论文部分内容阅读
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。
By comparing the effects of different solid phase extraction columns on the purification of sediment extracts and the GC-ECD baseline, a gas chromatographic method was developed for the determination of 15 organochlorine pesticides in sediments. 10 g of air-dried sediment samples were extracted with 1 g of Cu powder and 3 g of anhydrous Na2SO4 for 60 cycles with 100 mL of petroleum ether-acetone (1: 1, V / V) in a Soxhlet extraction system. Purification of carbon black with Pesticarb solid-phase extraction column and determination by GC-ECD. The methodological results showed that the 15 organochlorine pesticides in sediments had a good linear relationship with the detection limits of 0.035 ~ 0.464μg / kg and the limits of quantification of 0.12 ~ 1.55μg / kg. The average recovery of 15 organochlorine pesticides by Pesticarb-SPE The rate was 94.8% with a relative standard deviation of 1.6% -6.8%. The method was applied to the monitoring of sediments in the surface and bottom sediment of Xixi Wetland. Among 32 samples, all the pesticides except for aldrin were detected in different degrees.