分散固相萃取净化-液相色谱串联质谱法测定土壤中灭草松及其代谢产物残留  

Determination of bentazone and its metabolite residues in soil by dispersive solid phase extraction purification-liquid chromatography-tandem mass spectrometry

作　　者：范宏 谭莉 张慧[1] 谷继林 孟繁磊[1] FAN Hong;TAN Li;ZHANG Hui;GU Jilin;MENG Fanlei(Institute of Agricultural Quality Standard and Testing Technology,Jilin Academy of Agricultural Sciences/Risk Assessment Lab of Agri-Products Quality and Safety(Changchun),Ministry of Agriculture and Rural Affairs/Jilin Provincial Key Laboratory of Agro-environment and Agro-products Safety,Changchun 130033,China;Agricultural Comprehensive Administrative Law Enforcement Unit of Dehui City,Dehui 130300,Jilin,China)

机构地区：[1]吉林省农业科学院农业质量标准与检测技术研究所/农业农村部农产品质量安全风险评估实验室(长春)/吉林省农业环境与农产品安全重点实验室,长春130033 [2]吉林省德惠市农业综合行政执法大队,吉林德惠130300

出　　处：《农药》2024年第8期598-603,共6页Agrochemicals

基　　金：吉林省科技厅重点研发(20210202110NC)。

摘　　要：[目的]为建立分散固相萃取净化-液相色谱串联质谱法测定土壤中灭草松及其代谢产物残留量的检测方法。[方法]土壤样品经含0.5%乙酸的乙腈超声辅助提取,7.5 mg GCB、25 mg PSA、150 mg无水硫酸镁混合净化材料净化,C18色谱柱分离,以甲酸水溶液(甲酸为0.1%)-甲醇作为流动相进行梯度洗脱,多反应监测(MRM)负离子模式(ESI-)电离扫描,基质标准曲线外标法定量。[结果]灭草松及其代谢产物在0.1~200μg/L范围内相关系数均大于0.999,方法的检出限(S/N=3)为0.3~2.0μg/kg,定量限(S/N=10)为1.0~7.0μg/kg,加标回收率为90.1%~104.4%,相对标准偏差为1.94%~6.56%。[结论]方法操作简便快速、准确可靠,适用于土壤中灭草松及其代谢产物6-羟基灭草松和8-羟基灭草松残留量的同时检测。[Aims]The aim of this study is to establish a method for the determination of bentazone and its metabolite residues in soil by dispersion solid phase extraction purification-liquid chromatography-tandem mass spectrometry.[Methods]The soil samples were extracted by ultrasonic assisted extraction of 0.5%acidified acetonitrile.The extract was purified by solid phase extraction with mixture of 7.5 mg GCB,25 mg PSA and 150 mg anhydrous magnesium sulfate,separated by C18column,eluted by mobile phases of 0.1%formic acid water-methanol,and quantified by matrix standard curve external standard method with multiple reaction monitoring(MRM)negative ion mode(ESI-)ionization scanning.[Results]The correlation coefficients of bentazone and its metabolites were all greater than 0.999 when the mass concentration was in the range of 0.1-200μg/L,the limit of detection(S/N=3)were0.3-2.0μg/kg,the limit of quantification(S/N=10)were 1.0-7.0μg/kg,the recovery rate were 90.1%-104.4%,and the relative standard deviation were 1.94%-6.56%.[Conclusions]The method is simple,rapid,accurate and reliable,and is suitable for the simultaneous detection of residues of bentazone and its metabolites 6-hydroxybentazone and 8-hydroxybentazone in soil.

关 键 词：分散固相萃取净化 液相色谱串联质谱法 土壤 灭草松 6-羟基灭草松 8-羟基灭草松 

分 类 号：TQ450.2[化学工程—农药化工]