Determination of polychlorinated biphenyls in sediment by automatic solid phase extraction and chromatography coupled with triple quadrupole tandem mass spectrometry
建立了全自动固相萃取-三重四级杆串联质谱同时测定沉积物中27种多氯联苯的分析方法。样品经1; :1(体积比)丙酮正己烷超声提取后经全自动固相萃取仪净化,采用气相色谱/三重四级杆串联质谱在多反映监测模式(MRM)下进行测定。在MRM模式下用; 两对离子对对多氯联苯进行分析,对母离子进行了碰撞能优化;27种多氯联苯的线性范围为2~200 mug/L,线性的相关系数(r~2) > 0.; 9945,方法检出限在0. 023~0. 060 mug/kg之间,加标回收率为84. 0%~118%,相对标准偏差< 6. 5%。An analytical method was established for simultaneous determination of; 27 polychlorinated Biphenyls (PCBs) residues in sediment by automatic; solid phase extraction and gas chromatography coupled with triple; quadrupole mass spectrometry (GC/MS/MS) . The samples were extracted; with acetone hexane,cleaned up by automatic solid phase extracter,then; analyzed by GC/MS/MS using multiple reaction monitoring (MRM) mode. As; the results showed,27 PCBs were analyzed in the MRM mode using two pairs; of ions. The collision energy of the parent ion was optimized. The liner; range of 27 PCBs were all larger than 0. 9945,the method detection; limits (MDLs) were form 0. 023 mug/kg to 0. 060 mug/kg, the average; recovery rate were in the range of 84. 0% ~118% and the RSD were less; than 6. 5%. The method was proved to be highly automated,; simple,selective with good reproducibility and it can be suitable for; the trace analysis of PCBs in sediment.厦门南方海洋研究中心海洋生态环境监测和水产品检测服务平台项目基
