Animal residue detection

This standard specifies the sample preparation method, high-performance liquid chromatography detection method, and liquid chromatography-mass spectrometry/mass spectrometry confirmation method for the detection of tetracycline residues in animal derived foods. This standard is applicable to the determination of residues of seven tetracycline veterinary drugs, including dimethylamine tetracycline, oxytetracycline, tetracycline, demethyl aureomycin, aureomycin, methyloxytetracycline, and doxycycline, in animal muscle, visceral tissue, aquatic products, milk, and other animal derived foods by high-performance liquid chromatography, as well as the determination of residues of dimethylamine tetracycline, oxytetracycline, oxytetracycline, demethyl aureomycin, demethyl aureomycin, aureomycin, and methyloxytetracycline, Liquid chromatography-mass spectrometry/mass spectrometry determination of 10 tetracycline residues in doxycycline. 2 Normative References: The clauses in the following documents become clauses of this standard through reference in this standard. For dated reference documents, all subsequent amendments (excluding corrected content) or revisions are not applicable to this standard. However, parties to agreements based on this standard are encouraged to study whether the latest versions of these documents can be used. For undated references, the latest version applies to this standard. GB/T 6682 Specification and Test Methods of Water for Analytical Laboratory (GB/T 6682-1992, neq ISO 36961987) 3 Tetracycline antibiotics residues in principle samples are extracted with 0.1 mol/L Na, EDTA Mclvaine buffer solution (pH=4.0 ± 0.05), filtered and centrifuged, the supernatant is purified with HLB solid phase extraction column, determined by HPLC or liquid chromatography harmonic spray mass spectrometer, and quantified by external standard peak area method. Unless otherwise specified, all reagents and materials used are analytical pure, and the water is Grade 1 water according to GB/T 6682. 4.1 Methanol: High performance liquid chromatography pure. 4.2 Acetonitrile: High performance liquid chromatography pure. 4.3 Ethyl acetate. 4.4 Sodium ethylenediaminetetraacetic acid (NagEDTA · 2H, O). 4.5 Trifluoroacetic acid. 4.6 Citric acid (C, H, O, - HRO). 4.7 Disodium hydrogen phosphate (Nag HPO · 12HzO). 4.8. Citric acid solution: 0.1 mol/L. Weigh 21.01 g of citric acid (4.6), dissolve it in water, and bring to a constant volume of 1000 mL. 4.9 Disodium hydrogen phosphate solution: 0.2 mol/L. Weigh 28.41 g of disodium hydrogen phosphate (4.7), dissolve it in water, and bring to a constant volume of 1000 mL. 4.10 Mcllvaine buffer solution: Mix 1000 mL of 0.1 mol/L citric acid solution (4.8) with 625 mL of o. 2 mol/L disodium hydrogen phosphate solution (4.9), and adjust pH to 4.0 with sodium hydroxide or hydrochloric acid if necessary. 4.11 Na, EDTA McCllvine buffer solution; 0. l mol/L. Weigh 60.5 g of disodium ethylenediaminetetraacetic acid (4.4) and place it in 625 mL of Mcllvaine buffer solution (4.10), dissolve it, and shake well. 4.12 Methanol+Water (1-19): Measure 5 mL of methanol (4.1) and mix with 95 mL of water

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