微波辅助提取-固相萃取净化-气相色谱三重四极杆质谱联用测定水产品中17种多氯联苯（PCBs）

为了给食品中持久性有机污染物残留的定性与定量检测提供技术支持，建立了一种微波辅助提取-固相萃取净化-气相色谱三重四极杆质谱联用测定水产品中17种多氯联苯（PCBs）的检测方法。样品用V（正己烷）∶V（丙酮）=1∶1的混合溶剂于微波提取，经佛罗里硅土固相萃取柱净化，以氦气为载气，HP5-MS色谱柱分离，MS/MS多反应监测扫描模式（MRM）检测。方法线性相关系数r＞0.999，仪器定量限为1.0~3.0 μg/kg。在5.0、10.0、20.0 μg/kg 3种浓度添加水平，其平均回收率为83.1%~100.8%，相对标准偏差(RSD)为4.36%~9.38%。该方法已成功应用于复杂基质样品中17种PCBs的检测。

Determination of 17 Kinds of Polychlorinated Biphenyls(PCBs) in Fishery Product by MAE-SPE-GC-MS/MS

A microwave assisted extraction-solid phase extraction-gas chromatography-tandem mass spectrometry(MAE-SPE-GC-MS/MS) method for the determination of 17 kinds of PCBs in fishery product was developed.The fishery product samples were extracted with the solution(V(n-hexane)∶V(acetone)=1∶1) by microwave assisted extraction technique.Clean-up was carried out with florisil solid phase extraction.After HP5-MS chromatographic column separation using helium as a carrier gas,the eluents were determined under multi-reaction monitoring(MRM) scan type with tandem mass analyzer.The correlation coefficients are larger than 0.999,and the limit of quantification(LOD) is 0.5—1.0 μg/kg.At the spiked levels of 5.0,10.0,20.0 μg/kg,the average recoveries range from 83.1% to 100.8%,and the relative standard deviations(RSDs) range from 4.36% to 9.38%.The proposed method had been used for the determination of 17 kinds of PCBs in complex sample.