加速溶剂萃取和净化-气相色谱/三重四极杆串联质谱法测定水体沉积物中多氯联苯  

Simultaneous determination of polychlorinated biphenyls in sediments by accelerated solvent extraction and gas chromatography coupled with triple quadrupole mass spectrometry

作　　者：田丙正[1] 张付海[1] 张敏[1] 胡雅琴[1] 赵彬[1] 王鑫[1] TIAN Bing-zheng ZHANG Fu-hai ZHANG Min HU Ya-qin ZHAO Bin WANG Xin(Anhui Environmental Monitoring Center, Hefei 230071)

机构地区：[1]安徽省环境监测中心站,合肥230071

出　　处：《分析试验室》2017年第7期785-789,共5页Chinese Journal of Analysis Laboratory

基　　金：安徽省环保科研项目(2015004);安徽省环保科研项目(2013008)资助

摘　　要：建立了加速溶剂萃取同步净化-气相色谱/三重四极杆串联质谱法测定水体沉积物中7种指示性多氯联苯(PCB28,PCB52,PCB101,PCB118,PCB153,PCB138,PCB180)的方法。通过加速溶剂萃取条件和弗罗里硅土净化剂的优化,一步完成了萃取和净化过程,很好地去除了基质干扰。采用改进的色谱柱提高了分析效率,通过优化三重四极杆串联质谱的离子对(母离子/子离子)、碰撞电压、扫描峰宽等条件,显著提高了7种多氯联苯的灵敏度。7种多氯联苯在0.1~50μg/L浓度范围内线性良好,线性系数(R2)为0.9997~0.99993,方法检出限为0.005~0.010μg/kg。在2.0μg/kg和20.0μg/kg两个浓度添加水平,其回收率为83.5%~96.1%和85.1%~97.5%,相对标准偏差(RSD)为2.4%~7.6%和1.5%~8.2%。该方法已成功应用于实际水体沉积物中多氯联苯的测定。A method has been developed by using accelerated solvent extraction （ASE） and clean-up coupled with gas chromatography-triple quadrupole mass spectrometry （GC-QqQ/MS/MS） for simultaneous extraction , clean-up and determination of 7 indicator polychlorinated biphenyls （PCBs） in sediments, including PCB28, PCB52, PCB101, PCB118, PCB153, PCB138 and PCB180. The matrix interference was eliminated well by optimization of the conditions of simultaneous extraction and clean- up. The analysis efficiency was increased by use of improved chromatographic column. The detection sensitivity of 7 PCBs was improved markedly by optimizing conditions of ion pairs （ precursor ion/ product ion） , collision voltage, the scanning peak width of triple quadrupole mass spectrometry. The good correlation coefficients（ R2） for 7 PCBs were 0. 9997 - 0. 99993 in the range of 0. 1 - 50 μg/L. The limits of detection were 0. 005 - 0. 010 μg/kg. At the spiked levels of 2. 0 μg/kg and 20. 0 μg/kg, the recoveries range from 83.5% to 96. 1% and from 85.1% to 97.5% with the relative standard deviations（RSD） of 2. 4% -7.6% and 1.5% -8.2%, respectively. This method has been applied for determination of PCBs in actual sediments.

关 键 词：沉积物 多氯联苯 气相色谱/串联质谱 加速溶剂萃取 

分 类 号：X131.2[环境科学与工程—环境科学]