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GB 31604.51-2021 (GB31604.51-2021)

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GB 31604.51-2021: PDF in English
GB 31064.51-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S 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 μL 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 μm 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 μm.
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);
......
(Above excerpt was released on 2021-09-03, modified on 2021-09-03, translated/reviewed by: Wayne Zheng et al.)
Source: https://www.chinesestandard.net/PDF.aspx/GB31604.51-2021