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

doi:10.3785/j.issn.1008-9497.2017.01.015

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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：2 g样品与4 g酸性硅胶固相分散剂研磨10 min，混合物装入预先填好4 g无水硫酸钠和4 g酸性硅胶的玻璃柱中，以50 mL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2~200 ng·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75~950 pg·g^-1，可以满足土壤中痕量多溴联苯醚残留分析的要求.

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	魏孜
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	孙建腾

关键词 ：多溴联苯醚, 土壤, 基质固相分散, 气相色谱质谱法

Abstract：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 (R²>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% (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.

Key words： polybrominated diphenyl ethers soil matrix solid phase disperse GC/MS

收稿日期: 2016-01-28

ZTFLH:	O657
	X53

基金资助: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）

通讯作者: 孙建腾,ORCID:http://orcid.org/0000-0003-0014-199X,E-mail:sunjianteng@zju.edu.cn E-mail: sunjianteng@zju.edu.cn

作者简介: 魏孜(1986-),ORCID:http://orcid.org/0000-0002-3980-997X,女,硕士,助理实验师,主要从事环境有毒污染物的分析检测技术研究,E-mail:weizi@zju.edu.cn.

引用本文:

魏孜, 朱亚尔, 宋瑶, 张瑜铎, 孙建腾. 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[J]. 浙江大学学报（理学版）, 2017, 44(1): 106-111.
WEI Zi, ZHU Yaer, SONG Yao, ZHANG Yuduo, SUN Jianteng. Determination of 13 polybrominated diphenyl ethers in soil by matrix solid phase dispersion method and gas chromatography/mass spectrometry. Journal of ZheJIang University(Science Edition), 2017, 44(1): 106-111.

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http://www.zjujournals.com/sci/CN/10.3785/j.issn.1008-9497.2017.01.015 或 http://www.zjujournals.com/sci/CN/Y2017/V44/I1/106

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