基质固相分散-气相色谱/质谱法测定土壤中13种多溴联苯醚  

Determination of 13 polybrominated diphenyl ethers in soil by matrix solid phase dispersion method and gas chromatography/mass spectrometry

作　　者：魏孜[1] 朱亚尔[1] 宋瑶[2] 张瑜铎 孙建腾 WEI Zi ZHU Yaer SONG Yao ZHANG Yuduo SUN Jianteng(Analysis Center of Agrobiology and Environmental Sciences, Zhejiang University, Hangzhou 310058, China Department of Environmental Science, Zhejiang University, Hangzhou 310058, China)

机构地区：[1]浙江大学农生环测试中心,浙江杭州310058 [2]浙江大学环境科学系,浙江杭州310058

出　　处：《浙江大学学报（理学版）》2017年第1期106-111,共6页Journal of Zhejiang University（Science Edition）

基　　金：浙江大学实验技术研究项目(SYB201409);国家重点基础研究计划项目(2014CB441101);浙江省自然科学基金资助项目(LY14B070009)

摘　　要：建立了基质固相分散萃取-气相色谱/质谱法测定土壤中13种多溴联苯醚的分析方法.对固相分散剂种类、样品与分散剂用量比例、洗脱溶剂及用量进行了选择和优化.最佳前处理条件为:2g样品与4g酸性硅胶固相分散剂研磨10min,混合物装入预先填好4g无水硫酸钠和4g酸性硅胶的玻璃柱中,以50mL正己烷/二氯甲烷(v:v=1:1)混合液洗脱并浓缩至0.5 mL,进GC-MS分析.13种多溴联苯醚在2~200ng·g^(-1)内呈良好的线性关系(R2>0.992).平均加标回收率在81%~103%,相对标准偏差(RSD)小于15%(n=3),方法检出限为75~950pg·g^(-1),可以满足土壤中痕量多溴联苯醚残留分析的要求.A matrix solid phase dispersion extraction-gas chromatography/mass spectrometric method has been developed for the determination of 13 polybrominated diphenyl ethers in soil. Parameters including species of solid-phase dispersant, ratios of sample to dispersant, elution species and amount have been optimized. The best pretreatment conditions are as follows： 2 g sample was mixed with 4 g acidic silica, and then grinded for 10 min. The mixture was loaded into a glass column pre-filled with 4 g anhydrous sodium sulfate and 4 g acidic silica. Hexane/dichloromethane （v：v=1：1, 50 mL） mixture was used as eluent. The elution was concentrated to 0.5 mL prior to GC/MS analysis. 13 kinds of PBDEs all show good linear relationships （R^2〉 0. 992） in the range from 2 to 200 ng · g^-1. The average recoveries are 81% to 103% and the relative standard deviation is less than 15 M （n= 3）. The method detection limits ranged from 75 to 950 pg · g^-1, which meets the need for the analysis of trace PBDEs in soil.

关 键 词：多溴联苯醚 土壤 基质固相分散 气相色谱质谱法 

分 类 号：O657[理学—分析化学] X53[理学—化学]