固相萃取-气相色谱质谱法同时测定稻田水产品中11种农药残留  

Simultaneous Determination of Eleven Pesticide Residues in Rice-field Aquatic Products Using Solid Phase Extraction-gas Chromatography/Mass Spectrometry

作　　者：孙秀梅[1] 郝青[1] 金衍健[1] 胡红美[1] 郭远明[1] 尤炬炬[1] Sun Xiumei;Hao Qing;Jin Yanjian;Hu Hongmei;Guo Yuanming;You Juju(Marine Fisheries Research Institute of Zhejiang, Key Laboratory of Sustainable Utilization of Technology Research for Fishery Resource ofZhejiang Province, Zhoushan 316021,China)

机构地区：[1]浙江省海洋水产研究所浙江省海洋渔业资源可持续利用技术研究重点实验室,浙江舟山316021

出　　处：《山东化工》2017年第21期83-84,87,共3页Shandong Chemical Industry

基　　金：浙江省科技计划项目(2016F30021;2017F10020)

摘　　要：建立了同时测定稻田水产品中敌敌畏、莠去津、毒死蜱、丁草胺、噻虫嗪、DDT(p,p'-ddt,o,p'-ddt,p.p'-dde,p,p'-ddd)、氯氰菊酯、苯醚甲环唑11种农药残留的固相萃取/气相色谱-质谱检测方法。样品经饱和氯化钠溶液浸泡、乙腈振荡提取,上清液过无水硫酸钠-氧化铝-硅胶固相萃取小柱进行固相萃取净化,正己烷丙酮混合溶液洗脱,浓缩后正己烷定容,气相色谱质谱在选择离子监测模式下检测分析。实验结果表明:在20~1000μg/L浓度范围内,11中农药的进样浓度与其对应的峰面积见呈良好的线性关系,相关系数均大于0.995,方法检出限为5.0~15μg/kg。在0.020、0.040和0.100 mg/kg^3个添加水平下,11种农药在稻田水产品中的平均回收率为76%~113%,RSD值为2.8%~11.9%。利用该方法对黑龙江、吉林和辽宁共75个稻田养殖水产品中的11种农药残留情况进行检测,毒死蜱、丁草胺、p,p'-DDE及p,p'-DDD在样品中有检出。该方法高效、快速、准确度高,能够满足大批量稻田水产品中农药残留的检测分析需要。A gas chromatography-mass spectrometry based method has been developed for multi-determination of eleven pesticide residues（ including dichlorvos,atrazine,chlorpyrifos,butachlor,thiamethoxam,o,p＇-ddt,p. p＇-dde,p,p＇-ddd,p,p＇-ddt,cypermethrin,difenoconazole） in rice-field aquatic products. The homogenized sample was dispersed by sodium chloride solution. The analytes were extracted by acetonitrile. The extracts are cleaned up throuth anhydrous sodium sulfate-Alumina-Silica column. The SPE column was eluted by the mixture solution of hexane： acetone. The analytes were then analyzed by GC-MS using selective iom monitoring（ SIM） with positive electron impact ion source. The results showed that in the spiked levels of0. 020、0. 040 and 0. 100 mg/kg,the average recoveries ranged from 76% to 113%,with the relative standard deviations ranged from 2. 8% to 11. 9%. This method was used to analyze the real samples in Heilongjiang,Jilin and Liaoning province. 75 samples of rice-field aquatic products were selected,and four pesticides in those samples were detected. The other pesticides were not detected. The results indicated that this method is highly efficient,with goood sensitivity and accuracy,which can meet the detection requirements of the above 11 pesticide residues in rice-field aquatic products.

关 键 词：固相萃取 气相色谱质谱 稻田水产品 农药残留 

分 类 号：O657.63[理学—分析化学]