全自动固相萃取-气相色谱/串联质谱法测定沉积物中的多氯联苯

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2~200μg/L,线性的相关系数(r^2)﹥0.9945,方法检出限在0.023~0.060μg/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 μg/kg to 0. 060 μg/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.