HPLC-MS/MS法同时测定水体中残杀威和高效氯氰菊酯含量  

Determination of propoxur and beta-cypermethrin in water by HPLC-MS/MS

作　　者：何伟 何钰 HE Wei;HE Yu(Guizhou Testing Technology Research and Application Center,Guiyang 550002,China;Guizhou Academy of Testing and Analysis,Guiyang 550014,China)

机构地区：[1]贵州省检测技术研究应用中心,贵阳550002 [2]贵州省分析测试研究院,贵阳550002

出　　处：《世界农药》2024年第1期50-55,共6页World Pesticide

基　　金：流域水环境质量安全的农药监测、预警、应急技术研究与示范(黔科合支撑[2021]一般464)。

摘　　要：利用高效液相色谱-三重四极杆质谱仪建立水体中残杀威和高效氯氰菊酯含量检测方法。采用高效液相色谱串联质谱法,以乙腈-5 mmol/L乙酸铵水溶液(90%+10%)为流动相,使用以Eclipse Plus C18填充的色谱柱和质谱检测器,对水体中的残杀威和高效氯氰菊酯进行测定,外标法定量。结果表明:残杀威和高效氯氰菊酯分别在0.94~47.10、0.63~31.29μg/L质量浓度范围内线性关系良好,相关系数分别为0.9991和0.9994,变异系数分别为0.52%和2.05%,高质量浓度水平的平均回收率分别为102.26%和102.44%,低质量浓度水平的平均回收率分别为90.74%和98.24%。该方法具有操作简便、分离效果好、快速等优点,线性关系、准确度、精密度和灵敏度均满足要求,可用于水体中残留检测和水生生态环境毒理研究。This study aims to establish a high performance liquid chromatography triple quadrupole mass spectrometry for detecting the content of propoxur and beta-cypermethrin in water.Using HPLC-MS/MS method,with mobile phase of acetonitrile-5 mmol/L ammonium acetate aqueous solution(90%+10%),with column by Eclipse Plus C18 packing and MSD detector,propoxur and beta-cypermethrin were determined and quantified by external standard method.The results showed that the linear correlation coefficient between comcentrations of propoxur and beta-cypermethrin and their responding values were 0.9991 and 0.9994 in the mass concentration range of 0.94-47.10 and 0.63-31.29μg/L,the variation coefficient were 0.52%and 2.05%,the average recovery rates of high concentration levels were 102.26%and 102.44%,the average recovery rates of low concentration levels were 90.74%and 98.24%,respectively.The method is simple,effective separation and fast,and its linear relationship,accuracy,precision,and sensitivity all meet the requirements.It can be used for residue detection in water and toxicology research of aquatic ecological environment.

关 键 词：残杀威 高效氯氰菊酯 高效液相色谱-串联质谱法 

分 类 号：TQ450.7[化学工程—农药化工]