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GB 31604.29-2023 PDF EnglishSearch result: GB 31604.29-2023_English: PDF (GB31604.29-2023)
GB31604.29-2023: PDF in EnglishGB 31604.29-2023 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National food safety standard - Food contact materials and products - Determination of migration of acrylic acid and methacrylic acid and their esters ISSUED ON. SEPTEMBER 06, 2023 IMPLEMENTED ON. MARCH 06, 2024 Issued by. National Health Commission of the People's Republic of China; State Administration for Market Regulation. Table of Contents Foreword... 3 1 Scope... 4 2 Principle... 4 3 Reagents and materials... 4 4 Instruments and apparatuses... 6 5 Analysis steps... 7 6 Expression of analysis results... 9 7 Precision... 11 8 Others... 11 9 Principle... 12 10 Reagents and materials... 12 11 Instruments and apparatuses... 14 12 Analysis steps... 14 13 Expression of analysis results... 15 14 Precision... 16 15 Others... 16 Appendix A Relevant information and weighing conversion coefficients of 18 acrylate and methacrylate standards... 17 Appendix B Target retention time, quantitative ions and qualitative ions in gas chromatography-tandem mass spectrometry SIM mode... 18 Appendix C Typical gas chromatography-tandem mass spectrometry total ion chromatogram of standard working solution... 19 Appendix D Relevant information and weighing conversion coefficients of 6 acrylic acid, methacrylic acid and their ester standards... 21 Appendix E Gradient elution reference procedure for liquid chromatography... 22 Appendix F Standard working solution liquid chromatogram... 23 National food safety standard - Food contact materials and products - Determination of migration of acrylic acid and methacrylic acid and their esters 1 Scope This Standard specifies the determination method for the migration of acrylic acid and methacrylic acid and their esters in food contact materials and products. Part 1 – Gas chromatography-mass spectrometry applies to the determination of migration of 18 kinds of acrylate and methacrylate in food contact materials and products, including 2-acrylic acid-2-methylpropyl ester, ethylacrylate, n-butyl acrylate, isopropyl acrylate, acrylic acid n-propyl ester, 2-propenoic acid, 1,1-dimethylethyl ester, acrylic acid benzyl ester, 2-octyl acrylate, sec-butyl acrylate, ethyl methacrylate, isobutyl methacrylate, butyl methacrylate, 2-methyl-2-acrylic acid-1,1-dimethylethyl ester, phenyl methacrylate, 2-methyl-2-propyl acrylate, benzyl methacrylate, sec-butyl methacrylate and isopropyl methacrylate. Part 2 – Liquid chromatography applies to the determination of migration of 6 kinds of acrylic acid, methacrylic acid and their esters in food contact materials and products, including acrylic acid, methacrylic acid, 2-hydroxyethyl acrylate, 2-hydroxyethyl-2- methyl-2-acrylate, methyl acrylate and methyl methacrylate. Part 1 – Gas chromatography-mass spectrometry 2 Principle The water-based food simulants as well as oil and fat food simulants obtained from the migration test are headspace sampled; the 95% (volume fraction) ethanol and isooctane simulants are directly sample after diluted with ethyl acetate; the target substance is separated in the gas chromatography capillary column, detected by mass spectrometry, and quantified by the external standard method. 3 Reagents and materials Unless otherwise specified, all the reagents in this method are analytical reagents, and the water is grade-1 water specified by GB/T 6682. 3.1 Reagents 3.1.1 Methanol (CH4O). chromatographic pure. 3.1.2 Ethyl acetate (C4H8O2). chromatographic pure. 3.1.3 Sodium chloride (NaC1). 3.1.4 Anhydrous acetic acid (C2H4O2). 3.1.5 Absolute ethanol (C2H6O). 3.1.6 95% ethanol (C2H6O). 3.1.7 Isooctane (C8H18). 3.2 Preparation of reagents 3.2.1 Food simulant. Prepare in accordance with the provisions of GB 5009.156. 3.2.2 Isooctane-ethyl acetate solution (1+4). Mix 25 mL of isooctane and 100 mL of ethyl acetate evenly. 3.2.3 95% ethanol-ethyl acetate solution (1+4). Mix 25 mL of 95% ethanol and 100 mL of ethyl acetate evenly. 3.3 Standards 18 kinds of acrylate and methacrylate standards (see Appendix A). purity ≥98%, or standard products certified by the country and awarded a standard substance certificate. 3.4 Preparation of standard solutions 3.4.1 Standard stock solutions (1 000 mg/L). Accurately weigh 18 standards (accurate to 0.1 mg). The weighing mass calculation method is 25 mg divided by the conversion coefficient, which is shown in Appendix A. Dissolve them in ethyl acetate respectively and then transfer them to the 25 mL volumetric flasks; use ethyl acetate to dilute to the mark and mix well. Transfer the solutions to brown glass containers and store them in the dark at 4 °C for 6 months. 3.4.2 Mixture of standard intermediate solution A (50 mg/L). Respectively and accurately pipette 0.5 mL of the standard stock solutions (1 000 mg/L) into the 10 mL volumetric flasks; add methanol to adjust the volume to the mark; mix well. Transfer the solutions to brown glass containers and store them in the dark at 4 °C for 6 months. 3.4.3 Mixture of standard intermediate solution B (50 mg/L). Respectively and accurately pipette 0.5 mL of the standard stock solutions (1 000 mg/L) into the 10 mL volumetric flasks; add ethyl acetate to adjust the volume to the mark; mix well. Transfer the solutions to brown glass containers and store them in the dark at 4 °C for 6 months. 3.4.4 Water-based food simulant series standard working solutions. Respectively and accurately pipette 100 μL, 150 μL, 200 μL, 400 μL and 1 000 μL of the mixtures of standard intermediate solution A (50 mg/L) into the 100 mL volumetric flasks; use 50% (volume fraction) ethanol solution to adjust the volume. The concentrations of each target substance in the obtained standard working solutions are 0.050 mg/L, 0.075 mg/L, 0.10 mg/L, 0.20 mg/L, and 0.50 mg/L, respectively. Respectively pipette 10.0 mL of solutions of each concentration into the 20 mL glass headspace bottles to which 3.0 g of sodium chloride has been added; immediately use a spacer and an aluminum cap to seal them, for later testing. Use the same method to prepare a series of standard working solutions of the same concentration with water, 4% (volume fraction) acetic acid, 10% (volume fraction) ethanol, and 20% (volume fraction) ethanol. Prepare when necessary. 3.4.5 Oil and fat food simulant series standard working solutions. Respectively and accurately weigh 5.00 g (accurate to 0.01 g) of olive oil simulant into five 20 mL glass headspace bottles; use a pipette to respectively pipette 30 μL, 80 μL, 100 μL, 150 μL, and 300 μL of the mixture of standard intermediate solution B (50 mg/L) into the 20 mL glass headspace bottles; immediately use a spacer and an aluminum cap to seal them; vortex evenly, for later testing. The concentrations of each target substance in the obtained standard working solutions are 0.30 mg/kg, 0.80 mg/kg, 1.0 mg/kg, 1.5 mg/kg, and 3.0 mg/kg, respectively. Prepare when necessary. 3.4.6 Isooctane series standard working solutions. Respectively pipette 50 μL, 150 μL, 200 μL, 300 μL and 600 μL of the mixture of standard intermediate solution B (50 mg/L) into the 10 mL volumetric flasks; use isooctane-ethyl acetate solution (1+4) to adjust the volume to the mark; mix well. The concentrations of each target substance in the obtained standard working solution are 0.25 mg/L, 0.75 mg/L, 1.0 mg/L, 1.5 mg/L and 3.0 mg/L, respectively. Prepare when necessary. 3.4.7 95% (volume fraction) ethanol series standard working solutions. Respectively pipette 50 μL, 150 μL, 200 μL, 300 μL, and 600 μL of the mixture of standard intermediate solution B (50 mg/L) into the 10 mL volumetric flasks; use 95% ethanol- ethyl acetate solution (1+4) to adjust the volume to the mark. The concentrations of each target substance in the obtained standard working solution are 0.25 mg/L, 0.75 mg/L, 1.0 mg/L, 1.5 mg/L and 3.0 mg/L, respectively. Prepare when necessary. 4 Instruments and apparatuses 4.1 Gas chromatograph-mass spectrometer, equipped with electron impact source (EI) and headspace sampler. 4.2 Vortex oscillator. 4.3 Electronic balance. The sensitivity is 0.1 mg and 0.01 g, respectively. d) Oscillation speed. 500 r/min. e) Injection volume. 250 μL. 5.4.2 The reference conditions for gas chromatography mass spectrometry measurement are as follows. a) Chromatographic column. polyethylene glycol capillary column. column length 30.0 m, inner diameter 0.25 mm, film thickness 0.25 μm, or an analytical column with equivalent performance. b) Programmed temperature rise. initial temperature 35 °C, kept for 8 min; increased to 60 °C at 5 °C/min, kept for 3 min; increased to 160 °C at 20 °C/min, kept for 2 min; increased to 220 °C at 40 °C/min, kept for 3 min. c) Inlet temperature. 290 °C. d) Mass spectrometry joint temperature. 280 °C. e) Ion source temperature. 230 °C; f) Carrier gas. He (purity >99.999%), constant flow 1.0 mL/min. g) Injection volume. 1 μL. h) Injection method. split injection, the split ratio of water-based food simulant test solution is 20.1; the split ratio of oil and fat food simulant test solution is 50.1; the split ratio of isooctane test solution and 95% (volume fraction) ethanol test solution is 2.1. i) Ionization method. EI. j) Solvent delay. 5.0 min. k) Mass spectrometry scanning mode. selected ion mode (SIM). l) SIM acquisition parameters. see Appendix B. 5.5 Preparation of the standard curve According to the apparatus reference conditions listed in 5.4.1 and 5.4.2, inject the series standard working solutions into the gas chromatograph-tandem mass spectrometer respectively, and measure the corresponding peak areas. Draw the standard working curve with the concentration of the target substance in the standard series working solution as the abscissa and the corresponding quantitative ion peak area as the ordinate. See Appendix C for the typical total ion chromatogram .......Source: https://www.ChineseStandard.net/PDF.aspx/GB31604.29-2023 |