液相色谱串联质谱法检测大豆及其植株中异草松、异丙草胺及丙炔氟草胺残留量  

Determination of clomazone,propisochlor and flumioxazin in soybean and its plants by UPLC-MS/MS

作　　者：魏龙兵 梁星 王宽 潘兴鲁 吴小虎[1] 徐军[1] 董丰收[1] 郑永权[1,2] WEI Longbing;LIANG Xing;WANG Kuan;PAN Xinglu;WU Xiaohu;XU Jun;DONG Fengshou;ZHENG Yongquan(State Key Laboratory for Biology of Plant Diseases and Insect Pests,Institute of Plant Protection,Chinese Academy of Agricultural Sciences,Beijing 100193,China;College of Plant Health and Medicine,Qingdao Agricultural University,Qingdao 266109,Shandong,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 [2]青岛农业大学植物医学学院,山东青岛266109

出　　处：《农药》2025年第4期263-268,288,共7页Agrochemicals

基　　金：国家重点研发计划粮油农产品农药残留和生物毒素风险控制技术研究及应用(2023YFD1400904)。

摘　　要：[目的]为了明确大豆田除草剂施用后的作物中农药残留污染水平,基于分散固相萃取-超高效液相色谱-串联质谱技术,建立大豆、青豆、老秸秆、青秸杆中异草松、异丙草胺及丙炔氟草胺的残留分析方法。[方法]样品经1%甲酸乙腈提取,分散固相萃取净化,0.2%甲酸水-乙腈作流动相,C18色谱柱分离,三重四极杆质谱检测,基质外标法定量。[结果]4种基质中3种除草剂在0.01~0.5 mg/kg质量浓度范围内与其峰面积均呈现良好的线性关系,决定系数R2>0.99,3种除草剂在4种基质中的定量限均为0.01 mg/kg。在0.01、0.1、0.5 mg/kg 3个添加水平下4种基质中3种除草剂的平均添加回收率在88.0%~112.6%之间,RSD在1.5%~16.5%之间。48份田间样品均未检出上述3种除草剂残留。[结论]在推荐剂量下使用3种除草剂对大豆地上部位一般不会产生农药残留风险。试验建立的方法简便、高效、灵敏度高,适用于大豆、青豆、老秸秆、青秸杆中异草松、异丙草胺及丙炔氟草胺的测定。[Aims]In order to determine the level of pesticide residues in soybean after applying herbicide,a residue analysis method for clomazone,propisochlor and flumioxazin in soybean,green bean,old soybean straw and green soybean straw was developed using dispersive solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).[Methods]The samples were extracted with acetonitrile containing 1%formic acid,followed by dispersion solid phase extraction purification.The mobile phase comprised 0.2%formic acid aqueous solution and acetonitrile.Separation was achieved using a C18 column,and detection was performed by triple quadrupole mass spectrometry.Quantification was based on external matrix-matched calibration standards.[Results]The three herbicides in 4 matrices showed good linearity with peak areas corresponding to concentrations in the range of 0.01 to 0.5 mg/kg,with coefficients of determination(R2)greater than 0.99.The limits of quantifications(LOQs)for all three herbicides in the four substrates were 0.01 mg/kg.The mean recoveries of clomazone,propisochlor and flumioxazin in 4 matrices at spiked levels of 0.01,0.1 and 0.5 mg/kg ranged from 88.0%to 112.6%,with relative standard deviations(RSDs)between 1.5%and 16.5%.None of the 48 field samples contained detectable residues of the three herbicides.[Conclusions]The application of the three herbicides at recommended doses does not pose a residue risk.The developed method is simple,efficient and highly sensitive,making it suitable for the determination of clomazone,propisochlor and flumioxazin in soybean,green bean,old soybean straw and green soybean straw.

关 键 词：大豆 异草松 异丙草胺 丙炔氟草胺 液质联用 

分 类 号：TQ450.2[化学工程—农药化工]