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GB 31604.51-2021 English PDF (GB31604.51-2021)

GB 31604.51-2021 English PDF (GB31604.51-2021)

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GB 31604.51-2021: National food safety standard - Food-contact materials and articles - Determination of migration of 1,4-butanediol

This standard specifies the method for determining the migration of 1,4-butanediol in food contact materials and products. This standard applies to the determination of migration of 1,4-butanediol, in plastics, coatings, food contact materials and products, which use adhesives and inks.
GB 31064.51-2021
GB
NATIONAL STANDARD OF THE
PEOPLE REPUBLIC OF CHINA
National food safety standard - Food contact material
and products - Determination of migration of 1,4-
butanediol
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 Principle ... 3
3 Reagents and materials ... 3
4 Instrument and equipment ... 5
5 Analytical procedures ... 5
6 Expression of analysis results ... 7
7 Precision ... 9
8 Others ... 9
Appendix A Chromatogram of 1,4-butanediol standard solution ... 10
National food safety standard - Food contact material
and products - Determination of migration of 1,4-
butanediol
1 Scope
This standard specifies the method for determining the migration of 1,4- butanediol in food contact materials and products.
This standard applies to the determination of migration of 1,4-butanediol, in plastics, coatings, food contact materials and products, which use adhesives and inks.
2 Principle
Food contact materials and products are immersed in food simulants OR
alternative solvents. The 1,4-butanediol migrates into the food simulants. The migration amount of 1,4-butanediol in the food simulants is determined. For the water-based, acidic and alcoholic food simulants, it is tested after being diluted by methanol. For the oily food simulants, it is tested after being extracted by methanol. The test solution is separated by a gas chromatographic column; detected by a gas chromatograph, which is equipped with a flame ionization detector (FID). The retention time is used for qualitative, whilst the external standard method is used for quantification.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are all analytically pure; the water is the grade 1 water, as specified in GB/T 6682.
3.1 Reagents
3.1.1 Olive oil: It must meet the requirements of Appendix A in GB 5009.156. 3.1.2 Acetic acid (C2H4O2).
3.1.3 Ethanol (C2H6O).
standard intermediate solution 1 (3.4.2), into six 10 mL volumetric flasks. Respectively, accurately add 2.0 mL of corresponding food simulants. Use methanol to make its volume accurately reach to the mark. Shake well. Let stand. It gets the standard working solutions, which have mass concentrations of 0.20 mg/L, 0.40 mg/L, 0.60 mg/L, 0.80 mg/L, 1.00 mg/L, 2.00 mg/L. Prepare it before use.
3.4.4.2 Standard working solution (oily food simulant)
Respectively, accurately weigh 2.0 g (accurate to 0.001 g) of oily food simulant (olive oil) into six centrifuge tubes with stoppers. Respectively add 50 ??L of 6 standard intermediate solution 2 (3.4.3) of oily food simulant, at different mass concentrations. Shake well. Let it stand, to obtain standard working solutions, which have mass concentrations of 1.0 mg/kg, 2.0 mg/kg, 3.0 mg/kg, 4.0 mg/kg, 5.0 mg/kg, 10.0 mg/kg. Respectively add 2.00 mL of methanol solution for extraction. Mix well. Centrifuge for layering. Take the upper layer solution. Make it pass through a 0.45 ??m filter membrane. Prepare for testing.
3.4.4.3 Standard working solution [Alternative solvent (95% ethanol)]
Accurately pipette 0.20 mL, 0.40 mL, 0.60 mL, 0.80 mL, 1.00 mL, 2.00 mL of standard intermediate solution 1 (3.4.2), into six 10 mL volumetric flasks. Respectively, accurately add 2.0 mL of 95% ethanol food simulant. Use
methanol to make its volume reach accurately to the mark. Shake it well. Let it stand, to obtain the standard working solution, which has mass concentrations of 0.20 mg/L, 0.40 mg/L, 0.60 mg/L, 0.80 mg/L, 1.00 mg/L, 2.00 mg/L,
respectively. Prepare it before use.
4 Instrument and equipment
4.1 Gas chromatograph: It is equipped with hydrogen flame ionization detector (FID).
4.2 Analytical balance: The sensitivity is 0.1 mg and 1 mg.
4.3 Organic phase microporous filter membrane: 0.45 ??m.
4.4 Centrifuge: The maximum speed is > 3000 r/min.
5 Analytical procedures
5.1 Preparation of test solution
5.1.1 Migration test
5.2.5 Flow rate: 1 mL/min.
5.2.6 Detector (FID) temperature: 260 ??C; hydrogen flow rate: 30 mL/min; air flow rate: 400 mL/min.
5.3 Drawing of standard curve
Determine the standard working solution, in accordance with the instrument reference conditions, which are listed in 5.2. Use the mass concentration of 1,4- butanediol in the standard working solution, as the abscissa, AND the response value of the corresponding peak area, as the ordinate, to draw the standard curve. Refer to Appendix A for the reference chromatogram of 1,4-butanediol, in the food simulant standard solution.
5.4 Determination of test solution
According to the instrument reference conditions listed in 5.3, the sample solution (5.1.2) and the blank solution (5.1.3) are respectively determined, to obtain the peak area of the target object. From the standard curve, calculate the content of the 1,4-butanediol, c and c0, in the sample solution and the blank solution. The content of the 1,4-butanediol, c0, in the blank solution shall not be higher than the mass concentration of the method detection limit.
Note: As the specimen contains a small amount of water, it is recommended to maintain the equipment regularly, based on actual testing conditions.
6 Expression of analysis results
6.1 Calculation of specific migration of 1,4-butanediol in food contact materials and products (expressed in mg/kg)
When the specific migration of 1,4-butanediol in food contact materials and products is expressed in mg/kg, it is calculated according to formula (1). Where:
X - The specific migration of 1,4-butanediol, in milligrams per kilogram (mg/kg);
c - The content of 1,4-butanediol in the specimen soaking solution, in
milligrams per liter (mg/L) or milligrams per kilogram (mg/kg);
c0 - The content of 1,4-butanediol in the blank soaking solution, in milligrams per liter (mg/L) or milligrams per kilogram (mg/kg);

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