GB 31604.58-2023 National food safety standard - Food contact materials and products - Determination of migration of nine antioxidants (English Version)
1 Scope
This standard specifies the determination method of migration of 9 antioxidants in food contact materials and articles.
This standard is applicable to the determination of migration of antioxidant 2246, antioxidant 264, butyl hydroxyanisole (BHA), 2,4-di-tert-butylphenol, antioxidant 425, antioxidant 300, antioxidant 1010, antioxidant 1076 and antioxidant 168 in food contact materials and articles plastics, such as rubber, coatings, adhesives, inks, paper and paperboard.
Method I High performance liquid chromatography
2 Principle
The food contact materials and articles shall be subjected to test using high performance liquid chromatography after migration test according to GB 31604.1 and GB 5009.156. During test, water, 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol, 50% (volume fraction) ethanol-containing food simulants, and 95% (volume fraction) ethanol immersion solution of chemical alternative solvent are filtered and directly injected. The chemical alternative solvent isooctane immersion solution is dissolved in methanol after nitrogen blowing before injection. The contents are detected by ultraviolet detector or diode array detector, and are quantified by peak area external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents used are chromatographically pure. Class-I water specified in GB/T 6682 is adopted. The containers and transfer instruments during the test shall not be made of plastic materials.
3.1 Reagents
3.1.1 Ethanol-containing food simulants, acidic food simulants and chemical alternative solvents: the reagents used shall be in accordance with the requirements of GB 5009.156.
3.1.2 Methanol (CH4O).
3.1.3 Ethyl acetate (C4H8O2).
3.2 Preparation of reagents
Ethanol-containing food simulants, acidic food simulants and chemical alternative solvents: the reagents used shall be prepared in accordance with the provisions of GB 5009.156.
3.3 Standard sample
9 antioxidants standard samples (see Table A.1 in Annex A), with a purity of ≥98%; or standard material certified by the state and granted with standard material certificate.
3.4 Preparation of standard solutions
3.4.1 Standard stock solutions of 9 antioxidants (1,000 mg/L): accurately weigh 25 mg (accurate to 0.1 mg) of 9 antioxidants respectively, dissolve them with 1 mL ethyl acetate and transfer into nine 25 mL brown volumetric flasks, dilute to the scale with methanol, and then shake well. Transfer the solution to a brown glass bottle and store it at 4°C in refrigerator away from light for 6 month.
3.4.2 9 antioxidants standard intermediate solution A (solvent is methanol): accurately pipette 2.50 mL of BHA and antioxidant 300 standard stock solution, 5.00 mL of other 7 antioxidant standard stock solution in the same 50 mL brown volumetric flask, and dilute to the scale with methanol, thus obtaining standard intermediate solution A with 50 mg/L of BHA and antioxidant 300 and 100 mg/L of other 7 antioxidants. Transfer the solution to a brown glass bottle and store it at 4°C in refrigerator away from light for 3 month.
3.4.3 9 antioxidants standard intermediate solution B (solvent is ethyl acetate): accurately pipette 2.50 mL of BHA and antioxidant 300 standard stock solution, 5.00 mL of other 7 antioxidant standard stock solution in the same 50 mL brown volumetric flask, and dilute to the scale with ethyl acetate, thus obtaining standard intermediate solution B with 50 mg/L of BHA and antioxidant 300 and 100 mg/L of other 7 antioxidants. Transfer the solution to a brown glass bottle and store it at 4°C in refrigerator away from light for 3 month.
3.4.4 Preparation of standard working solution
3.4.4.1 Standard working solution of chemical alternative solvent isooctane
Accurately pipette 9 antioxidants standard intermediate solutions B (0.03 mL, 0.1 mL, 0.3 mL, 1 mL, 3 mL) into five 10 mL volumetric flasks respectively, and dilute to the scale with isooctane, thus obtaining standard working solution with 0.15 mg/L, 0.50 mg/L, 1.5 mg/L, 5 mg/L and 15 mg/L of BHA and antioxidant 300 and 0.30 mg/L, 1.0 mg/L, 3.0 mg/L, 10 mg/L, 30 mg/L of other 7 antioxidants. Accurately pipette 2.00 mL of each standard working solution to five 10 mL test tubes, blow to dry at 40°C by termovap sample concentrator, then accurately add 2.00 mL of methanol for dissolution, shake it with a vortex oscillator for re dissolution, filter through pin type nylon filter, and wait for determination on the analyzer.
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and equipment
5 Analysis procedures
6 Expression of analysis results
7 Precision
8 Others
9 Principle
10 Reagents and materials
11 Instruments and equipment
12 Analysis procedures
13 Expression of analysis results
14 Precision
15 Others
Annex A Relevant information on 9 antioxidants standard samples
Annex B High performance liquid chromatogram of 9 antioxidants
Annex C Mass spectrometry reference conditions
Annex D Liquid chromatography-tandem mass spectrometry total ion flow (TIC) chromatogram of 9 antioxidants
Annex E Liquid chromatography-tandem mass spectrometry multi-reaction monitoring (MRM) spectra of 9 antioxidants
Standard
GB 31604.58-2023 National food safety standard - Food contact materials and products - Determination of migration of nine antioxidants (English Version)
Standard No.
GB 31604.58-2023
Status
valid
Language
English
File Format
PDF
Word Count
11000 words
Price(USD)
258.0
Implemented on
2024-9-6
Delivery
via email in 1 business day
Detail of GB 31604.58-2023
Standard No.
GB 31604.58-2023
English Name
National food safety standard - Food contact materials and products - Determination of migration of nine antioxidants
1 Scope
This standard specifies the determination method of migration of 9 antioxidants in food contact materials and articles.
This standard is applicable to the determination of migration of antioxidant 2246, antioxidant 264, butyl hydroxyanisole (BHA), 2,4-di-tert-butylphenol, antioxidant 425, antioxidant 300, antioxidant 1010, antioxidant 1076 and antioxidant 168 in food contact materials and articles plastics, such as rubber, coatings, adhesives, inks, paper and paperboard.
Method I High performance liquid chromatography
2 Principle
The food contact materials and articles shall be subjected to test using high performance liquid chromatography after migration test according to GB 31604.1 and GB 5009.156. During test, water, 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol, 20% (volume fraction) ethanol, 50% (volume fraction) ethanol-containing food simulants, and 95% (volume fraction) ethanol immersion solution of chemical alternative solvent are filtered and directly injected. The chemical alternative solvent isooctane immersion solution is dissolved in methanol after nitrogen blowing before injection. The contents are detected by ultraviolet detector or diode array detector, and are quantified by peak area external standard method.
3 Reagents and materials
Unless otherwise specified, all reagents used are chromatographically pure. Class-I water specified in GB/T 6682 is adopted. The containers and transfer instruments during the test shall not be made of plastic materials.
3.1 Reagents
3.1.1 Ethanol-containing food simulants, acidic food simulants and chemical alternative solvents: the reagents used shall be in accordance with the requirements of GB 5009.156.
3.1.2 Methanol (CH4O).
3.1.3 Ethyl acetate (C4H8O2).
3.2 Preparation of reagents
Ethanol-containing food simulants, acidic food simulants and chemical alternative solvents: the reagents used shall be prepared in accordance with the provisions of GB 5009.156.
3.3 Standard sample
9 antioxidants standard samples (see Table A.1 in Annex A), with a purity of ≥98%; or standard material certified by the state and granted with standard material certificate.
3.4 Preparation of standard solutions
3.4.1 Standard stock solutions of 9 antioxidants (1,000 mg/L): accurately weigh 25 mg (accurate to 0.1 mg) of 9 antioxidants respectively, dissolve them with 1 mL ethyl acetate and transfer into nine 25 mL brown volumetric flasks, dilute to the scale with methanol, and then shake well. Transfer the solution to a brown glass bottle and store it at 4°C in refrigerator away from light for 6 month.
3.4.2 9 antioxidants standard intermediate solution A (solvent is methanol): accurately pipette 2.50 mL of BHA and antioxidant 300 standard stock solution, 5.00 mL of other 7 antioxidant standard stock solution in the same 50 mL brown volumetric flask, and dilute to the scale with methanol, thus obtaining standard intermediate solution A with 50 mg/L of BHA and antioxidant 300 and 100 mg/L of other 7 antioxidants. Transfer the solution to a brown glass bottle and store it at 4°C in refrigerator away from light for 3 month.
3.4.3 9 antioxidants standard intermediate solution B (solvent is ethyl acetate): accurately pipette 2.50 mL of BHA and antioxidant 300 standard stock solution, 5.00 mL of other 7 antioxidant standard stock solution in the same 50 mL brown volumetric flask, and dilute to the scale with ethyl acetate, thus obtaining standard intermediate solution B with 50 mg/L of BHA and antioxidant 300 and 100 mg/L of other 7 antioxidants. Transfer the solution to a brown glass bottle and store it at 4°C in refrigerator away from light for 3 month.
3.4.4 Preparation of standard working solution
3.4.4.1 Standard working solution of chemical alternative solvent isooctane
Accurately pipette 9 antioxidants standard intermediate solutions B (0.03 mL, 0.1 mL, 0.3 mL, 1 mL, 3 mL) into five 10 mL volumetric flasks respectively, and dilute to the scale with isooctane, thus obtaining standard working solution with 0.15 mg/L, 0.50 mg/L, 1.5 mg/L, 5 mg/L and 15 mg/L of BHA and antioxidant 300 and 0.30 mg/L, 1.0 mg/L, 3.0 mg/L, 10 mg/L, 30 mg/L of other 7 antioxidants. Accurately pipette 2.00 mL of each standard working solution to five 10 mL test tubes, blow to dry at 40°C by termovap sample concentrator, then accurately add 2.00 mL of methanol for dissolution, shake it with a vortex oscillator for re dissolution, filter through pin type nylon filter, and wait for determination on the analyzer.
Contents of GB 31604.58-2023
1 Scope
2 Principle
3 Reagents and materials
4 Instruments and equipment
5 Analysis procedures
6 Expression of analysis results
7 Precision
8 Others
9 Principle
10 Reagents and materials
11 Instruments and equipment
12 Analysis procedures
13 Expression of analysis results
14 Precision
15 Others
Annex A Relevant information on 9 antioxidants standard samples
Annex B High performance liquid chromatogram of 9 antioxidants
Annex C Mass spectrometry reference conditions
Annex D Liquid chromatography-tandem mass spectrometry total ion flow (TIC) chromatogram of 9 antioxidants
Annex E Liquid chromatography-tandem mass spectrometry multi-reaction monitoring (MRM) spectra of 9 antioxidants
