摘要
[目的]建立超高效液相色谱串联质谱法(LC-MS/MS)同时测定土壤中三环唑、福美双、萎锈灵、唑螨酯和苄嘧磺隆5种农药残留的分析方法。[方法]样品加入适量硅藻土研磨均匀后,经乙腈超声提取,离心分层并取上清液经吸附剂净化,以乙腈和0.1%乙酸水溶液梯度洗脱,然后以超高效液相色谱串联质谱仪在多反应监测模式(MRM)下进行定量与定性分析检测。[结果]5种农药质量浓度在0.1~50.0μg/L具有良好的线性关系(R^(2)≥0.995);检出限在0.009~0.022μg/kg;平均加标回收率在71.9%~114.0%;重复性和精密度RSD(n=6)均在10.0%以内。[结论]该方法具有前处理简单、操作简便快速、检测结果准确、重复性好等优点,适用于土壤中的三环唑、福美双、萎锈灵、唑螨酯和苄嘧磺隆5种农药残留的检测。
[Objective]To establish an analytical method for determination of 5 pesticide residue(tricyclazole, thiram, carboxin, fenpyroximate and bensulfuron-methyl) in soil by LC-MS/MS method.[Method]After adding an appropriate amount of diatomaceous earth to the sample and grinding evenly, the sample was ultrasonically extracted with acetonitrile, centrifuged and stratified, and the supernatant was purified by adsorbent, eluted with a gradient of acetonitrile and 0.1% acetic acid aqueous solution, and then quantitative and qualitative analysis and detection were carried out by ultra-high performance liquid chromatography-tandem mass spectrometer in multiple reaction monitoring mode(MRM).[Result]The five pesticides had a good linear relationship between the mass concentrations of 0.1-50.0 μg/L(R^(2)≥0.995);the detection limit was 0.009-0.022 μg/kg;the average spike recovery rate was 71.9%-114.0%;the RSD of repeatability and precision(n=6) were both within 10.0%.[Conclusion]The method has the advantages of simple pretreatment, simple and rapid operation, accurate detection results and good repeatability, etc.It is suitable for the detection of 5 pesticide residues in soil, including tricyclazole, thiram, carboxin, fenpyroximate and bensulfuron-methyl.
作者
汤莹
TANG Ying(SEP Analytical Services(Shanghai)Co.,Ltd.,Shanghai 201108)
出处
《安徽农业科学》
CAS
2022年第21期192-195,共4页
Journal of Anhui Agricultural Sciences
基金
国家重点研发计划(2019YFC1806100)。
