液相色谱串联质谱法检测草铵膦、草甘膦及其代谢物在水和土壤中的残留  

Determination of glufosinate-ammonium,glyphosate and their metabolites in soil and water by HPLC-MS/MS

作　　者：姬乐园 王平平 朱丽珍 毛连纲[1] 张兰[1] 蒋红云[1] 刘新刚[1] JI Leyuan;WANG Pingping;ZHU Lizhen;MAO Liangang;ZHANG Lan;JIANG Hongyun;LIU Xingang(State Key Laboratory for Biology of Plant Diseases and Insect Pests,Institute of Plant Protection,Chinese Academy of Agricultural Sciences,Beijing 100193,China)

机构地区：[1]中国农业科学院植物保护研究所,植物病虫害综合治理全国重点实验室,北京100193

出　　处：《植物保护》2024年第2期235-239,共5页Plant Protection

基　　金：国家自然科学基金国际(地区)合作与交流项目(32261133527)。

摘　　要：利用超高效液相色谱-串联质谱仪(UHPLC-MS/MS),结合固相萃取净化建立了在水和土壤中同时快速测定草甘膦、草铵膦及其6种代谢物的多残留分析方法。前处理采用Oasis MCX和Oasis MAX固相萃取柱提取,2%甲酸甲醇-水(体积比为1∶1)洗脱,旋干后0.1%氨水定容,UHPLC-MS/MS检测。方法的线性范围为0.02~0.5 mg/L;在水中添加水平为0.0001 mg/L和0.001 mg/L时,草甘膦、草铵膦及其代谢物的回收率为72.8%~94.2%,RSD为2.3%~16.1%;土壤中添加水平为0.001 mg/kg和0.01 mg/kg时,草甘膦、草铵膦及其代谢物的回收率为70.6%~88.5%,RSD为3.6%~12.8%。本方法准确、灵敏、全面,适用于草甘膦、草铵膦及其代谢物在水土环境中的残留检测及监测。An ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)combined with solid-phase extraction purification was used to establish a multi-residue analysis method for the simultaneous determination of glyphosate,glufosinate-ammonium and their six metabolites in water or soil.Oasis MCX and Oasis MAX solid phase extraction columns were used in pre-treatment,and then 2% formic acid methanol water(volume ratio of 1∶1)was used for elution.The eluent collected was evaporated to dryness by a rotary evaporator and diluted with 0.1%ammonia.The linear range of the method was 0.02-0.5 mg/L.Under the spiked level of 0.0001 and 0.001 mg/L in the purified water,the recoveries were 72.8%-94.2% and the relative standard deviations were 2.3%-16.1%,respectively.Under the spiked level of 0.001 mg/kg and 0.01 mg/kg in the soil,the recoveries were 70.6%-88.5% and the relative standard deviations were 3.6%-12.8%,respectively.The method is accurate,sensitive and comprehensive,which could be used to analyze the content of glyphosate,glufosinate-ammonium and their metabolites in low concentration samples in environmental test.

关 键 词：水和土壤 草铵膦 草甘膦 代谢物 UHPLC-MS/MS 残留检测 

分 类 号：S481.8[农业科学—农药学]