Food additive residue detection

This standard specifies the determination method for chloropropanol and chloropropanol fatty acid esters in food. This standard is applicable to the determination of the content of hydrogenpropanol and chloropropanol fatty acid esters in food. This standard includes three detection methods: determination of 3-chloro-1,2-propanediol content in food, determination of multi-component content of chloropropanol in food, and determination of chloropropanol fatty acid ester content in food. The first method is the determination of 3-chloro-1,2-propanediol content in food. This standard uses isotope dilution technology and uses D-3-chloro-1,2-propanediol (D-3-MCPD) as the internal standard. Add internal standards to the sample, use diatomaceous earth as adsorbent, perform solid-phase supported liquid-liquid extraction, wash with n-hexane anhydrous ether solution (9+1) to remove non-polar lipid components, and wash with anhydrous ether to remove 3-chloro-1.2-propanediol (3-MCPD). Derived from heptafluorobutyrylimidazole, determined by gas chromatography-mass spectrometry, and quantified by internal standard method. Unless otherwise specified, all reagents and materials used in this method are analytical pure, and the water is the first grade water specified in GB/T 6682. 3.1 Reagent 3.1.1 Ethyl acetate (CHgO:): Chromatically pure. 3.1.2 n-hexane (CaH): Chromatically pure. 3.1.3 Anhydrous ether (CH,, O): Before use, it needs to be re steamed, and a small amount of reduced iron powder should be added during re steaming. 3.1.4 Sodium chloride (NaC1). 3.1.5 Anhydrous sodium sulfate (NagSO): Bake at 120 ℃ for 4 hours before use. 3.1.6 Heptafluorobutyrylimidazole (C, H, F-N O, CAS No. 32477-35-3): Purity ≥ 98%. 3.2 Reagent Preparation 3.2.1 Sodium Chloride Solution (20%): Weigh 20 g of sodium chloride, add 80 mL of water, and stir until the sodium chloride is fully dissolved. 3.2.2 n-hexane anhydrous ether solution (9+1): Mix 450 mL of n-hexane with 50 mL of anhydrous ether evenly. 3.3 Standard 3.3.13 Chloro-1,2-propanediol (3-MCPD) Standard (CH, ClO, CAS No. 96-24-2): Purity ≥ 98%. 3.3.2 D-3-Chloro-1,2-propanediol (D-3-MCPD) standard (C, D-H, CIOz): purity ≥ 98%

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