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GB 31604.58-2023: National food safety standard - Food contact materials and products - Determination of migration of nine antioxidants
GB 31604.58-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Nine
Antioxidants
ISSUED ON. SEPTEMBER 06, 2023
IMPLEMENTED ON. MARCH 06, 2024
Issued by. National Health Commission of the People’s Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope... 3
2 Principle... 3
3 Reagents and Materials... 3
4 Instruments and Equipment... 5
5 Analytical Procedure... 5
6.Expression of Analytical Results... 7
7 Precision... 9
8 Others... 9
9 Principle... 10
10 Reagents and Materials... 10
11 Apparatus... 12
12 Analytical Procedures... 12
13 Expression of Analytical Results... 14
14 Precision... 14
15 Others... 14
Appendix A Relevant Information of Standard Products of 9 Antioxidants... 16
Appendix B High Performance Liquid Chromatogram of 9 Antioxidants... 17
Appendix C Mass Spectrometry Reference Conditions... 18
Appendix D Total Ion Current (TIC) Chromatograms of Liquid Chromatography-
Tandem Mass Spectrometry of 9 Antioxidants... 19
Appendix E Multiple Reaction Monitoring (MRM) Spectra of Liquid
Chromatography-Tandem Mass Spectrometry of 9 Antioxidants... 20
National Food Safety Standard - Food Contact Materials
and Products - Determination of Migration of Nine
Antioxidants
1 Scope
This Standard specifies methods for the determination of migration of nine antioxidants in food
contact materials and products.
This Standard applies to the determination of migration of antioxidant 2246, antioxidant 264,
butylated hydroxyanisole (BHA), 2,4-di-tert-butylphenol, antioxidant 425, antioxidant 300,
antioxidant 1010, antioxidant 1076, and antioxidant 168.
Method-I High Performance Liquid Chromatography
2 Principle
After food contact materials and products undergo migration tests in accordance with GB
31604.1 and GB 5009.156, high performance liquid chromatography is used for detection.
Among them, after filtration of water, 4% (volume fraction) acetic acid, 10% (volume fraction)
ethanol, 20% (volume fraction) ethanol, 50% (volume fraction) ethanol food simulant and
chemical alternative solvent 95% (volume fraction) ethanol soaking solution, the sample is
injected directly. After the nitrogen blowing of the chemical alternative solvent isooctane
soaking solution, dissolve it in methanol; and then inject the sample. Detect by UV detector or
diode array detector, and quantified by peak area external standard method.
3 Reagents and Materials
Unless otherwise stated, all reagents are chromatographically pure. The water is Class-I water
specified in GB/T 6682.During the test, plastic materials shall be avoided as much as possible
for containers and transfer equipment.
3.1 Reagents
3.1.1 Foods containing ethanol, acidic food simulants and chemical alternative solvents. the
reagents used must comply with the provisions of GB 5009.156.
3.1.2 Methanol (CH4O).
3.1.3 Ethyl acetate (C4H8O2).
3.2 Preparation of reagent
Foods containing ethanol, acidic food simulants and chemical alternative solvents. Prepared
according to the requirements of GB 5009.156.
3.3 Standard product
9 antioxidant standard products (see Table A.1 in Appendix A), with purity ≥98%, or standard
products certified by the country and awarded a reference material certificate.
3.4 Preparation of standard solution
3.4.1 9 Antioxidant standard stock solutions (1000 mg/L). Accurately weigh 25mg of each of
the 9 antioxidant standard products (accurate to 0.1mg); dissolve them in 1mL of ethyl acetate.
And then transfer to 9 pieces of 25mL brown volumetric flask; and make constant volume by
adding methanol and shake well. Transfer the solution to a brown glass container and store it
in an airtight container away from light in a 4°C refrigerator. The shelf life is 6 months.
3.4.2 9 antioxidant standard intermediate solution A (solvent is methanol). Accurately pipet
2.50mL of each of BHA and antioxidant 300 standard stock solutions, and 5.00mL of each of
the other 7 antioxidants standard stock solutions into the same 50mL brown volumetric flask;
make constant volume by methanol to obtain standard intermediate solution A of BHA and
antioxidant 300 with mass concentration of 50.0 mg/L, and of the other 7 antioxidants with the
mass concentration of 100 mg/L. Transfer the solution to a brown glass container and store it
in an airtight container away from light in a 4°C refrigerator. The storage period is 3 months.
3.4.3 9 antioxidant standard intermediate solution B (solvent is ethyl acetate). Accurately pipet
2.50mL of each of BHA and antioxidant 300 standard stock solutions, and 5.00mL of each of
the other 7 standard stock solutions into the same 50mL brown volumetric flask; make constant
volume by ethyl acetate to obtain a standard intermediate solution B of BHA and antioxidant
300 with mass concentration of 50 mg/L, and the other 7 antioxidants with mass concentration
of 100 mg/L. Transfer the solution to a brown glass container and store it in an airtight container
away from light in a 4°C refrigerator. The storage period is 3 months.
3.4.4 Preparation of standard working solution
3.4.4.1 Chemical alternative solvent isooctane standard working solution
Accurately transfer 0.03mL, 0.1mL, 0.3mL, 1mL, and 3mL of 9 antioxidant standard
intermediate solutions B into 5 pieces of 10mL volumetric flasks; and make constant volume
with isooctane to obtain the standard working solutions of BHA and antioxidant 300 with mass
concentration of 0.15 mg/L, 0.50 mg/L, 1.5mg/L, 5mg/L, 15mg/L, respectively; and other 7
antioxidants with the mass concentration of 0.30mg/L, 1.0mg/L, 3.0mg/L, 10mg/ L, 30mg/L,
respectively. Accurately transfer 2.00mL of each standard working solution into 5 pieces of
10mL test tubes; blow with nitrogen at 40°C until nearly dry; then add 2.00mL of methanol to
dissolve. Vortex and shake to reconstitute; and filter through a needle nylon filter; and then
waiting to be measured on the machine.
3.4.4.2 Standard working solution of other food simulants and chemical alternative
solvents 95% (volume fraction) ethanol
Accurately transfer 0.03mL, 0.1mL, 0.3mL, 1mL, and 3mL of 9 antioxidant standard
intermediate solutions A into 5 pieces of 10mL volumetric flasks; and make constant volume
with 10% ethanol; and obtain the standard working solution of BHA and antioxidant 300 with
mass concentrations of 0.15mg/L, 0.50mg/L, 1.5 mg/L, 5 mg/L, 15 mg/L, respectively; and
other 7 antioxidants with mass concentrations of 0.30 mg/L, 1.0 mg/L, and 3.0mg/L, 10mg/L,
30mg/L, respectively. Using the same method, prepare 9 antioxidant standard working solutions
of the same concentration series by water, 4% acetic acid, 10% ethanol, 20% ethanol, 50%
ethanol food simulant and chemical alternative solvent 95% ethanol. Take 1 mL of each
standard working solution; filter it through a needle nylon filter; and then wait for measurement
on the machine.
4 Instruments and Equipment
4.1 High performance liquid chromatograph. Equipped with UV detector or diode array detector.
4.2 Analytical balance. Sensitivity is 0.0001g.
4.3 Nitrogen blowing concentrator.
4.4 Glass micro-syringe. 10μL, 100μL and 1000μL.
4.5 Thermostatic equipment.
4.6 Vortex oscillator.
4.7 Needle nylon filter. Pore size is 0.22μm.
5 Analytical Procedure
5.1 Preparation of test solution
5.1.1 Migration test
Food contact materials and produ...