加速溶剂萃取-GC-MS/MS法检测土壤中5种有机氯农药残留  

ASE-GC-MS/MS Method for Determination of 5 Organochlorine Pesticides Residuals in Soil

作　　者：张文锦 后小龙 付宁 ZHANG Wenjin;HOU Xiaolong;FU Ning(Gansu Province Dingxi City Environmental Monitoring Station,Dingxi 743000)

机构地区：[1]甘肃省定西市环境监测站,定西743000

出　　处：《食品工业》2020年第7期263-266,共4页The Food Industry

摘　　要：建立加速溶剂萃取(ASE)-气相色谱质谱联用(GC-MS/MS)法同时测定土壤中的5种常见有机氯农药(艾氏剂、狄氏剂、氯丹、七氯和五氯硝基苯)残留量的分析方法。选用乙酸乙酯-正己烷(1︰1,V/V)作为萃取溶剂,采用加速溶剂萃取仪对过筛后的土壤样品进行萃取、净化。通过优化质谱分析参数和加速溶剂萃取条件,样品于气相色谱质谱仪上运用多反应监测模式(MRM)进行分析,外标法定量。结果表明:5种有机氯农药在0.04~4.0μg/mL质量浓度范围内线性关系良好。检出限为:艾氏剂0.008 mg/kg,狄氏剂0.010 mg/kg,氯丹0.006 mg/kg,七氯0.006mg/kg,五氯硝基苯0.007 mg/kg。5种有机氯农药3个不同浓度点(0.2,0.8和1.5 mg/kg)的加标回收率在86.9%~100.7%之间,6针进样精密度测试相对标准偏差(RSD)小于5%。该方法前处理简单,定性及定量结果准确,适用于土壤中有机氯农药残留的监测。It was to establish accelerated solvent extractor(ASE)-GC-MS/MS method for determination of 5 organochlorine pesticides(aldrin,dieldrin,chlordane,heptachlor and quintozene)residuals in soil.Hexane and ethyl acetate solution(1︰1,V/V)were selected as extraction solvent,sifted soil samples were extracted and purified on accelerated solvent extractor(ASE).By optimizing mass spectrometry parameters and accelerated solvent extraction conditions,samples were analyzed on GCMS/MS using multiple response monitoring(MRM)mode,external standard method for quantitative.The result showed that the 5 organochlorine pesticide residuals showed good linear relationships in the concentration range 0.04-4.0μg/mL.The detection limits were as follows:aldrin 0.008 mg/kg,dieldrin 0.010 mg/kg,chlordane 0.006 mg/kg,heptachlor 0.006 mg/kg and quintozene 0.007 mg/kg.Recoveries of 5 organochlorine pesticides in 3 different concentration levels were ranged from 86.9%to 100.7%.The relative standard deviation(RSD)which measured by 6 needle injection precision was below 5%.The method was simple in pretreatment,accurate in qualitative and quantitative results,and it was suitable for detection of organochlorine pesticides in soil.

关 键 词：加速溶剂萃取 气相色谱串联质谱 土壤 有机氯 艾氏剂 

分 类 号：O657.63[理学—分析化学] S481.8[理学—化学]