidoreductase (EC 1.11.1.6)
1. ß-D-glucose + O2
--> D-glucono-delta-lactone + H2O2
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Invertase
(EC 3.2.1.26)
Off-white
to brown liquids; soluble in water and practically insoluble in ethanol,
chloroform and ether
Enzyme preparation.
Used in
the preparation or use of milk, cheese, eggs, beverages and salads
Must
conform to the general specifications for enzyme preparations used in food
processing
Reaction shows
glucose oxidase activity (see Vol 4.)
Reaction shows
typical catalase activity (see Vol 4.)
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Foreword
QCVN 4-21:2011/BYT is prepared by the Drafting Board of
national technical regulations on food additive and processing aids, presented
by the Vietnam Food Administration and promulgated under the Circular No.
01/2011/TT-BYT dated January 13, 2011 of the Minister of Health.
I. GENERAL
1. Scope
This
national technical regulation (hereinafter referred to as “document”) provides
for specifications and regulatory requirements for quality, hygiene and safety
of thickeners used as food additive.
2. Regulated entities
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2.1.
Importers, exporters, producers, traders and users of thickeners as food
additive (hereinafter referred to as “entities”).
2.2.
Relevant regulatory agencies.
3.
Interpretation of terms and acronyms:
3.1.
“thickener” refers to a food additive which is used to increase the viscosity
of a foodstuff.
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).
3.3.
“C.A.S number” (Chemical Abstracts Service) refers to registry numbers of
chemical substances identified by the American Chemical Society.
3.4.
“TS” stands for test solution.
3.5.
“ADI” stands for acceptable daily intake.
3.6.
“INS” stands for International Numbering System for Food Additives.
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1. Specifications and tests for thickeners
are provided in annexes to this document:
1.1.
Annex
1:
Specifications
and tests for alginic acid
1.2.
Annex
2:
Specifications
and tests for potassium alginate
1.3.
Annex
3:
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1.4.
Annex
4:
Specifications
and tests for calcium alginate
1.5.
Annex
5:
Specifications
and tests for propylene glycol alginate
1.6.
Annex
6:
Specifications
and tests for agar
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Annex
7:
Specifications
and tests for carrageenan and its Na, K, NH4 salts
1.8.
Annex
8:
Specifications
and tests for carob bean gum
1.9.
Annex
9:
Specifications
and tests for guar gum
1.10.
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Specifications
and tests for tragacanth gum
1.11.
Annex
11:
Specifications
and tests for arabic gum
1.12.
Annex
12:
Specifications
and tests for xanthan gum
1.13.
Annex
13:
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1.14.
Annex
14:
Specifications
and tests for tara gum
1.15.
Annex
15:
Specifications
and tests for gellan gum
1.16.
Annex
16:
Specifications
and tests for pectins
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Annex
17:
Specifications
and tests for methyl cellulose
1.18.
Annex
18:
Specifications
and tests for methyl ethyl cellulose
1.19.
Annex
19:
Specifications
and tests for sodium carboxymethyl cellulose
1.20.
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Specifications
and tests for edible gelatin
2. Specifications in this document are
tested according to JECFA monograph 1 - Vol. 4, except for certain specific
tests prescribed in annexes herein. Tests prescribed in this document are not
mandatory. Different tests with equivalent degree of precision may be employed.
3. Sampling adheres to the guidelines in the
Circular No. 16/2009/TT-BKHCN dated June 02, 2009 by the Ministry of Science
and Technology and relevant law regulations.
III.
REGULAORY REQUIREMENTS
1. Declaration of conformity
1.1. Declarations of conformity of thickeners
shall be submitted in accordance with regulations of this document.
1.2. Methods and procedures for submission of
declarations of conformity shall comply with the Regulation on certification
and declaration of conformity and conformance under the Decision No.
24/2007/QD-BKHCN dated September 28, 2007 by Minister of Science and Technology
and the laws.
2. Inspection of thickeners
The
quality, hygiene and safety of thickeners must be inspected in accordance with
the law regulations.
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1. Entities must declare their
conformity with the specifications mentioned this document, register their
declarations of conformity at the Vietnam Food Administration and ensure the
quality, hygiene and safety of thickeners as declared.
2. Entities are only entitled to import, export,
produce, sell and use thickeners after their completion of registration of
declarations of conformity and their fulfillment of law regulations on quality,
hygiene, safety and labeling.
V.
IMPLEMENTATION
1. Vietnam Food Administration shall take charge and
cooperate with authorities concerned to provide guidance on and organize the
implementation of this document.
2. The Vietnam Food Administration shall, according to its
managerial duties, recommend amendments to this document to the Ministry of
Health.
3. In the cases where any of the international guidelines for
tests and regulations referred to in this document is amended or replaced, the
newest one shall apply