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

发布时间：2018-06-21 12:59

本文选题：净化 + 沉积物　；参考：《分析试验室》2017年03期

【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。
[Abstract]:The effects of different solid phase extraction columns on the purification of sediment extracts and on the baseline of gas chromatography microelectron capture detector (GC ECD) were compared. A gas chromatographic method for the determination of 15 organochlorine pesticides in sediments was established. Ten g air-dried sediment samples were added 1 g Cu powder and 3 g anhydrous Na _ 2SO _ 4 to extract 60 cycles in Soxhlet extraction system with 100 mL petroleum ether-acetone 1: 1 V / V). The extraction solution was purified by GC-ECD with graphitized carbon black (Pesticarb) solid phase extraction column. The results showed that there was a good linear relationship between the 15 organochlorine pesticides in sediments, the detection limit was 0.035 ~ 0.464 渭 g / kg, the quantitative limit was 0.12 ~ 1.55 渭 g / kg, the average recovery rate of 15 organochlorine pesticides purified by Pesticarb-SPE was 94.8 and the relative standard deviation was 1.6 ~ 6.8 渭 g 路kg ~ (-1). The method was applied to the monitoring of surface and bottom sediments in Xixi Wetland. In 32 samples, all pesticides except Aldrin were detected to some extent.
【作者单位】：中国林业科学研究院亚热带林业研究所;杭州市富阳区食品安全检验检测中心;
【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
【分类号】：X839.2;O657.71

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