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建立了液相色谱-串联质谱法测定水产品中麻醉剂3-氨基苯甲酸乙酯甲基磺酸盐(MS-222)残留量的方法。提取液为50%的甲醇及乙酸-乙酸钠缓冲溶液,提取液经C18固相萃取柱净化处理后用液相色谱-串联质谱仪进行测定,外标法定量。流动相为0.5%的甲酸溶液和乙腈(V:V=60:40),流速为0.2 mL/min。该方法的线性范围为0.001~1.0 mg/L,相关系数大于0.999,检出限为1μg/kg,定量限为2μg/kg。加标回收率可以达到80%~110%。
A liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of 3-aminobenzoate methyl methanesulfonate (MS-222) residues in aquatic products was established. The extract was 50% methanol and acetic acid - sodium acetate buffer solution, the extract was purified by C18 solid phase extraction column with liquid chromatography - tandem mass spectrometry for determination, external standard. The mobile phase consisted of 0.5% formic acid solution and acetonitrile (V: V = 60:40) at a flow rate of 0.2 mL / min. The linear range of the method was 0.001-1.0 mg / L, the correlation coefficient was greater than 0.999, the detection limit was 1μg / kg and the limit of quantification was 2μg / kg. Spike recovery rate can reach 80% to 110%.