ASE-SPE-HPLC-MS/MS检测水产品中阿维菌素类药物残留

目的]建立水产品中阿维菌素、伊维菌素、莫西菌素、爱普利诺菌素、多拉菌素5种阿维菌素类药物残留量的快速溶剂萃取-液相色谱-串联质谱(ASE-SPE-HPLC/MS/MS)测定方法。方法]样品采用快速溶剂萃取,乙腈为提取液,提取液浓缩后经C18小柱净化;经SHISEIDO CAPCELL PAK C18MG S5质谱柱分离,乙腈-2.5 mmol/L乙酸铵水(0.1%乙酸)溶液为流动相,在电喷雾电离负离子(ESI-)、多反应监测模式(MRM)下测定5种阿维菌素类药物残留,基质标准曲线外标法定量。结果]5种阿维菌素类药物在2.0~50.0μg/kg范围内线性关系良好,相关系数大于0.997,莫西菌素在5.0、10.0、20.0μg/kg,其他4种化合物在2.0、5.0、10.0μg/kg加标水平的平均回收率为81.7%~93.5%,相对标准偏差为7.54%~13.26%。结论]该方法提取效率高、净化较彻底,适合水产品中阿维菌素多药物残留量的测定。

Deter mination of Avermectin Residues in Aquatic Products by ASE-SPE-HPLC-MS/MS

Objective] A sensitive and rapid method for the simultaneous detection of abamectin,eprinomectin,ivemectin,doramectin and moxidectin residues in aquatic products by ASE-SPE-HPLC/MS/MS was developed.Method]The sample was extracted by ASE200 with acetonitrile and purified by SPE C18.With the gradient elution of acetonitrile and water（containing 2.5 mmol/L ammonium acetate and 0.1％ acetic acid）,the target compounds were separated on chromatographic column and detected in the mode of electrospry ionization （ESI-） and multiple reaction monitoring（MRM） by liquid chromatography tandem mass spectrometry.Result] The quantification was carrid out by matrix-matched external standard curve,the linear ranges of five avermectins were 2.0-50.0 μg/kg and the correlation coefficients were all above 0.997.The average recoveries at the concentration of 5.0,10.0 and 20.0 μg/kg for moxidectin and 2.0,5.0 and 10.0 μg/kg for other analytes in aquatic products from 81.7％ to 93.5％ with the relative standard deviations of 7.54％ to 13.26％.Conclusion] This method had better overall recovery and extraction efficiency,suitable for the deter mination of avermectin residues in aquatic products.