GB 31604.29-2023 National food safety standard - Determination of migration of acrylic acid, methacrylic acid and their esters in food contact materials and articles
1 Scope
This standard specifies the determination method of migration of acrylic acid, methacrylic acid and their esters in food contact materials and articles.
Part I Gas Chromatography-Mass spectrometry is applicable to determination of migration of 18 kinds of acrylate and methacrylate in food contact materials and articles, including 2-Acrylic acid-2-Methylpropyl ester, ethyl acrylate, n-butyl acrylate, isopropyl acrylate, propyl acrylate, 2-Acrylic acid-1, 1-Dimethylethyl ester, benzyl acrylate, 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, methyl methacrylate benzyl ester, sec-butyl methacrylate, isopropyl methacrylate.
Part II Liquid chromatography is applicable to determination of migration of 6 kinds of acrylic acid, methacrylic acid and their esters in food contact materials and articles, including acrylic acid, methacrylic acid, acrylic acid 2-hydroxyethyl ester, 2-hydroxyethyl-2-methyl-2-acrylate, methyl acrylate, methyl methacrylate.
Part I Gas chromatography - mass spectrometry (GC-MS)
2 Principle
The water-based food simulant and the oil-based food simulant obtained by the migration test are injected by headspace,dilute 95% (v/v) ethanol and isooctane simulants with ethyl acetate and directly inject. Separate the target substances in gas chromatography capillary column, detect by mass spectrometry, and set volume by external standard method.
3 Reagents and materials
Unless otherwise specified, analytically pure reagents, and Class-I water as defined in GB/T 6682, are used for the purpose of this method.
3.1 Reagents
3.1.1 Methanol (CH4O): chromatographically pure.
3.1.2 Ethyl acetate (C4H8O2): chromatographically pure.
3.1.3 Sodium chloride (NaCl).
3.1.4 Acetic anhydrid (C2H4O2).
3.1.5 Anhydrous ethanol (C2H6O).
3.1.6 95% ethanol (C2H6O).
3.1.7 Isooctane (C8H18).
3.2 Preparation of reagents
3.2.1 Food simulants: prepared in accordance with as GB 5009.156.
3.2.2 Isooctane-Ethyl acetate solution (1+4): mix 25 mL of Isooctane and 100 mL of ethyl acetate well.
3.2.3 95% ethanol-ethyl acetate solution (1+4): mix 25 mL of 95% ethanol and100 mL of ethyl acetate well.
3.3 Standards
18 kinds of acrylate and methacrylate standards (See Annex A): Purity≥98%, or standards that have been certified by the state and granted a reference material certificate.
3.4 Preparation of standard solutions
3.4.1 Standard stock solution (1,000 mg/L): Accurately weigh 18 kinds of standards (accurate to 0.1 mg), the weighing mass calculation method is 25 mg divided by the conversion factor, which is shown in the Annex A, separately dissolve it in ethyl acetate and then transfer it into a 25 mLvolumetric flask, set volume to the mark with ethyl acetate and mix well. Transfer the solution to a brown glass container, store it at 4℃ in the dark from light, with shelf life of 6 months.
3.4.2 Mixed standard intermediate solution A (50 mg/L): Accurately pipet 0.5 mL standard stock solution (1 000 mg/L) into 10 mL volumetric flask separately, add methanol to set volume to the mark and mix well.Transfer the solution to a brown glass container, store it at 4℃ in the dark from light, with shelf life of 6 months.
3.4.3 Mixed standard intermediate solution B (50 mg/L): Accurately pipet 0.5 mL standard stock solution (1 000 mg/L) into a 10 mL volumetric flask separately, add ethyl acetate to se volume to the mark and mix well.Transfer the solution to a brown glass container, store it at 4℃ in the dark from light, with shelf life of 6 months.
Foreword i
1 Scope
Part I Gas chromatography - mass spectrometry (GC-MS)
2 Principle
3 Reagents and materials
4 Apparatus
5 Analytical procedures
6 Expression of analysis results
7 Accuracy
8 Others
Part II Liquid chromatography
9 Principle
10 Reagents and materials
11 Apparatus
12 Analytical procedures
13 Expression of analysis results
14 Accuracy
15 Others
Annex A Related information and weighing conversion factors for 18 kinds of acrylate and methacrylate standards
Annex B Target retention time, quantitative ions and qualitative ions in SEM mode by gas chromatography - tandem mass spectrometry
Annex C Total ion current diagram of typical gas chromatography-tandem mass spectrometry of standard working solution
Annex D Related information and weighing conversion factors of 6 kinds of standards of acrylic acid and methacrylic acid and their esters
Annex E Reference procedure for gradient elution by liquid chromatography
Annex F Liquid chromatogram of standard working solution
