Detail of GB 5009.191-2024

Introduction of GB 5009.191-2024

GB 5009.191-2024 National food safety standard - Determination of chloropropanol and its fatty acid ester and glycidyl ester in foods 1 Scope Volume I of this standard specifies the determination of chloropropanol in foods. Volume II of this standard specifies the determination of chloropropanol fatty acid ester and glycidyl ester in foods. Volume I is applicable to the determination of 3-chloro-1, 2-propanediol (3-MCPD), 2-chloro-1, 3-propanediol (2-MCPD), 1, 3-dichloro-2-propanol (1, 3-DCP) and 2, 3-dichloro-1-propanol (2, 3-DCP) in condiments containing acid hydrolyzed vegetable protein, meat and meat products, and formula foods for infants and young children. Methods I and II in Volume II are suitable for the determination of 3-chloro-1, 2-propanediol ester (3-MCPDE), 2-chloro-1, 3-propanediol ester (2-MCPDE) and glycidyl ester (GE) in oils and fats and their products, formula foods for infant and young children, milk and dairy products, aquatic animals and their products, meat and meat products, puffed food, baked food and fried food. Method III is suitable for the determination of 3-MCPDE, 2-MCPDE and GE in oils and fats and their products. Volume I Determination of chloropropanol content in foods - Isotope dilution - Gas chromatography-mass spectrometry 2 Principle Add isotope internal standard to the specimen, extract with sodium chloride solution, purify by diatomite column, elute chloropropanol with n-hexane and ethyl acetate in sequence, then determine by gas chromatography-mass spectrometry and quantify by internal standard method after the eluant is derived with N-Heptafluorobutyrylimidazole. 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. 3.1 Reagents 3.1.1 Ethyl acetate (C4H8O2): chromatographically pure. 3.1.2 N-hexane (C6H14): chromatographically pure. 3.1.3 Sodium chloride (NaCl). 3.1.4 Anhydrous sodium sulfate (Na2SO4): baked at 120°C for 4h before use, and then put in a desiccator for later use. 3.1.5 N-Heptafluorobutyrylimidazole (C7H3F7N2O, CAS No.: 32477-35-3): with a purity greater than or equal to 97%. Keep it sealed and protected from moisture after use. 3.2 Reagent preparation Sodium chloride solution (200g/L): weigh 200g of sodium chloride, add water to dissolve it and dilute the solution to 1L. 3.3 Standard substances 3.3.1 3-chloro-1, 2-propanediol (3-MCPD) (C3H7ClO2, CAS No. 96-24-2): standard substance with a purity of more than or equal to 98% or certified by the state with a certificate of standard substance. 3.3.2 D5-3-chloro-1, 2-propanediol (D5-3-MCPD) (C3H2D5ClO2, CAS No. 342611-01-2): with a purity of more than or equal to 98%. 3.3.3 2-chloro-1, 3-propanediol (2-MCPD) (C3H7ClO2, CAS No. 497-04-1): standard substance with a purity of more than or equal to 98% or certified by the state with a certificate of standard substance. 3.3.4 D5-2-chloro-1, 3-propanediol (D5-2-MCPD) (C3H2D5ClO2, CAS No. 1216764-05-4): with a purity of more than or equal to 98%. 3.3.5 1, 3-dichloro-2-propanol (1,3-DCP) (C3H6Cl2O, CAS No. 96-23-1): standard substance with a purity of more than or equal to 98% or certified by the state with a certificate of standard substance. 3.3.6 D5-1, 3-dichloro-2-propanol (D5-1, 3-DCP) (C3HD5Cl2O, CAS No. 1173020-20-6): with a purity of more than or equal to 98%. 3.3.7 2, 3-dichloro-1-propanol (2, 3-DCP) (C3H6ClO2, CAS No. 616-23-9): standard substance with a purity of more than or equal to 98% or certified by the state with a certificate of standard substance. 3.3.8 D5-2, 3-dichloro-1-propanol (D5-2,3-DCP) (C3HD5Cl2O, CAS No. 1189730-34-4): with a purity of more than or equal to 97%. 3.4 Preparation of standard solution 3.4.1 Chloropropanol standard solution 3.4.1.1 Chloropropanol standard stock solution (1,000μg/mL): weigh 10.0mg (accurate to 0.01mg) of chloropropanol standard substance respectively, transfer to a 10mL volumetric flask after dissolving with ethyl acetate, then dilute with ethyl acetate to scale and mix well. Transfer the solution to well-sealed brown glass bottles, and store them at -20°C for 12 months. 3.4.1.2 Mixed standard intermediate solution of chloropropanol (10.0μg/mL): Accurately take an appropriate amount of chloropropanol standard stock solution (1,000μg/mL), dilute it with n-hexane to a concentration of 10.0μg/mL, shake well and transfer to well-sealed brown glass bottle, and store at -20℃ for 6 months.

Contents of GB 5009.191-2024

Foreword i 1 Scope 2 Principle 3 Reagents and materials 4 Instruments and apparatus 5 Analytical procedure 6 Expression of analysis results 7 Precision 8 Others 9 Principle 10 Reagents and materials 11 Apparatus 12 Analytical procedure 13 Expression of analysis results 14 Precision 15 Others 16 Principle 17 Reagents and materials 18 Instruments and apparatus 19 Analysis procedures 20 Expression of analysis results 21 Precision 22 Others 23 Principle 24 Reagents and materials 25 Instruments and apparatus 26 Analytical procedure 27 Expression of analysis results 28 Precision 29 Others Annex A Volume I Chromatograms and mass spectra of chloropropanol and its derivatives with deuterated isotopic internal standards Annex B Volume II Information about the Method-I standard and its chromatogram and mass spectra of phenylboronic acid derivatives Annex C Volume II Monitoring parameters and chromatograms and mass spectra of Method II chloropropanol and 3-MBPD derivatives Annex D Volume II Monitoring parameters, chromatograms and mass spectra of Method-III chloropropanol and its isotopic phenylboronic acid derivatives