饮水中16种多环芳烃和6种多氯联苯的固相微萃取-气相色谱-三重四极杆质谱同时测定法

Simultaneous determination of 16 kinds of PAHs and 6 kinds of PCBs in drinking water by automated solid phase micro-extraction coupled with gas chromatography-triple quadrupole mass spectrometry

目的建立饮用水中16种多环芳烃（polycyclic aromatic hydrocarbons, PAHs ）和6种多氯联苯（ polychlorinated biphenyls, PCBs）的自动固相微萃取（SPME）-气相色谱-三重四极杆质谱（Gc—QqQ—MS／MS）同时测定方法。方法选用100μm聚二甲基硅氧烷（PDMS）萃取纤维，于50℃、以350r／min振动萃取30min；在GC进样口经280℃解吸6min后，采用气相色谱-三重四极杆质谱在多反应监测（MRM）模式下进行测定。结果在0．5～5μg／L的线性范同内，该方法对水中16种PAHs和6种PCBs所得的回归方程均具有较好的线性关系，r值为0．9914-0．9991。方法的检出限为0．0003～0．054μg/L，回收率为85．5％～124．5％，相对标准偏差为5．8％～15．2％。结论该方法简便、快速、灵敏，能同时准确定性定量测定饮用水中16种PAHs和6种PCBs。

Objective To develop a method for the simultaneous analysis of 16 polycyclic aromatic hydrocarbons （PAHs） and 6 polyehlorinated biphenyls （PCBs） in drinking water based on automated solid phase micro-extraction （SPME） coupled to gas chromatography-triple quadrupole mass spectrometry. Methods 100 μm polydimethylsiloxane （PDMS） was used in extraction at 50 ℃ for 30 min, along with stirring at 350 r/min. The sample extracts were desorbed for 6 min at 280 ℃ directly in the gas chromatograph injector port and analyzed by GC-QqQ-MS/MS in the multi-reaction monitoring （MRM） mode. Results The method showed a good linear relationship for 16 PAHs and 6 PCBs in the range of 0.5-5 μg/L,the linear correlation coefficients were 0.991 4-0.999 1. The limits of detection were 0.000 3-0.05 μg/L with recoveries of 85.5%-124.5% and relative standard deviations of 5.8%-15.2% （n=6）. Conclusion The method is simple,rapid,sensitive and applicable to qualitative and quantitative determination of 16 PAHs and 6 PCBs in drinking water at one time.