超声提取-固相萃取小柱净化-气相色谱法测定土壤中14种有机氯农药  

Determination of Organochlorine Pesticides in Soil Samples by Gas Chromatography with Ultrasonic Extraction and Solid Phase Extraction

作　　者：刘文长[1] 陶文靖[1] 程丽娅[1] 余兴[1] 田旻[1] 黄勤[1] 李胜生[1] 

机构地区：[1]安徽省地质实验研究所,安徽合肥230001

出　　处：《岩矿测试》2009年第6期541-544,共4页Rock and Mineral Analysis

基　　金：国土资源部地质大调查项目资助(1212010511218)

摘　　要：对土壤中14种有机氯农药的超声提取技术和磺化、固相萃取小柱两种净化方法进行系统研究。结果表明,超声提取节省提取时间,提高分析效率;磺化法和固相萃取小柱法都有净化作用,但磺化法使样品中的艾氏剂、狄氏剂和异狄氏剂全部损失;固相萃取小柱净化当丙酮-正己烷淋洗液体积比为1∶9、淋洗液收集8 mL时回收率〉90%,干扰最小。方法检出限为0.63-2.59μg/kg,精密度（RSD,n=7）为1.17%-14.66%,基体加标平均回收率为82.78%-106.94%。方法用于生态地球化学调查评价批量土壤样品的实际分析,检测结果满足评价工作需要。In this paper sample pretreatment techniques including ultrasonic extraction and decontamination techniques of sulfonation and solid phase extraction （SPE） for determination of organochlorine pesticided in soil samples by gas chromatography were presented. The results show that ultrasonic extraction could save the sample treatment time and improve the efficiency of sample analysis. And both of the sulfonation and SPE provide better decontamination effect. But aldrin, dieldrin and endrin in the samples would be lost when sulfonation method was used. Under the optimized condition of acetone/n-hexane = 1 ： 9 and using 8 mL leaching solution in SPE decontamination, the recovery of the analytes was better than 90% and with less interference. Detection limits of the method for organochlorine pesticides were 0.63 - 2.59μg/kg and average recovery was 82.78% - 106.94% with precision of 1.17% - 14.66% RSD （n = 7）. The method has been successfully applied to the determination of organochlorine pesticides in soil samples in Eco-geochemical Investigation and Assessment Program.

关 键 词：有机氯农药 超声提取 磺化 固相萃取 气相色谱法 土壤 

分 类 号：O657.63[理学—分析化学] S482.32[理学—化学]