第 50 卷第 5 期 Vol. 50 No. 5 2020 年 10 月 Oct 2020

所属栏目：分析与测试 UPLC-MS／MS测定西瓜中噁霉灵和吡唑醚菌酯的残留量

侯根连1，2，3，曾利红1，2，3，俞 泉4 （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）

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0.22 μm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0.001~0.1 μg·mL-1范围内线性良好，相关系数（R2）>0.99；在0.02、0.5、2.0 mg·kg-1 3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。

关键词：UPLC-MS／MS；噁霉灵；吡唑醚菌酯；西瓜；残留检测

中图分类号：O657.7　　文献标识码：A　　文章编号：1009-9212（2020）05-0073-04

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

HOU Gen-lian1,2,3, ZENG Li-hong1,2,3, YU Quan4 (1. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry Co.,Ltd., Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China; 3. Hunan J&F Test Co., Ltd., Changsha 410014, China; 4. Hunan University of Humanities, Science and Technology, Loudi 417000, China)

Abstract：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% and 1%~4%. The limit of quantification was 0.005 mg·kg-1.

Key words：UPLC-MS/MS; Hymexazol; Pyraclostrobin; watermelon; detecting residues

基金项目：国家自然科学基金项目（21572050）。

作者简介：侯根连（1979—），女，山西平遥人，主要从事农药残留分析（E-mail:76251033@qq.com）。

收稿日期： 2020-08-1