同位素稀释-液相色谱-串联质谱法同时测定养殖水体中23种镇静剂

Simultaneous Determination of 23 Sedative Residues in Aquaculture Water by Isotope Dilution Liquid Chromatography Tandem Mass Spectrometry

建立了同位素稀释液相色谱串联质谱法(LC-MS/MS)同时测定养殖水体中23种镇静剂残留的方法。样品经0.45μm滤膜过滤后,用Oasis HLB固相萃取柱净化,浓缩后用50%的甲醇水定容。以1%甲酸水溶液和乙腈为流动相,采用Agilent InfiniityLab Poroshell 120 SB-C18色谱柱分离后,在多反应监测模式下测定,内标法定量。结果表明,23种镇静剂在0.5~100 ng/L质量浓度范围内线性关系良好(r>0.99),检出限和定量限分别为0.1~0.3和0.4~1.0 ng/L。加标回收率为73.5%~117.6%,相对标准偏差(RSD)为1.1%~9.9%。该方法前处理简单,净化效果较好,灵敏度较高,适用于池塘养殖水体中23种镇静剂类药物残留的快速检测。

A method for simultaneous determination of 23 sedative residues in aquaculture water by isotope dilution liquid chromatography tandem mass spectrometry(LC-MS/MS)was established.The samples were filtered by 0.45μm filter membrane,purified by solid phase extraction column(Oasis HLB column),then concentrated the eluate and brought to volume with 50%methanol-50%water.By using 1%formic acid aqueous solution and acetonitrile as mobile phase,the targets were separated by an Agilent InfinityLab Poroshell 120 SB-C18 chromatographic column,and determined in multi reaction monitoring mode and quantified by internal standard method.The results showed that the linearity of 28 sedatives was good in the concentration range of 0.5~100 ng/L(r>0.99),and the detection limits and quantitative limits were 0.1~0.3 and 0.4~1.0 ng/L,respectively.The average recovery was 73.5%~117.6%and the relative standard deviations(RSD)were 1.1%~9.9%.This method has simple pretreatment,good purification effect and high sensitivity.It can be used for the rapid detection of 23 sedative drug residues in pond aquaculture water.