摘要
[目的]建立一种超高效液相色谱-串联质谱的分析方法,同时测定小麦籽粒和秸秆中砜吡草唑及其3个代谢物的残留量。[方法]样品经乙腈-水混合溶液提取,十八烷基硅烷键合硅胶吸附剂净化,超高效液相色谱分离,三重四极杆串联质谱的多反应监测模式检测,采用基质匹配外标法定量。[结果]砜吡草唑及其3个代谢物在0.1~100 ng/L质量浓度范围内呈现出良好的线性关系(r > 0.999),在小麦籽粒和秸秆中的添加质量分数分别为0.002、0.01、0.5 mg/kg时,砜吡草唑及其3种代谢物(M-1、M-3、M-25)在小麦籽粒和秸秆中的平均回收率为82.0%~110.1%,相对标准偏差为0.9%~13.9%。[结论]方法灵敏度高、准确度好、精密度优良,完全满足农药残留分析的技术要求,适用于小麦中砜吡草唑及其代谢物的残留检测。
[Aims]To establish an ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLCMS/MS)method for the simultaneous determination of pyroxasulfone and its three metabolites in wheat grains and straw.[Methods]Samples were extracted with an acetonitrile-water mixture,purified using octadecylsilane-bonded silica gel(C18)adsorbent,separated by UHPLC,and detected in multiple reaction monitoring(MRM)mode with a triple quadrupole tandem mass spectrometer.Matrix-matched external standard calibration was employed for quantification.[Results]Pyroxasulfone and its three metabolites(M-1,M-3,M-25)exhibited excellent linearity(r>0.999)in the concentration range of 0.1-100 ng/L.At spiked levels of 0.002,0.01 and 0.5 mg/kg in wheat grains and straw,the average recoveries ranged from 82.0%to 110.1%,with relative standard deviations(RSDs)of 0.9%-13.9%.[Conclusions]The method demonstrates high sensitivity,accuracy and precision,fully meeting the technical requirements for pesticide residue analysis,and is suitable for the determination of pyroxasulfone and its metabolites in wheat matrices.
作者
秦晓彤
陈莉
王东
吴俊学
张高铭
郑永权
贺敏
QIN Xiaotong;CHEN Li;WANG Dong;WU Junxue;ZHANG Gaoming;ZHENG Yongquan;HE Min(Institute of Plant Protection,Beijing Academy of Agriculture and Forestry Sciences,Beijing 100097,China;College of Plant Health and Medicine,Qingdao Agricultural University,Qingdao 266109,Shandong,China)
出处
《农药》
北大核心
2025年第12期896-903,共8页
Agrochemicals
基金
国家重点研发项目(2023YFD1701300)
国家重点研发项目(2022YFD1401200)。
