第 49 卷第 5 期 Vol. 49 No. 5 2019 年 10 月 Oct 2019

所属栏目：分析与测试 超高效液相色谱-串联质谱法同时检测葡萄中吡唑醚菌酯、氟吡菌胺及其代谢物（BAM）残留

罗 傲1，陈恒辉1，熊 胜1，张宸宇1，邓小岚1，龚道新1，2* （1. 湖南农业大学 资源环境学院，湖南 长沙 410128；2. 湖南农业大学 农业环境保护研究所，湖南 长沙 410128）

摘　要：建立了超高效液相色谱-串联质谱（UPLC-MS／MS）快速检测葡萄中吡唑醚菌酯、氟吡菌胺及其代谢物2，6-二氯苯甲酰胺（BAM）残留量的方法。葡萄样品用乙腈提取，过0.22 μm有机系滤膜后，在电喷雾正离子模式下以多反应监测（MRM）模式测定，基质校正标准溶液外标法定量。结果表明：方法的线性范围为0.05～2.00 mg·kg-1，决定系数（r）＞0.99；在0.05 mg·kg-1、0.50 mg·kg-1和2.00 mg·kg-1，3个添加水平下，吡唑醚菌酯、氟吡菌胺和2，6-二氯苯甲酰胺（BAM）的平均回收率为91%~97%、91%~93%和94%~100%，相对标准偏差为 4%~7%、1%~3%和2%~3%，定量限为0.05 mg·kg-1。该处理方法准确、简单、快速，是葡萄中吡唑醚菌酯、氟吡菌胺和BAM残留检测理想的办法。

关键词：超高效液相色谱-串联质谱（UPLC-MS／MS）；葡萄；吡唑醚菌酯；氟吡菌胺；2，6-二氯苯甲酰胺（BAM）

中图分类号：O657.7　　文献标识码：A　　文章编号：1009-9212（2019）05-0068-05

Determination of Pyraclostrobin, Fluopyram and Its Metabolites in Grape by Ultra Performance Liquid Chromatography-tandem Mass Spectrometry

LUO Ao1, CHEN Heng-hui1, XIONG Sheng1, ZHANG Chen-yu1, DENG Xiao-lan1, GONG Dao-xin1,2* (1. College of resources and environment, Hunan Agricultural University, Changsha 410128, China; 2. Institute of agricultural environmental protection, Hunan Agricultural University, Changsha 410128, China)

Abstract：A rapid method for the determination of pyraclostrobin ether ester, fluopicolide and its 2,6-dichlorobenzamide(BAM) residues in grapes by ultra-high performance liquid chromatography-tandem mass spectrometry(HPLC-MS) was established. The grape samples were extracted with acetonitrile, and then passed through a 0.22 μm organic membrane. After being monitored by multiple reaction monitoring (MRM) mode under the electrospray ionization mode, the standard solution was corrected by external standard method. The results showed that the linear range of the method was 0.05~2.00 mg·kg-1, and the determination coefficient (r) was > 0.99. At the three levels of 0.05, 0.50 and 2.00 mg·kg-1, the average recovery of pyraclostrobin ether ester, fluopicolide and its 2,6-dichlorobenzamide (BAM) was 91%~97%, 91%~93% and 94%~100%, the relative standard deviation was 4%~7%, 1%~3% and 2%~3%, and the quantitative limit was 0.05 mg·kg-1. The method is stable, accurate and sensitive. It is very suitable for practical operation. This method is accurate, simple and fast, and is an ideal method for the determination of pyrazolyl ester, flupirimide and bam residues in grape.

Key words：ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS); grape; pyraclostrobin ether ester; fluopicolide; 2,6-dichlorobenzamide(BAM)

作者简介：罗 傲（1994-），男，湖南邵阳人，硕士研究生，研究方向：有机污染物检测（E-mail：452729285@qq.com）。

联 系 人：龚道新，教授，主要从事有机污染物检测及治理（E-mail：gdx4910@163.com；E-mail：Author of correspondence）。

收稿日期：2019-10-10