Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces GB/T 23296.9-2009 Food Contact Materials - Polymer - Determination of Acrylamide in Food Simulants - High Performance Liquid Chromatography.
The following main changes have been made with respect to GB/T 23296.9-2009 (the previous edition):
——This standard is renamed as National Food Safety Standard - Food Contact Materials and Articles - Determination of Migration of Acrylamide;
——Application scope is added;
——Preparation of food simulants is modified;
——Treatment process of oil-based food simulant test solution is modified.
National Food Safety Standard
Food Contact Materials and Articles
Determination of Migration of Acrylamide
1 Scope
This standard specifies the determination of migration of acrylamide in food contact materials and articles.
This standard is applicable to the detection of migration of acrylamide in food contact materials and articles by liquid chromatography.
2 Principle
Detect the food simulants of food contact materials and articles by liquid chromatography, directly inject the sample of water-based, acidic and alcoholic food simulants, inject the sample of oil-based food simulant after water extraction, separate through high performance liquid chromatograph (with ion exclusion column), detect with ultraviolet detector, and carry out quantitative determination by external standard peak area method.
3 Reagents and Materials
Unless otherwise specified, analytically-pure reagents and Class-I water (defined in GB/T 6682) are adopted for the purpose of this method. Containers and transfer appliances in test shall not be made of plastic materials.
3.1 Reagents
3.1.1 Water-based, acidic, alcoholic and oil-based food simulants: the reagents used shall be in accordance with the requirements of GB 31604.1.
3.1.2 Acetonitrile (C2H3N): chromatographically pure.
3.1.3 Methanol (CH3OH): chromatographically pure.
3.1.4 Sulfuric acid (H2SO4): guaranteed reagent.
3.2 Reagent preparation
3.2.1 Water-based, acidic, alcoholic and oil-based food simulants: prepare according to GB 5009.156 as well as the intended use and service conditions of to-be-tested sample.
3.2.2 Sulphuric acid solution (0.0036 mol/L): measure 0.1 mL sulfuric acid, scale the volume with water to 500 mL and mix well.
3.3 Standard product
Acrylamide (C3H5NO): with purity≥99%.
3.4 Preparation of standard solutions
3.4.1 Acrylamide standard stock solution (1000 mg/L): accurately weigh 10 mg (accurate to 0.1 mg) acrylamide standard, scale the volume to 10 mL with methanol, keep the stock solution in 0℃~4℃ refrigerator.
3.4.2 Acrylamide standard intermediate solution (10 mg/L): pipet 1.0 mL acrylamide stock solution and scale the volume to 100 mL with methanol.
4 Instruments and Apparatus
4.1 High performance liquid chromatograph: equipped with ultraviolet detector.
4.2 Analytical balance: with sensibility of 0.1 mg and 0.01 g.
4.3 Microporous filter membrane: 0.2 μm.
4.4 Colorimetric tube with stopper: 25 mL.
5 Analysis Steps
5.1 Preparation of test solutions
5.1.1 Preparation of food simulant test solution
Carry out migration test according to the intended use and service conditions of to-be-tested sample and the migration test methods and conditions specified in GB 5009.156 and GB 31604.1. After completion of the migration test, mix the simulants obtained from migration test sufficiently well for the next analysis.
5.1.2 Preparation of water-based, acidic and alcoholic food simulants test solution
Filter the food simulant test solution with 0.2 μm microporous filter membrane for determination.
5.1.3 Preparation of oil-based food simulant test solution
Weigh 10 g (accurate to 0.01 g) oil-based food simulant test solution into the colorimetric tube, add 10.0 mL water, violently oscillate for 1 min, and keep it still until layering. Filter the lower water solution with 0.2 μm filter membrane for determination.
5.1.4 Preparation of blank solution
5.1.4.1 Water-based, acidic and alcoholic food simulants blank solution
Transfer the food simulant not in contact with the sample and filter with 0.2 μm microporous filter membrane for determination.
5.1.4.2 Oil-based food simulant blank solution
Transfer 10 g (accurate to 0.01 g) food simulant not in contact with the sample and operate according to 5.1.3.
5.1.5 Water-based, acidic and alcoholic food simulants standard working solution
Accurately pipet 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL and 0.5 mL acrylamide standard intermediate solutions into 10mL-volumetric flasks, then scale the volume with food simulant not in contact with the sample to obtain the standard working solutions with the concentrations of acrylamide of 0.00 mg/L, 0.03 mg/L, 0.05 mg/L, 0.08 mg/L, 0.10 mg/L and 0.50 mg/L respectively. In the same way, prepare acrylamide standard working solution with the same concentration series with corresponding water-based, acidic and alcoholic food simulants respectively.
5.1.6 Oil-based food simulant standard working solution
Weigh 10 g (accurate to 0.01 g) oil-based food simulants and put into five colorimetric tubes respectively, pipet 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL and 0.5 mL acrylamide standard intermediate solutions (10 mg/L) into the colorimetric tubes and mix well, add 10.0 mL water, violently oscillate for 1 min and keep it still until layering to obtain the standard working solutions with the concentrations of acrylamide of 0.00 mg/kg, 0.03 mg/kg, 0.05 mg/kg, 0.08 mg/kg, 0.10 mg/kg and 0.50 mg/kg. Filter the lower water solution with 0.2 μm filter membrane for determination.
5.2 Determination
5.2.1 Liquid chromatographic conditions
a) Chromatographic column: Venusil CIS ion-exclusion chromatographic column with length of 250 mm, inside diameter of 4.6 mm and particle size of 5 μm, or equivalent;
b) Mobile phase: sulfuric acid solution: acetonitrile (91+9);
c) Flow rate: 0.5 mL/min;
d) Column temperature: 50℃;
e) Ultraviolet detector: with wavelength of 198 nm;
f) Sample injection amount: 20 μL.
5.2.2 Chromatographic determination
Inject the standard solution and sample solution in sequence for determination, plot the standard curve with the concentration of acrylamide in the standard working solution as x-axis (in mg/L or mg/kg) and the corresponding peak area of acrylamide as y-axis. Carry out the qualitative determination by retention time and quantitative determination by external standard method. Under the above chromatographic conditions, the retention time of acrylamide is 11.6 min, see Annex A for the chromatogram of acrylamide.
The regression parameter is calculated according to Formula (1):
y=a×x+b (1)
Where,
y——the peak area of acrylamide in food simulant standard working solution;
a——the slope of regression curve;
x——the concentration of acrylamide in the food simulant standard working solution, mg/L or mg/kg;
b——the intercept of regression curve.
Foreword i
1 Scope
2 Principle
3 Reagents and Materials
4 Instruments and Apparatus
5 Analysis Steps
6 Expression of Analysis Results
7 Accuracy
8 Other
Annex A Chromatogram of Standard Solution
Codeofchina.com is in charge of this English translation. In case of any doubt about the English translation, the Chinese original shall be considered authoritative.
This standard replaces GB/T 23296.9-2009 Food Contact Materials - Polymer - Determination of Acrylamide in Food Simulants - High Performance Liquid Chromatography.
The following main changes have been made with respect to GB/T 23296.9-2009 (the previous edition):
——This standard is renamed as National Food Safety Standard - Food Contact Materials and Articles - Determination of Migration of Acrylamide;
——Application scope is added;
——Preparation of food simulants is modified;
——Treatment process of oil-based food simulant test solution is modified.
National Food Safety Standard
Food Contact Materials and Articles
Determination of Migration of Acrylamide
1 Scope
This standard specifies the determination of migration of acrylamide in food contact materials and articles.
This standard is applicable to the detection of migration of acrylamide in food contact materials and articles by liquid chromatography.
2 Principle
Detect the food simulants of food contact materials and articles by liquid chromatography, directly inject the sample of water-based, acidic and alcoholic food simulants, inject the sample of oil-based food simulant after water extraction, separate through high performance liquid chromatograph (with ion exclusion column), detect with ultraviolet detector, and carry out quantitative determination by external standard peak area method.
3 Reagents and Materials
Unless otherwise specified, analytically-pure reagents and Class-I water (defined in GB/T 6682) are adopted for the purpose of this method. Containers and transfer appliances in test shall not be made of plastic materials.
3.1 Reagents
3.1.1 Water-based, acidic, alcoholic and oil-based food simulants: the reagents used shall be in accordance with the requirements of GB 31604.1.
3.1.2 Acetonitrile (C2H3N): chromatographically pure.
3.1.3 Methanol (CH3OH): chromatographically pure.
3.1.4 Sulfuric acid (H2SO4): guaranteed reagent.
3.2 Reagent preparation
3.2.1 Water-based, acidic, alcoholic and oil-based food simulants: prepare according to GB 5009.156 as well as the intended use and service conditions of to-be-tested sample.
3.2.2 Sulphuric acid solution (0.0036 mol/L): measure 0.1 mL sulfuric acid, scale the volume with water to 500 mL and mix well.
3.3 Standard product
Acrylamide (C3H5NO): with purity≥99%.
3.4 Preparation of standard solutions
3.4.1 Acrylamide standard stock solution (1000 mg/L): accurately weigh 10 mg (accurate to 0.1 mg) acrylamide standard, scale the volume to 10 mL with methanol, keep the stock solution in 0℃~4℃ refrigerator.
3.4.2 Acrylamide standard intermediate solution (10 mg/L): pipet 1.0 mL acrylamide stock solution and scale the volume to 100 mL with methanol.
4 Instruments and Apparatus
4.1 High performance liquid chromatograph: equipped with ultraviolet detector.
4.2 Analytical balance: with sensibility of 0.1 mg and 0.01 g.
4.3 Microporous filter membrane: 0.2 μm.
4.4 Colorimetric tube with stopper: 25 mL.
5 Analysis Steps
5.1 Preparation of test solutions
5.1.1 Preparation of food simulant test solution
Carry out migration test according to the intended use and service conditions of to-be-tested sample and the migration test methods and conditions specified in GB 5009.156 and GB 31604.1. After completion of the migration test, mix the simulants obtained from migration test sufficiently well for the next analysis.
5.1.2 Preparation of water-based, acidic and alcoholic food simulants test solution
Filter the food simulant test solution with 0.2 μm microporous filter membrane for determination.
5.1.3 Preparation of oil-based food simulant test solution
Weigh 10 g (accurate to 0.01 g) oil-based food simulant test solution into the colorimetric tube, add 10.0 mL water, violently oscillate for 1 min, and keep it still until layering. Filter the lower water solution with 0.2 μm filter membrane for determination.
5.1.4 Preparation of blank solution
5.1.4.1 Water-based, acidic and alcoholic food simulants blank solution
Transfer the food simulant not in contact with the sample and filter with 0.2 μm microporous filter membrane for determination.
5.1.4.2 Oil-based food simulant blank solution
Transfer 10 g (accurate to 0.01 g) food simulant not in contact with the sample and operate according to 5.1.3.
5.1.5 Water-based, acidic and alcoholic food simulants standard working solution
Accurately pipet 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL and 0.5 mL acrylamide standard intermediate solutions into 10mL-volumetric flasks, then scale the volume with food simulant not in contact with the sample to obtain the standard working solutions with the concentrations of acrylamide of 0.00 mg/L, 0.03 mg/L, 0.05 mg/L, 0.08 mg/L, 0.10 mg/L and 0.50 mg/L respectively. In the same way, prepare acrylamide standard working solution with the same concentration series with corresponding water-based, acidic and alcoholic food simulants respectively.
5.1.6 Oil-based food simulant standard working solution
Weigh 10 g (accurate to 0.01 g) oil-based food simulants and put into five colorimetric tubes respectively, pipet 0.00 mL, 0.03 mL, 0.05 mL, 0.08 mL, 0.1 mL and 0.5 mL acrylamide standard intermediate solutions (10 mg/L) into the colorimetric tubes and mix well, add 10.0 mL water, violently oscillate for 1 min and keep it still until layering to obtain the standard working solutions with the concentrations of acrylamide of 0.00 mg/kg, 0.03 mg/kg, 0.05 mg/kg, 0.08 mg/kg, 0.10 mg/kg and 0.50 mg/kg. Filter the lower water solution with 0.2 μm filter membrane for determination.
5.2 Determination
5.2.1 Liquid chromatographic conditions
a) Chromatographic column: Venusil CIS ion-exclusion chromatographic column with length of 250 mm, inside diameter of 4.6 mm and particle size of 5 μm, or equivalent;
b) Mobile phase: sulfuric acid solution: acetonitrile (91+9);
c) Flow rate: 0.5 mL/min;
d) Column temperature: 50℃;
e) Ultraviolet detector: with wavelength of 198 nm;
f) Sample injection amount: 20 μL.
5.2.2 Chromatographic determination
Inject the standard solution and sample solution in sequence for determination, plot the standard curve with the concentration of acrylamide in the standard working solution as x-axis (in mg/L or mg/kg) and the corresponding peak area of acrylamide as y-axis. Carry out the qualitative determination by retention time and quantitative determination by external standard method. Under the above chromatographic conditions, the retention time of acrylamide is 11.6 min, see Annex A for the chromatogram of acrylamide.
The regression parameter is calculated according to Formula (1):
y=a×x+b (1)
Where,
y——the peak area of acrylamide in food simulant standard working solution;
a——the slope of regression curve;
x——the concentration of acrylamide in the food simulant standard working solution, mg/L or mg/kg;
b——the intercept of regression curve.
Contents of GB 31604.18-2016
Foreword i
1 Scope
2 Principle
3 Reagents and Materials
4 Instruments and Apparatus
5 Analysis Steps
6 Expression of Analysis Results
7 Accuracy
8 Other
Annex A Chromatogram of Standard Solution
