UPLC-MS/MS测定西瓜中噁霉灵和吡唑醚菌酯的残留量  

Determination of Hymexazol and Pyraclostrobin in Watermelon by UPLC-MS/MS

作　　者：侯根连 曾利红 俞泉[4] HOU Gen-lian;ZENG Li-hong;YU Quan(National Engineering Research Center for Agrochemicals,Hunan Research Institute of Chemical Industry Co.,Ltd.,Changsha 410014,China;Hunan Province Key Laboratory for Agrochemicals,Changsha 410014,China;Hunan J&F Test Co.,Ltd.,Changsha 410014,China;Hunan University of Humanities,Science and Technology,Loudi 417000,China)

机构地区：[1]湖南化工研究院有限公司国家农药创制工程技术研究中心,湖南长沙410014 [2]农用化学品湖南省重点实验室,湖南长沙410014 [3]湖南加法检测有限公司,湖南长沙410014 [4]湖南人文科技学院,湖南娄底417000

出　　处：《精细化工中间体》2020年第5期73-76,共4页Fine Chemical Intermediates

基　　金：国家自然科学基金项目(21572050)。

摘　　要：建立了超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定西瓜中噁霉灵、吡唑醚菌酯残留量的方法。样品用乙腈提取,过0.22μm有机系滤膜,以0.1%甲酸水溶液-乙腈为流动相梯度洗脱,多反应监测(MRM)模式下,正离子扫描,外标法定量。结果表明:方法在0.001~0.1μg·m L-1范围内线性良好,相关系数(R2)>0.99;在0.02、 0.5、 2.0 mg·kg-13个添加水平下,噁霉灵和吡唑醚菌酯的平均回收率分别为96%~109%和90%~99%,相对标准偏差分别为1%~3%和1%~4%,定量限为0.005 mg·kg-1。A method for rapid determination of Hymexazol and Pyraclostrobin in watermelon by ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) was established. Samples were prepared through extraction using acetonitrile followed by filtration using 0.22 μm organic filtration membrane. 0.1%formic acid water/acetonitrile was used as mobile phase and the multi-reaction monitoring(MRM) mode was used to measure the samples. The results showed that the linear range of the method was 0.001 ~0.1 mg·kg-1, and the determination coefficient(R2) was more than 0.99. At the three levels including 0.02, 0.5 and 2.0 mg·kg-1, the average recovery of the Hymexazol and Pyraclostrobin was 96%~109% and 90%~99%, the RSD were 1%~3% and1%~4%. The limit of quantification was 0.005 mg·kg-1.

关 键 词：UPLC-MS/MS 噁霉灵 吡唑醚菌酯 西瓜 残留检测 

分 类 号：O657.7[理学—分析化学]