Testing parameters for agricultural products

This standard specifies the sample preparation method and high-performance liquid chromatography-mass spectrometry/mass spectrometry detection method for the detection of 14 quinolone drug residues in animal derived foods. This standard is applicable to the liquid chromatography-mass spectrometry/mass spectrometry determination and confirmation of residues of 14 quinolone veterinary drugs, including enrofloxacin, norfloxacin, pefloxacin, ciprofloxacin, ofloxacin, levofloxacin, lomefloxacin, pipemidic acid, naphthinic acid, oxalic acid, fluoroquine, cinofloxacin, and monofloxacin, in animal derived foods such as pork, pig liver, pig kidney, milk, and eggs. 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/T6682 Specification and Test Methods for Analytical Laboratory Water (GB/T 6682-1992, neq ISO 3696:1987) 3 Method Abstract: Quinolone antibiotics were extracted from the sample using 0.1mol/L EDTA-McCllvine buffer (pH4.0), filtered and centrifuged, and the supernatant was purified by HLB solid-phase extraction column. High performance liquid chromatography mass spectrometry/mass spectrometry, quantitative analysis using negative sample matrix addition external standard method. During the sample preparation process, it is necessary to prevent contamination or changes in residual content of the sample. 4.1 Animal muscles and viscera: The samples collected on site are transported to the laboratory in a small freezer, stored at a temperature below 10 ℃, and processed within a week. Take fresh or frozen thawed animal tissue samples from suitable locations, remove tendons, and mash them evenly. 4.2 Milk: The samples collected on site will be transported to the laboratory in a small freezer, stored below -10 ℃, and processed within a week. Take an appropriate amount of fresh or frozen thawed samples and mix evenly. 4.3 Eggs: Place the on-site collected samples into a small freezer and transport them to the laboratory. Store them at a temperature below 10 ℃ and process them within a week. Take an appropriate amount of fresh sample, remove the shell, and mix evenly. Unless otherwise specified, all reagents and materials used in this method are chromatographically pure, and the water is grade - water according to GB/T 6682. 5.1 Citric acid: analytically pure. 5.2 Disodium hydrogen phosphate: analytically pure. 5.3 Methanol. 5.4 Acetonitrile. 5.5 Methanol acetonitrile solution; 40+6O (volume ratio)

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