气相色谱-串联质谱法测定贝类中指示性多氯联苯  

Determination of Polychlorinated Biphenyls in Seashell by Gas Chromatography-tandem Mass Spectrometry

作　　者：孙伟红[1,2] 魏志强 冷凯良[1,2] 王志杰[1,2] 翟毓秀[1,2] 

机构地区：[1]农业部海洋渔业资源可持续利用重点开放实验室中国水产科学研究院黄海水产研究所,山东青岛266071 [2]国家水产品质量监督检验中心,山东青岛266071 [3]青岛市环境监测中心站,山东青岛266003

出　　处：《分析科学学报》2009年第6期647-651,共5页Journal of Analytical Science

基　　金：农业部948资助项目(No.2006G56);国家科技支撑计划项目(No.2007BAD62B02);国家863计划项目(No.2008AA100805)

摘　　要：研究并建立了测定贝类中多氯联苯残留的气相色谱-串联质谱（GC—MS／MS）方法。通过正己烷和丙酮的混合溶液超声提取，硅胶柱净化，旋转蒸发浓缩，采用GC—MS／MS多反应监测（MRM）方式测定，可同时对贝类中的7种指示性多氯联苯进行定性和定量。研究结果表明：7种指示性多氯联苯的检出限（S／N=3）为0．0066～0．0098μg／kg，定量限（S／N=10）为0．02μg／kg；在0．1～50．0ng／mL时峰强度与质量浓度的线性关系良好（r〉0．99）。方法的平均回收率为73％～113％。该法简便快捷，降低了分析成本，在一定程度上实现了持久性污染物的快速检测和确证。A method for determining residues of seven polychlorinated biphenyls （7 PCBs） in seashell was developed by gas chromatography-tandem mass spectrometry. The sample was extracted with blended solution of hexane and acetone, cleaned-up by column of silica gel, and concentrated with a rotary evaporator. The mass spectrometer was operated using multiple reaction monitoring （MRM）for qualitative and quantitative analysis of 7 PCBs in seashell at the same time. The results showed that the limits of detection for 7 PCBs were 0. 0066- 0. 0098 μg/kg （S/N= 3）, and the limits of quantitation were 0.02 μg/kg （S/N=10）. The method was linear over the range from 0.1 ng/mL to 50 ng/mL with correlation coefficients 〉0. 99, and the average recoveries for 7 PCBs were between 73% and 113%. The method is simple, fast and low cost, which facilitates the fast analysis of the permanent contaminations.

关 键 词：多氯联苯 贝类 气相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]