超高效液相色谱-串联质谱法测定蜂蜜中氟虫腈及其代谢物残留量  

Determination of Fipronil and Its Metabolites in Honey by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：郑坤明 陈劲星 陈冬花 连文浩 徐佳 薛伟[2] 张钰萍[2] 苏建峰 胡德禹[2] ZHENG Kun-ming;CHEN Jin-xing;CHEN Dong-hua;LIAN Wen-hao;XU Jia;XUE Wei;ZHANG Yu-ping;SU Jian-feng;HU De-yu(Fujian CF-Fifrach Food Safety Testing Co.,Ld,Fuzhou 350028,China;Research and Development Center for Fine Chemicals,State Key Laboratory Breeding Base of Green Pesticide and Agricultural Bioengineering,Key Laboratory of Green Pesticide and Agricultural Bioengineering,Minstry of Education,Guizhou University,Guiyang 550025,China)

机构地区：[1]福建中检华日食品安全检测有限公司,福州350028 [2]贵州大学精细化工研究开发中心,绿色农药与农业生物工程国家重点实验室培育基地和教育部重点实验室,贵阳550025

出　　处：《农药》2019年第12期898-900,共3页Agrochemicals

基　　金：国家自然科学基金(21667007)

摘　　要：[目的]建立超高效液相色谱-串联质谱法同时测定蜂蜜中氟虫腈及其代谢物残留量的分析检测方法。[方法]蜂蜜样品用乙腈提取,50 mg无水硫酸镁、50 mg石墨化炭黑(PSA)和50 mg十八烷基硅烷(C18)净化。氟虫腈及其代谢物采用电喷雾负离子(ESI-)电离,多反应监测(MRM)模式检测,基质标准溶液外标法定量。[结果]氟虫腈及其代谢物4种化合物在0.001~0.02 mg/L质量浓度范围内线性关系良好(R2>0.99),方法的检出限分别为0.17μg/kg,定量限分别为5.0μg/kg。在5.0、10.0、20.0μg/kg添加水平下,氟虫腈及其代谢物4种化合物的平均回收率为80.9%~94.7%,相对标准偏差(RSD)在0.9%~3.4%之间。[结论]方法简便、快速、灵敏度高、重现性好,适用于蜂蜜中氟虫腈及其代谢物4种化合物的快速测定。[Aims] An analytical method for the simultaneous determination of fipronil and its metabolite residues in honey using ultra performance liquid chromatography-tandem mass spectrometry. [Methods] The samples were extracted with acetonitrile, cleaned up by MgSO4, PSA and C18. Fipronil and its metabolites were performed under in negative electrospray ionization, and multiple reaction monitoring. The quantitative analysis was carried out by external standard method. [Results] A good linear relationship, with the correlation coefficient more than 0.99, was found in the mass concentration range of 0.001-0.02 mg/L. The limit of detection and limit of quantitation were 0.17 and 5 μg/kg,respectively. The recoveries of fipronil and its metabolites at 3 spiked with 5, 10 and 20 μg/kg varied from 80.9 to 94.7% and the relative standard deviations(RSDs) were between 0.9 and 3.4% in honey. [Conclusions] The method is simple, rapid, sensitive and reproducible, which is suitable for rapid determination of fipronil and its metabolites in honey.

关 键 词：蜂蜜 超高效液相色谱-串联质谱 氟虫腈 代谢物 

分 类 号：TQ450.2[化学工程—农药化工]