A method for the simultaneous extraction,cleanup,determination of 28 polychlorinated biphenyls (PCBs) and 16 polycyclic aromatic hydrocarbons (PAHs) in sediments has been developed by using accelerated solvent extraction (ASE) and solid phase extraction (SPE) cleanup coupled with capillary gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS).The conditions of extraction,cleanup,and instrumental operating were optimized.The results indicated that the optimal conditions of ASE were operated at 90 ℃ for 6min; the Silica gel-Florisil composite columns (packing the Florida silica,0.7 g activated silica gel,1 g anhydrous sodium from bottom to top) was chosen as column of purification; the optimal elution solvent was mixture solvent of acetone/hexane (1 ∶ 19,V/V),0.6 mL/min was optimum for elution rate.The correlation coefficients (R2) for PCBs and PAHs were 0.9987-0.9999 and 0.9939-0.9999 in the range of 2-500 μg/L and 5-1000 μg/L,respectively.The limits of detection of PCBs and PAHs were in the range of 0.001-0.08 ng/g,0.07-0.45 ng/g,and the limits of quantitation were 0.003-0.25 ng/g,0.24-1.67 ng/g,respectively.The average recoveries of the spiked samples ranged from 95.6％ to 125.7％ with RSD (n=6) of 0.7％-6.4％ for PCBs,and from 70.4％ to 124.7％ with RSD (n=6) of 1.1％-12.8％ for PAHs.The present method was applied for the determination of PCBs and PAHs in surface sediments collected from the estuaries around Dianchi Lake,and the results displayed that the concentrations of PCB congeners ranged from n.d.to 0.13 ng/g,and 0.79 to 131.12 ng/g for PAHs congeners in this area.%建立了加速溶剂萃取-固相萃取净化-气相色谱/三重四极杆串联质谱联用(ASE-SPE-GC-QqQ-MS/MS)法同时测定沉积物中28种多氯联苯(PCBs)和16种多环芳烃(PAHs).对萃取、净化及仪器分析条件进行了优化.优化条件为:ASE萃取温度90℃,萃取时间6 min；净化小柱为硅胶-Florisil固相复合柱(填料自下而上为弗罗里硅土、0.7g活化硅胶、lg无水硫酸钠)；洗脱溶液为丙酮-正己烷(1∶19,V/V)混合溶液,洗脱速率为0.6 mL/min.PCBs和PAHs在2～500 μg/L和5～ 1000 μg/L浓度范围内的线性相关系数(R2)分别为0.9987 ～0.9999和0.9939～0.9999；PCBs和PAHs方法检出限分别为0.001 ～0.08 ng/g和0.07 ～0.45 ng/g；定量限为0.003 ～0.25 ng/g和0.24 ～ 1.67 ng/g;实际样品平均加标回收率为95.6％ ～ 125.7％和70.4％ ～ 124.7％；方法相对标准偏差(n=6)为0.7％ ～6.4％和1.1％～12.8％.运用本方法对滇池入湖河口表层沉积物样品进行测定,该区域PCBs单体浓度为n.d.(未检出)～0.13 ng/g,PAHs单体浓度为0.79 ～ 131.12 ng/g.
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