GB 31604.52-2021 PDF English
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National food safety standard - Food-contact materials and articles - Determination of migration of primary aromatic amine
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GB 31604.52-2021: National food safety standard - Food-contact materials and articles - Determination of migration of primary aromatic amine ---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/GB31604.52-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National food safety standard - Food contact material
and products - Determination of migration of primary
aromatic amine
Issued on. FEBRUARY 22, 2021
Implemented on. AUGUST 22, 2021
Issued by. National Health Commission of PRC;
State Administration for Market Regulation.
Table of Contents
1 Scope... 3
2 Principles... 3
3 Reagents and materials... 3
4 Instruments and equipment... 5
5 Analytical procedures... 5
6 Expression of analysis results... 8
7 Precision... 10
8 Others... 10
Appendix A The names, CAS numbers, molecular formulas of 29 aromatic
primary amines... 11
Appendix B Mass spectrometry reference conditions... 12
Appendix C Chromatograms of liquid chromatography-mass
spectrometry/mass total ion current (TIC) AND chromatograms of multiple
reaction monitoring (MRM) of 29 aromatic primary amines... 16
National food safety standard - Food contact material
and products - Determination of migration of primary
aromatic amine
1 Scope
This standard specifies the method for determining the migration of 29 aromatic
primary amines, in food contact materials and products.
This standard applies to the determination of the migration of aromatic primary
amines, in food contact materials and products.
2 Principles
After the migration test of food contact materials and products, according to GB
31604.1 and GB 5009.156, they are detected by liquid chromatography-mass
spectrometry/mass spectrometry. Among them, the food simulants, including 4%
acetic acid, 10% ethanol, 20% ethanol, 50% ethanol, AND the alternative
chemical solvents, that is, 95% ethanol, are filtered and injected directly. The
alternative chemical solvent isooctane is extracted by methanol-water solution;
then the water layer is filtered and injected. Use the peak area external standard
method for quantification.
3 Reagents and materials
The water is the grade 1 water, which is specified in GB/T 6682.
3.1 Reagents
3.2 Reagent preparation
3.2.1 Acidic and alcoholic food simulants and alternative chemical solvents.
Prepared according to GB 5009.156.
3.2.2 The 0.1% formic acid. Take 1 mL of formic acid (3.1.3) in a volumetric
flask; add water to make the volume reach to 1 L.
3.2.3 Methanol-water extract. Measure 50 mL of methanol (3.1.2) AND 50 mL
of water. Pipette 0.4 mL of glacial acetic acid (3.1.5). Mix it uniformly.
3.3 Standard substances
The 29 kinds of aromatic primary amines. Standard substances (see appendix
A), purity ≥ 98%; or standard substances that have been certified by the country
and awarded a standard material certificate.
3.4 Preparation of standard solution
3.4.1 The 29 kinds of standard stock solutions of aromatic primary amine (1000
mg/L). Accurately weigh 25 mg (accurate to 0.1 mg) of each of 29 kinds of
aromatic primary amine standard substances. Use methanol to dissolve them,
respectively. Transfer it into a 25 mL brown volumetric bottle. Use methanol to
dilute it to the mark. Seal and store it in a 4 °C refrigerator in the dark. The shelf
life is 1 month.
3.4.4 Preparation of standard working solution
3.4.4.1 Isooctane standard working solution
Accurately pipette 30 µL, 50 µL, 100 µL, 300 µL, 500 µL of the standard
intermediate solution B of aromatic primary amine (3.4.3), in a 10 mL volumetric
flask. Use isooctane to make the volume reach to the mark, to obtain the
standard working solution, which has an aromatic primary amine concentration
of 3.0 µg/L, 5.0 µg/L, 10.0 µg/L, 30.0 µg/L, 50.0 µg/L, respectively.
3.4.4.2 Standard working solutions for other food simulants and
alternative chemical solvents
Accurately pipette 30 µL, 50 µL, 100 µL, 300 µL, 500 µL of the standard
intermediate solution A (3.4.2) of aromatic primary amine, in a 10 mL volumetric
flask.
4 Instruments and equipment
4.1 Liquid chromatography tandem mass spectrometer. Electrospray ion source (ESI)
4.2 Analytical balance. Sensitivity is 0.0001 g.
4.3 Micro syringe. 10 µL, 100 µL, 1000 µL.
4.5 Vortex mixer.
4.6 Needle type nylon filter. Pore size 0.22 µm.
5 Analytical procedures
5.1 Preparation of food simulants
5.1.1 General
The migration test of this standard uses 4% acetic acid, 10% ethanol, 20%
ethanol, 50% ethanol food simulants, alternative chemical solvent (95%
ethanol), isooctane. Vegetable oil is not suitable for the determination of the
migration of aromatic primary amines.
5.1.2 Migration test
The condition selection and operation steps of the migration test are in
accordance with the provisions of GB 31406.1 and GB 5009.156.
5.1.3 Preparation of test solution
5.1.3.3 Preparation of blank test solution
Food simulants and alternative chemical solvents, which are not in contact with
food contact materials and products, are treated in accordance with 5.1.3.1 and
5.1.3.2, to obtain a blank test solution.
5.2 Instrument reference conditions
5.2.1 Liquid chromatography conditions
The liquid chromatography conditions are as follows.
5.2.2 Mass spectrometry conditions
The mass spectrometry conditions are as follows.
5.3 Drawing of standard curve
According to the instrument reference conditions listed in 5.2, the standard
working solution is determined. Use the concentration of the aromatic primary
amine in the standard working solution as the abscissa, the corresponding
quantitative ion peak area as the ordinate, to draw the standard curve, to obtain
the linear equation.
5.4 Determination of test solution
5.4.1 Qualitative determination
Determine the food simulant sample solution (5.1.3) and standard working
solution, according to the instrument reference condition (5.2). If the deviation
of the retention time of the mass chromatographic peak of the food simulant
sample solution and the standard solution is within ±2.5%;
5.4.2 Quantitative determination
Inject the test solution and the blank test solution (5.1.3) into the liquid
chromatography-mass spectrometer/mass spectrometer, to obtain the peak
area.
6 Expression of analysis results
6.1 Calculation of the specific migration of a single aromatic primary
amine in food contact materials and products of non-sealed products
(expressed in mg/kg)
6.2 Calculation of specific migration of single aromatic primary amine in
food contact materials and products of sealed products (expressed in
mg/kg)
6.3 Calculation of specific migration of single aromatic primary amine in
food contact materials and products of sealed products (expressed in
mg/piece)
7 Precision
The absolute difference between two independent determination results, which
are obtained under repeatability conditions, shall not exceed 10% of their
arithmetic mean.
8 Others
This method has a detection limit of 1.0 µg/kg AND a quantification limit of 3.0
µg/kg, for a single aromatic primary amine in food simulants, including 4%
acetic acid, 10% ethanol, 20% ethanol, 50% ethanol, alternative chemical
solvents (95% ethanol), isooctane.
...... Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al.
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