文献类型：期刊文献

中文题名：固相萃取净化-气相色谱法测定沉积物中15种持久性有机氯农药

英文题名：Determination of 15 organochlorine pesticides in sediments with solid phase extraction by gas chromatography

作者：沈丹玉[1] 袁新跃[2] 邵学新[1] 刘毅华[1] 钟冬莲[1] 莫润宏[1] 汤富彬[1]

第一作者：沈丹玉

机构：[1]中国林业科学研究院亚热带林业研究所;[2]杭州市富阳区食品安全检验检测中心

年份：2017

卷号：36

期号：3

起止页码：277-282

中文期刊名：分析试验室

外文期刊名：Chinese Journal of Analysis Laboratory

收录：CSTPCD;;北大核心:【北大核心2014】；CSCD:【CSCD2017_2018】；

基金：中国林科院基本科研业务费专项资金(CAFYBB2017QA006);浙江省科技厅公益技术应用研究项目(2017C32062)资助

语种：中文

中文关键词：净化;沉积物;有机氯

外文关键词：Clean-up; Sediment; Organochlorine pesticides

分类号：X830.2

摘要：通过比较不同固相萃取柱对沉积物提取液的净化效果和对气相色谱微电子捕获检测器(GC-ECD)基线的影响,建立了沉积物中15种有机氯农药的气相色谱分析方法。10 g风干的沉积物样品加入1 g Cu粉和3 g无水Na2SO4用100 m L石油醚-丙酮(1:1,V/V)于索氏抽提系统提取60个循环,提取液用石墨化炭黑(Pesticarb)固相萃取柱净化,GC-ECD测定。方法学结果表明,沉积物中15种有机氯农药具有良好的线性关系,检出限0.035~0.464μg/kg,定量限0.12~1.55μg/kg,经Pesticarb-SPE净化15种有机氯农药平均回收率为94.8%,相对标准偏差为1.6%~6.8%。方法应用于西溪湿地表层和底层沉积物监测,32个样品中,除了艾氏剂,其余农药均有不同程度的检出。
A method based on solid-phase extraction cartridge and gas chromatography（ GC） was developed for the determination of 15 organochlorine pesticides in sediments. 10 g dry sediment sample adding 1 g copper powder and 3 g anhydrous sodium sulfate with 100 m L of petroleum ether and acetone（ 1： 1,V/V） was used with Soxhlet extraction in 60 cycles. The extracted solutions were cleanup with Pesticarb as dispersive solid phase extraction and determined by GC-ECD. All the 15 pesticides could be completely separated with an excellent linear relationship. The determination limits and quantification limits for the 15 pesticides were 0. 035 ~ 0. 464 μg/kg and 0. 12 ~ 1. 55 μg/kg,respectively. For all the samples,the mean spiked recovery was 94. 8 % with a relative standard deviation（ RSD,n = 3） less than 6. 8 %. The extraction,purification and analysis methods were developed and assessed. The method was successfully applied to the 32 samples from Xixi Wetland region in Hangzhou. Apart from Aldrin,all the other pesticides were detected from the 32 samples. p,p＇-DDE（ 56. 25 %）,δ-BHC（ 31. 25 %） and p,p＇-DDD（ 31. 25 %） showed high detection rates.The pesticides detected in highest concentration were p,p＇-DDT（ 451. 73 μg/kg）, heptachlor（ 205. 83 μg/kg） and α-BHC（ 154. 86 μg/kg）.