ASE萃取-GPC净化-GC／ECD测定小麦中有机氯农残和多氯联苯

J4 ›› 2011, Vol. 46 ›› Issue (1): 11-15.

ASE萃取-GPC净化-GC／ECD测定小麦中有机氯农残和多氯联苯

薛海全¹,崔兆杰¹*,杜世勇²

1. 山东大学环境科学与工程学院, 山东济南 250100;
2. 济南市环境监测站, 山东济南 250014

收稿日期:2010-02-01 出版日期:2011-12-14 发布日期:2011-03-16
通讯作者: 崔兆杰(1963-),男,教授,博士生导师,研究方向为环境监测与清洁生产. Email:cuizj@sdu.edu.cn
作者简介:薛海全(1986-),男,硕士研究生,研究方向为持久性有机污染物监测分析.Email:blue8614@126.com
基金资助:
山东省自然科学基金资助项目(Z2008E04);山东省环境保护科技计划资助项目(［2006］048)

Determination of organochlorine pesticides and polychlorinated biphenyls in wheat by gas chromatography with accelerated solvent extraction and gel permeation chromatography cleanup

XUE Hai-quan¹, CUI Zhao-jie¹*, DU Shi-yong²

1. School of Environmental Science and Engineering, Shandong University, Jinan 250100, Shandong, China;
2. Jinan Environmental Monitoring Center, Jinan 250014, Shandong, China

Received:2010-02-01 Online:2011-12-14 Published:2011-03-16

摘要/Abstract

摘要：

建立了加速溶剂萃取、全自动在线凝胶渗透色谱-浓缩联用系统和氟罗里硅土柱前处理、GC／ECD测定小麦样品中7种多氯联苯(PCBs)和7种有机氯农药(OCPs)的分析方法,并优化了加速溶剂萃取、凝胶渗透色谱净化、GC／ECD的分析条件。结果表明,该方法的样品加标回收率和相对标准偏差分别为:多氯联苯69.8％～87.4％、1.48％～11.0％;有机氯农药70.4％～113.9％、3.54％～17.0％。方法检测限为0.03～0.29μg／kg。用该方法测得小麦样品中7种PCBs质量分数范围为0～157.9μg／kg;7种OCPs质量分数在2.38～10.02μg／kg范围内。该方法快速、灵敏、准确,并且在一个流程中可以同时测定小麦样品中多氯联苯和有机氯农残,适合于大批量样品的测定。

关键词: 小麦;有机氯农残;多氯联苯;加速溶剂萃取;凝胶渗透色谱

Abstract:

A new analytical method was developed for the determination of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in wheat samples. The extraction and purification procedures, accelerated solvent extraction (ASE) and gel permeation chromatography (GPC) cleanup were respectively presented by optimizing different extraction conditions and the fraction collection time. The detection conditions could be achieved by gas chromatography with electroncapture detection (GC／ECD). The results showed that the method recovery percentages and relative standard deviations (RSD) were 69.8％～87.4％ and 1.48％～11.0％ for PCBs, 70.4％～113.9％ and 3.54％～17.0％ for OCPs. The method detection limits (MDL) ranged in 0.03～0.29μg／kg. This analytical method was applied to exam the wheat samples collected from Shanghe of Jinan city, Shandong province. The concentrations of these seven kinds of PCBs ranged in 0～157.9μg／kg, and the concentration of these seven kinds of OCPs 2.38～10.02μg／kg. The method was suitable for batch samples with high accuracy, sensitivity and less pre-treatment time, meanwhile, by which the PCBs and OCPs could be analyzed simultaneously. Therefore, it is an ideal choice for determining PCBs and OCPs in wheat.

Key words: wheat; organochlorine pesticides; polychlorinated biphenyls; accelerated solvent extraction; gel permeation chromatography

薛海全1,崔兆杰1*,杜世勇2. ASE萃取-GPC净化-GC／ECD测定小麦中有机氯农残和多氯联苯[J]. J4, 2011, 46(1): 11-15.

XUE Hai-quan1, CUI Zhao-jie1*, DU Shi-yong2. Determination of organochlorine pesticides and polychlorinated biphenyls in wheat by gas chromatography with accelerated solvent extraction and gel permeation chromatography cleanup[J]. J4, 2011, 46(1): 11-15.

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