快速检测水产饲料中氯霉素、甲砜霉素、氟甲砜霉素残留

Simultaneous analysis of trace chlorampheicol,thiamphenicol and fiorfenicol in aquatic feeds

建立了水产养殖饲料中氯霉素、甲砜霉素、氟甲砜霉素3种氯霉素类抗菌素同时检测的液相色谱-串联质谱(HPLC-MS/MS)方法。优化了样品前处理过程中提取溶剂、提取溶剂碱性、固相萃取柱类型,采用三重串联四级杆质谱的电喷雾电离负离子模式和选择离子反应监测模式,建立了水产饲料中3种氯霉素类抗菌素HPLC-MS/MS的同时分析方法。方法的加标回收率为84.7%~101.0%,相对标准偏差3.7%~7.0%(n=6),检出限为0.1~0.2μg/kg,定量限为0.3~0.5μg/kg。

An chlorampheicol, analytical method was established for the simultaneous determination of trace thiamphenicol and fiorfenicol in aquatic feeds by high-performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS）. Several crucial conditions for sample preparation were optimized in detail including the extraction solvent, the basicity of extraction solvent and the types of solid phase extraction cartridges. Then, HPLC-MS/MS based on the negative mode of electrospray ionization and selective reaction monitoring mode was adopted for the determination. The satisfied recoveries based on spiked samples were achieved in the range of 84. 7% - 101.0% with relative standard deviations of 3.7% -7.0% （n = 6）. The detection limits were in range of 0. 1 0.2 μg/kg, and the limits of quantification were in range of 0. 3 - 0. 5 μg/kg.