分析化学2013，Vol.41Issue(6)：861-868,8.DOI:10.3724/SP.J.1096.2013.21013
加速溶剂萃取-固相萃取净化-气相色谱/质谱法测定沉积物中多氯联苯和多环芳烃
Simultaneous Determination of 28 Polychlorinated Biphenyls and 16 Polycyclic Aromatic Hydrocarbons in Sediments Using ASE-SPE-GC-QqQ-MS/MS
摘要
Abstract
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.关键词
沉积物/多氯联苯/多环芳烃/气相色谱/串联质谱Key words
Sediment/Polychlorinated biphenyls/Polycyclic aromatic Hydrocarbons/Gas chromatographytriple quadrupole mass spectrometry引用本文复制引用
王道玮,赵世民,金伟,沈秋莹,胡平,黄斌,潘学军..加速溶剂萃取-固相萃取净化-气相色谱/质谱法测定沉积物中多氯联苯和多环芳烃[J].分析化学,2013,41(6):861-868,8.基金项目
本文系国家自然科学基金(No.21267012),国家水体污染控制与治理科技重大专项(No.2010ZX07102-006)和云南省应用基础研究计划项目(No.2012FB124)资助 （No.21267012）
