GB 31604.18-2016 English PDF

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GB 31604.18-2016: National food safety standard - Food contact materials and articles - Determination of migration of acrylamide
GB 31604.18-2016
Food contact materials--Polymer--Determination of acrylamide in food simulants--High performance liquid chromatography
National Standards of People's Republic of China
National food safety standards
Food contact materials and products
Determination of acrylamide migration
Published on.2016-10-19
2017-04-19 Implementation
China
National Health and Family Planning Commission released
Foreword
This standard replaces GB/T 23296.9-2009 Determination of acrylamide in food simulants for food contact materials and polymers
High Performance Liquid Chromatography.
Compared with GB/T 23296.9-2009, the main changes are as follows.
--- The name of the standard was revised as "Determination of migration of acrylamide in food contact materials and products of food safety national standards";
--- Increased the scope of application;
--- Modified food simulant preparation;
--- Modified the oil-based food simulant test solution processing.
National food safety standards
Food contact materials and products
Determination of acrylamide migration
1 Scope
This standard specifies the determination of the migration of acrylamide in food contact materials and products.
This standard applies to liquid chromatography detection of acrylamide migration in food contact materials and products.
2 principle
Food simulants for food contact materials and their products are tested using liquid chromatography, including water-based, acidic, and alcohol-based food molds.
Samples were directly injected, oil-based food simulants were sampled by water extraction, and fractionated by HPLC (Ion Exclusion Column).
The UV detector was used for detection. The method was calibrated using the external standard peak area method.
3 Reagents and materials
Unless otherwise stated, the reagents used in this method are of analytical grade, and the water is a grade one water according to GB/T 6682. Test container and transfer
Appliances should avoid plastic materials.
3.1 Reagents
3.1.1 Water-based, acidic, alcoholic, oil-based food simulants. The reagents used are in accordance with the provisions of GB 31604.1.
3.1.2 Acetonitrile (C2H3N). Chromatographically pure.
3.1.3 Methanol (CH3OH). Chromatographically pure.
3.1.4 Sulfuric acid (H2SO4). pure grade.
3.2 reagent preparation
3.2.1 water-based, acidic, alcoholic, oil-based food simulants. According to the intended use of the sample to be tested and the conditions of use, according to GB 5009.156
operating.
3.2.2 Sulfuric acid solution (0.0036 mol/L). Measure 0.1 mL of sulfuric acid, dilute to 500 mL with water, and mix.
3.3 Standards
Acrylamide (C3H5NO). purity ≥99%.
3.4 standard solution preparation
3.4.1 acrylamide standard stock solution (1000mg/L). Accurately weigh 10mg of acrylamide standard (accurate to 0.1mg).
The alcohol was brought to a volume of 10 mL and the stock solution was stored in a refrigerator at 0°C to 4°C.
3.4.2 acrylamide standard intermediate solution (10mg/L). Pipette 1.0mL acrylamide stock solution to 100mL with methanol.
4 Instruments and Equipment
4.1 High performance liquid chromatograph. equipped with a UV detector.
4.2 Analytical balance. Sensing amount 0.1mg and 0.01g.
4.3 Microporous filter. 0.2 μm.
4.4 plug colorimetric tube. 25mL.
5 Analysis steps
5.1 Preparation of test solution
5.1.1 Preparation of food simulant test solution
According to the intended use and the conditions of use of the sample to be tested, the migration test method and test in accordance with GB 5009.156 and GB 31604.1
Test conditions for the migration test. After the migration test was completed, the mimic of the migration test was thoroughly mixed and used for the following analysis.
5.1.2 Preparation of Water-based, Acidic, Alcoholic Food Simulator Test Solution
The food simulant test solution was filtered through a 0.2 μm microporous filter for measurement.
5.1.3 Preparation of oil-based food simulant test solution
Weigh 10g (accurate to 0.01g) oil-based food simulant test solution into the colorimetric tube, add 10.0mL water, shake vigorously for 1min, and set it aside.
Layered. The aqueous layer was taken off and filtered through a 0.2 μm filter for measurement.
5.1.4 Preparation of Blank Solutions
5.1.4.1 blank solutions for water-based, acidic, alcoholic food simulants
The food simulant not contacted with the sample was removed and filtered through a 0.2 μm microporous membrane for measurement.
5.1.4.2 Oil-based food simulant blank solution
Pipette 10g (accurate to 0.01g) of the food simulant that has not been contacted with the sample and operate according to 5.1.3.
5.1.5 standard working solution for water-based, acidic, alcoholic food simulants
Accurate absorption of acrylamide standard intermediate solution 0.00mL, 0.03mL, 0.05mL, 0.08mL, 0.1mL, 0.5mL in 10mL
In a volumetric flask, using a food simulant not in contact with the sample, the acrylamide concentration was 0.00 mg/L, 0.03 mg/L, respectively.
0.05mg/L, 0.08mg/L, 0.10mg/L, 0.50mg/L standard working solution. In the same way, with the corresponding water base, acid,
Alcoholic food simulants are formulated with the same concentration series of acrylamide standard working solutions.
5.1.6 Standard working solution for oil-based food simulants
Weigh 10g (accurate to 0.01g) of oil-based food simulants into 5 colorimetric tubes and draw the acrylamide standard intermediate solution.
(10mg/L) 0.00mL, 0.03mL, 0.05mL, 0.08mL, 0.1mL, 0.5mL in a colorimetric tube, mix, add 10.0mL of water,
Vibrate vigorously for 1 min and stand still. The acrylamide concentrations were 0.00 mg/kg, 0.03 mg/kg, 0.05 mg/kg, 0.08 mg/kg, respectively.
0.10mg/kg, 0.50mg/kg standard working solution. The aqueous layer was taken off and filtered through a 0.2 μm filter for measurement.
5.2 Determination
5.2.1 Liquid Chromatography Conditions
a) Column. VenusilCIS, ion exclusion column, column length 250 mm, inner diameter 4.6 mm, particle size 5 μm, or equivalent;
b) mobile phase. sulfuric acid solution. acetonitrile (91 9);
c) Flow rate. 0.5mL/min;
d) Column temperature. 50°C;
e) UV detector. wavelength 198nm;
f) Injection volume. 20 μL.
5.2.2 Chromatographic determination
The standard solution and the sample solution were measured by sequential injection, and the concentration of acrylamide in the standard working solution was plotted as the abscissa, and the unit was “mg/L or
Mg/kg” indicates that the corresponding peak area is plotted on the ordinate, and a standard curve is drawn. Qualitatively using the retention time and external standard method for quantitation.
The acrylamide retention time is 11.6 minutes. See Appendix A for the chromatograms.
The regression parameters are calculated according to equation (1).
y=a×xb (1)
In the formula.
y--- peak area of acrylamide in the standard working solution of the food simulant;
a---the slope of the regression curve;
x - the concentration of acrylamide in the standard working solution of the food simulant in milligrams per liter or milligrams per kilogram (mg/L or mg/kg);
b --- The intercept of the regression curve.
6 Expression of analysis results
The concentration of acrylamide in the sample solution was obtained from the standard curve, and the migration amount was calculated according to GB 5009.156 to obtain food contact materials.
Amount of acrylamide migration in products. The calculation result is retained to two decimal places.
7 Precision
The absolute difference between two independent determinations obtained under repeated conditions must not exceed 10%.
8 Others
The detection limit of acrylamide in water-based, acidic, and alcoholic food simulants was 0.01 mg/L.
The detection limit of enamide was 0.01 mg/kg.
The quantification limit of acrylamide in water-based, acidic, and alcoholic food simulants was 0.03 mg/L, and C in oil-based food simulants
The limit of quantification of enamide was 0.03 mg/kg.
Appendix A
Standard solution chromatogram
A.1 Standard HPLC chromatogram of acrylamide in n-hexane simulants
The standard liquid chromatogram of acrylamide in the n-hexane simulant is shown in Figure A.1.
Figure A.1 Standard HPLC chromatogram of acrylamide in n-hexane simulants (0.05 mg/L)
A.2 Standard liquid chromatogram of acrylamide in 10% ethanol simulants
The standard liquid chromatogram of acrylamide in the 10% ethanol simulant is shown in Figure A.2.
Figure A.2 Standard chromatogram of acrylamide in 10% ethanol simulant (0.05 mg/L)
A.3 Standard liquid chromatogram of acrylamide in 20% ethanol simulants
The standard liquid chromatogram of acrylamide in the 20% ethanol simulant is shown in Figure A.3.
Figure A.3 Standard liquid chromatogram of acrylamide in a 20% ethanol mimic (0.05 mg/L)
A.4 Standard liquid chromatogram of acrylamide in 50% ethanol simulants
The standard liquid chromatogram of acrylamide in the 50% ethanol mimic is shown in Figure A.4.
Figure A.4 Standard chromatogram of acrylamide in a 50% ethanol mimic (0.05 mg/L)
A.5 Standard HPLC chromatogram of acrylamide in 5 % acetic acid simulants
The standard liquid chromatogram of acrylamide in the 4% acetic acid simulant is shown in Figure A.5.
Figure A.5 Standard chromatogram of acrylamide in 4% acetic acid mimic (0.05 mg/L)