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 for the simultaneous determination of 27 PCBs in sediments by automatic quadrupole SPE and triple quadrupole tandem mass spectrometry was established. The samples were extracted with 1: 1 (by volume) acetone-n-hexane and purified by an automated SPE. Gas chromatography / triple quadrupole tandem mass spectrometry was used to determine the results in multiple reaction monitoring mode (MRM). In the MRM mode, two pairs of ion pairs were used to analyze PCBs. The collision of precursor ions was optimized. The linear range of 27 PCBs was 2 ~ 200μg / L, and the linear correlation coefficient (r ~ 2 )> 0.9945. The detection limits of the method ranged from 0.023 to 0.060 μg / kg with recoveries of 84.0% -118% and relative standard deviations <6.5%.