超声辅助萃取气相色谱-三重四极杆质谱法测定室内灰尘中的39种多氯联苯  

Determination of 39 polychlorinated biphenyls in indoor dust using ultrasonic extraction and gas chromatography-tandem mass spectrometry

作　　者：王炳玲[1] 张晓玲[2] 张琦[3] 陆晓梅[2] 崔媛[2] 张正东[3] 

机构地区：[1]青岛市疾病预防控制中心,山东青岛266033 [2]南京医科大学公共卫生学院卫生检验学系,江苏南京211166 [3]南京医科大学公共卫生学院职业医学与环境卫生学系,江苏南京211166

出　　处：《色谱》2014年第1期74-80,共7页Chinese Journal of Chromatography

基　　金：国家自然科学基金面上项目(81072268);江苏省自然科学基金面上项目(BK2010535);江苏省博士后基金(1001017C);江苏高校优势学科建设工程项目

摘　　要：建立了测定室内灰尘样品中39种多氯联苯（PCBs）的分析方法。样品经吸尘器采集、正己烷一二氯甲烷（1：1，v／v）超声萃取、浓缩后，利用气相色谱一三重四极杆质谱法（GC—MS／MS）在选择反应监测（SRM）模式下测定。结果表明，39种PCBs在30min内得到了很好的分离，在0．1～100μg／L范围内线性关系良好，相关系数为0．9910～0．9999，方法的加标回收率为57．2％--120．3％，日内测定的相对标准偏差（RSD）为0．3％-24．7％，日间测定的RSD为0．6％--29．9％，检出限（信噪比为3）为0．0003～0．2080ng／g。本方法灵敏度高、准确度和精密度好，简便快速，溶剂消耗量少，适用于灰尘中多种多氯联苯的同时测定。A method for the determination of 39 polychlorinated biphenyls （PCBs） in indoor dust was developed. A vacuum cleaner was used for gathering the house dust. N-Hexane-di- chloromethane （ 1 ： 1, v/v） was added and the extraction was performed in an ultrasonic bath. The supernatant was concentrated and then 0. 1 mL n-hexane-dichloromethane （ 1 ： 1, v/v） was added. Gas chromatography-tandem mass spectrometry （GC-MS/MS） in selected-reaction monitoring （SRM） mode has been investigated for the determination of the 39 PCBs congeners in indoor dust. The 39 PCBs had highly efficient separation within 30 rain and showed good lin- earity in the range of 0. 1 - 100μg/L with the correlation coefficients of 0. 991 0 - 0. 999 9. The spiked recoveries were 57.2% - 120.3%. The intra-day relative standard deviations （RSDs） were between 0.3% and 24.7%, while the inter-day RSDs were between 0.6% and 29.9%. This method has good linearity, high sensitivity, high accuracy and precision. Also, it is simple, rapid and low solvent consumption. The low chemical background interference allowed it to be used in more complex matrices.

关 键 词：气相色谱-串联质谱 多氯联苯 室内灰尘 

分 类 号：O658[理学—分析化学]