GB 31604.8-2021 PDF English
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Food safety national standard - Food contact materials and products - Determination of total migration
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GB 31604.8-2021: Food safety national standard - Food contact materials and products - Determination of total migration
---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB31604.8-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact
Materials and Products - Determination of Total
Migration
Issued on: SEPTEMBER 07, 2021
Implemented on: MARCH 07, 2022
Issued by. National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
Foreword... 3
1 Scope... 4
Part One -- Determination of total migration in water-based food simulants,
chemical alternative solvents... 4
2 Principle... 4
3 Reagents and materials... 4
4 Instruments and equipment... 5
5 Analysis steps... 5
6 Expression of analysis results... 7
7 Precision... 11
Part Two -- Determination of total migration in olive oil... 12
8 Principle... 12
9 Reagents and materials... 12
10 Instruments and equipment... 14
11 Analysis steps... 14
12 Expression of analysis results... 20
13 Precision... 24
Annex A Suitability Judgment... 25
Annex B Confirmation of moisture-sensitive specimens and adjustment of
moisture content -- Vacuum drying method... 26
Annex C Confirmation of moisture-sensitive specimens and adjustment of
moisture content -- Constant humidity method... 28
Annex D Typical chromatogram... 30
1 Scope
This Standard specifies the methods for determination of total migration for food
contact materials and products.
This Standard is applicable to the determination of total migration for food
contact materials and products.
Part One -- Determination of total migration in water-
based food simulants, chemical alternative solvents
2 Principle
The specimen uses water-based food simulants and chemical alternative
solvents [such as n-hexane, isooctane, 95% (volume fraction) ethanol solution,
n-heptane]. Perform migration test under selected migration test conditions.
Evaporate and dry the soaking liquid obtained from the migration test. After
deducting the corresponding blanks, the total amount of all non-volatile
substances migrated from the specimen to water-based food simulants and
chemical substitute solvents is obtained.
3 Reagents and materials
Unless otherwise specified, the reagents used in this method are analytically
pure, and the water is grade two water specified in GB/T 6682.
3.1 Reagents
3.1.1 Absolute ethanol (C2H6O).
3.1.2 Acetic acid (C2H4O2).
3.1.3 Trichloromethane (CHCl3).
3.1.4 N-hexane (C6H14).
3.1.5 Isooctane (C8H18).
3.1.6 95% ethanol.
3.1.7 N-heptane (C7H16).
4 Instruments and equipment
4.1 Balance. Resolution is 0.1mg.
4.2 Electric heating constant temperature drying oven.
4.3 Electric heating constant temperature water bath or other electric heating
equipment.
5 Analysis steps
5.1 Migration test
Food contact materials and products are subjected to migration tests in
accordance with the requirements of GB 31604.1 and GB 5009.156.
5.2 Determination of total migration of water-based food simulants and
chemical substitute solvents
Wash and drain the evaporating dish before use. Dry for 2h in a 100°C±5°C
electric heating constant temperature drying oven. Then weigh it after cooling
for 0.5h in a desiccator. Repeat drying, cooling, and weighing until constant
weight (that is, the difference in mass between the two weighings does not
exceed 0.5mg). The last weighed mass is the mass of the empty evaporating
dish.
5.3 Determination of trichloromethane extract
The determination steps are applicable to food contact materials and products
that require the detection of chloroform extracts in the product standard.
Add 20mL of chloroform to the residue obtained in 5.2.Wetting the residue. Use
the filter paper to filter. Collect the filtrate into an evaporating dish with constant
weight. Then use 20mL of chloroform to extract the residue twice respectively.
Use a little chloroform to rinse the filter paper. The filtrate is incorporated into
the evaporating dish. Steam to dry according to step 5.2.Obtain the mass of
the residue extracted with chloroform from the soaking solution for the
specimen determination.
5.4 Blank test
Treat water-based food simulants, chemical alternative solvents, and
chloroform that are not in contact with food contact materials and products
according to 5.1, 5.2, and 5.3.Obtain the residue mass of the blank soaking
solution and the residue mass of the blank soaking solution extracted with
chloroform.
6 Expression of analysis results
6.1 Total migration calculation
6.1.1 Expressed in mg/dm2
6.1.1.1 Food contact materials and products of non-sealed products
When the total migration of food contact materials and products other than
sealed products such as lids, gaskets, and connectors (hereinafter referred to
as sealing products) is expressed in mg/dm2, it is calculated according to
formula (1).
Where,
6.1.2 Expressed in mg/kg
6.1.2.1 Food contact materials and products of non-sealed products
When the total migration amount of food contact materials and products of non-
sealed products is expressed in mg/kg, it is calculated according to formula (3).
7 Precision
When the total migration result is ≤ 10.0mg/dm2 or 60.0mg/kg, the difference
between the two independent determination results obtained under
repeatability conditions and the arithmetic mean shall not exceed 1.0mg/dm2 or
6.0mg/kg. The determination result after applying the correction factor shall also
meet this requirement.
When the total migration result is > 10.0mg/dm2 or 60.0mg/kg, the difference
between the two independent determination results obtained under
repeatability conditions and the arithmetic mean shall not exceed 10% of the
arithmetic mean. The determination result after applying the correction factor
shall also meet this requirement.
8 Principle
The specimen uses olive oil as a food simulant. The migration test is carried
out under the selected conditions. The total migration is determined by the
specimen mass reduction method. That is, use the initial mass of the specimen
before the migration test to subtract the net mass of the specimen after soaking
in olive oil to obtain the mass of non-volatile substances migrated from the
specimen. Calculate the corresponding total migration amount according to the
formula. The net mass of the specimen after soaking in olive oil is the mass of
the specimen when it is taken out of the olive oil minus the mass of olive oil
absorbed by the specimen plus the mass of volatile matter. The olive oil
absorbed by the specimen is extracted, saponified, and methyl esterified by the
Soxhlet extractor to generate fatty acid methyl esters. Use gas chromatography
to analyze. Use internal standard method to quantify.
9 Reagents and materials
Unless otherwise specified, the reagents used in this method are analytically
pure, and the water is grade two water specified in GB/T 6682.
9.1 Reagents
9.1.1 Olive oil. Its mass requirements shall meet the requirements of Annex A
of GB 5009.156.
9.1.2 N-Pentane (C5H12).
9.1.3 Absolute ethanol (C2H6O).
9.1.4 N-Heptane (C7H16). Chromatographically pure.
9.1.5 Cyclohexane (C6H12).
9.1.6 Anhydrous sodium sulfate (Na2SO4).
9.1.7 Ether (C4H10O).
9.1.8 Potassium hydroxide (KOH).
9.1.9 Methanol (CH4O).
9.1.10 Boron trifluoride methanol solution. about 150g/L boron trifluoride (BF3).
9.1.11 Sulfuric acid (H2SO4).
9.2 Preparation of reagents
9.2.1 N-pentane-ethanol (95+5) mixed solution. Measure 950mL of n-pentane
and mix it with 50mL of absolute ethanol.
9.2.2 Potassium hydroxide-methanol solution (11.0g/L). Weigh 5.5g of
(accurate to 0.1g) potassium hydroxide and dissolve it in 500mL of methanol.
Mix well.
9.2.3 Saturated sodium sulfate solution. Weigh 50g (accurate to 0.1g) of
anhydrous sodium sulfate in a 250mL beaker. Add 100mL of water on the
electric hot plate and boil to dissolve. After cooling to room temperature, use a
funnel equipped with qualitative filter paper to filter into a breaker.
9.3 Standard product
Heptadecanoic acid triglyceride (C54H104O6, CAS number. 2438-40-6). Purity
≥98%, or standard material certified by the country and awarded with a standard
material certificate.
9.4 Preparation of standard solution
9.4.1 Internal standard solution (2.0mg/mL)
Accurately weigh 1.0g (accurate to 0.1mg) of heptadecanoic acid triglyceride.
Place in a 100mL beaker. Add cyclohexane to dissolve. Transfer to a 500mL
volumetric flask. Wash the beaker 3 times with cyclohexane. The washing liquid
is combined into the volumetric flask. Use cyclohexane to set volume. Store in
a refrigerator at 4°C. The validity period is 1 month.
9.4.2 Olive oil standard stock solution (100mg/mL)
Weigh 5.0g of blank olive oil obtained from migration test (accurate to 0.1mg).
Place in a 50mL beaker. Add n-heptane to dissolve. Transfer to a 50mL
volumetric flask. Wash the beaker 3 times with n-heptane. The washing liquid
is combined into the volumetric flask. Use N-heptane to set volume. Prepare it
when it is required.
9.5 Materials
9.5.1 Heating plate.
9.5.2 Airtight moisture content adjustment container. Such as glass dryer.
9.5.3 Filter membrane. Organic phase, 0.22μm.
9.5.4 Filter paper. Qualitative filter paper, fast.
9.5.5 Dust-free wipe paper.
9.5.6 Glass fiber filter cartridge.
10 Instruments and equipment
10.1 Gas chromatograph. Equipped with a hydrogen flame ionization detector
(FID).
10.2 Analytical balance. Resolutions are 0.1mg, 0.1g.
10.3 Soxhlet extractor.
10.4 Low temperature circulating condensate pump.
10.5 Electric heating constant temperature water bath.
10.6 Rotary evaporator.
10.7 Vacuum drying oven.
10.8 Humidity chamber.
11 Analysis steps
11.1 Specimen preparation
Food contact materials and products are prepared according to the
requirements of GB 31604.1 and GB 5009.156 for migration test. The specimen
preparation area of total immersion method and filling method shall be ≥1dm2.
The area of the specimen in the test cell method is calculated based on the
actual area of the specimen in contact with the food simulant. The specimen
preparation area of bagging method shall be ≥2dm2.Each specimen can be
prepared from multiple products. The number of specimens is determined
according to the following purposes.
a) Migration test. At least 3 specimens of disposable products; At least 3
specimens per set of specimens for repeated use of products;
b) Volatile matter determination. 2 specimens;
c) Suitability judgment (see Annex A). 2 specimens;
d) Surface area determination. 1 specimen;
e) Confirmation of moisture sensitivity. 2 specimens.
11.2 Suitability Judgment
Take 2 specimens to determine the suitability of the method according to the
steps described in Annex A. If the previous test has confirmed the suitability of
the method, it can omit the steps in Annex A.
11.3 Weighing of the initial mass of the specimen
Determine whether the specimen is moisture sensitive according to the steps
described in Annex B or Annex C. If the previous test has confirmed that the
specimen is a non-moisture-sensitive specimen, it can omit the steps in Annex
B or Annex C.
If the specimen is a non-moisture sensitive specimen, directly weigh the initial
mass. If the specimen is moisture sensitive, after adjusting the moisture content
according to the steps described in the relevant appendix, the initial mass of
the specimen is obtained. If the specimen adopts the steps described in Annex
C to adjust the moisture content and cannot reach a constant weight within 5d,
use Annex B to adjust the moisture content.
11.4 Migration test
The migration test of food contact materials and products shall be conducted in
accordance with the requirements of GB 31604.1 and GB 5009.156.For
reusable products, test on 3 sets of specimens prepared from the same batch
of test specimens. Each group of specimens differs only in the migration test
time. The migration test time of the first group of specimens is the migration test
time determined according to the requirements of relevant standards. The
migration test time of the second group of specimens is twice that of the first
group. The migration test time of the third group of specimens is 3 times that of
the first group. The number of parallel specimens for migration test should meet
the requirements of 11.1a).
11.5 Weighing the final mass of the specimen
Remove the specimen from the olive oil as soon as possible after the migration
test is completed. Cool to room temperature. Place the specimen between two
filter papers or dust-free wipes. Lightly press it. Suck off the olive oil on the
surface of the specimen. Repeat the pressing steps until no oil spots appear on
the paper. No paper fibers shall remain on the surface of the specimen. For
non-moisture sensitive specimens, directly weigh the final mass. After adjusting
the moisture content of the moisture-sensitive specimen in the same way as in
11.3, weigh the final mass.
11.6 Determination of the volatile matter of the specimen
Prepare 2 parallel specimens according to the steps described in 11.1.Obtain
the initial mass of the specimen according to the steps described in 11.3.Except
that no olive oil is added, carry out the migration test according to the steps
described in 11.4.For non-moisture sensitive specimens, directly weigh the
final mass. After adjusting the moisture content of the moisture-sensitive
specimen in the same way as in 11.3, weigh the final mass.
The mass of volatile matter per unit area of each parallel specimen is calculated
by dividing the difference between the initial mass and the final mass of the
specimen by the corresponding sampling area. If the moisture content of the
specimen is adjusted according to the steps described in Annex B, this step can
be omitted.
11.7 Blank test
Follow the steps in 11.4 to dispose of olive oil that is not in contact with food
contact materials and products. Use it to prepare olive oil standard stock
solution.
11.8 Determination of the absorption of olive oil by the specimen
11.8.1 The first extraction of olive oil
The extraction solvent is selected according to the main polymer material of the
food contact surface of the food contact materials and products. When the main
material is the specimen of non-polar polymer (such as polyethylene,
polypropylene), use N-pentane. When the main material is a specimen of polar
polymer (such as polyethylene terephthalate), use a mixed solution of n-
pentane-ethanol (95+5).
Add 10.0mL of internal standard solution (2.0mg/mL) and extraction solvent to
the collection bottle of the Soxhlet extractor. Add zeolite or glass beads to
prevent explosion boiling. Cut the specimen into suitable size. Wrap it with
qualitative filter paper or put it in a glass fiber sleeve barrel (including specimen
debris, particles generated during the cutting process). Put into Soxhlet
extractor. Perform reflux extraction for 7h~8h. Cycle at least 6 times per hour.
Make sure that the specimen is completely immersed in the solvent and kept
separate from each other during each cycle.
11.8.2 The first methyl esterification of olive oil
11.8.2.1 Transfer of extract
The obtained extraction solution is evaporated to about 10mL with a rotary
evaporator or distillation device and transferred to a 50mL flask. Wash the
collection bottle with extraction solvent 3 times. Combine the detergent that
have been washed for 3 times into the flask. Evaporate to dryness on a rotary
evaporator.
12 Expression of analysis results
12.1 Expressed in mg/dm2
12.1.1 Food contact materials and products of non-sealed products
When the total migration amount of food contact materials and products of non-
sealed products is expressed in mg/dm2, it is calculated according to formula
(8).
12.3 Expressed in mg/piece
The total migration amount of food contact materials and products of sealed
products is expressed in mg/piece. Calculate according to formula (12). The
migration test method used and the area of contact between a single sealed
product and the food simulant in the migration test shall be indicated.
12.4 Correction of results
When GB 31604.1 specifies the correction factor for fat-containing food
simulants, the determination results shall be divided by the corresponding
correction factor.
12.5 Expression of results
The calculation result of total migration is the arithmetic mean of 3 parallel
determination results. The calculation result is accurate to one decimal place.
13 Precision
When the total migration result is ≤ 10.0mg/dm2 or 60.0mg/kg, the difference
between the three independent determination results obtained under
repeatability conditions and the arithmetic mean shall not exceed 3.0mg/dm2 or
20.0mg/kg. The determination result after applying the correction factor shall
also meet this requirement.
When the total migration result is > 10.0mg/dm2 or 60.0mg/kg, the difference
between the three independent determination results obtained under
repeatability conditions and the arithmetic mean shall not exceed 30% of the
arithmetic mean. The determination result after applying the correction factor
shall also meet this requirement.
......
Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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