QuEChERS-高效液相色谱-串联质谱法测定蜜蜂及蜂产品中5种农药及氟虫腈代谢物残留  

Determination of 5 Pesticides and Fipronil Metabolites in Honeybees and Bee Products by QuEChERS-HPLC-MS/MS

作　　者：宋梓豪 张金振[1,2] 周欣欣 陈朗 周艳明 袁善奎 SONG Zi-hao;ZHANG Jin-zhen;ZHOU Xin-xin;CHEN Lang;ZHOU Yan-ming;YUAN Shan-kui(Institute of Apicultural Research,Chinese Academy of Agricultural Sciences,Beijing 100193,China;Bee Products Quality Supervision and Testing Center,Ministry of Agriculture and Rural Affairs,Beijing 100193,China;Institute for the Control of Agrochemicals,Ministry of Agriculture and Rural Affairs,Beijing 100125,China)

机构地区：[1]中国农业科学院蜜蜂研究所,北京100093 [2]农业农村部蜂产品质量监督检验测试中心,北京100193 [3]农业农村部农药检定所,北京100125

出　　处：《农药》2021年第5期347-351,共5页Agrochemicals

摘　　要：[目的]建立蜜蜂及蜂蜜和蜂花粉中氟虫腈、氟甲腈、氟虫腈硫醚、氟虫腈砜、灭幼脲、氟啶脲、氟铃脲、杀铃脲等5种农药及氟虫腈代谢物的QuEChERS-高效液相色谱-串联质谱分析方法(HPLC-MS/MS),并将该方法用于实际样品检测。[方法]样品中的农药残留用乙腈提取,盐析后用C_(18)、PSA吸附剂净化,经C_(18)色谱柱分离,在电喷雾离子源(ESI-),多反应监测模式(MRM)下分析,外标法定量。[结果]方法的线性范围为0.1~100μg/L,相关系数均≥0.999,定量限为1~10μg/kg(S/N=10);在1~50μg/kg范围内的添加回收率为76.2%~117.9%,相对标准偏差≤22.5%。[结论]该方法简单、快速、灵敏、稳定,适合蜜蜂和蜂产品中5种农药及氟虫腈代谢物的检测。[Aims]This study aims to establish a QuEChERS-High Performance Liquid Chromatography-Tandem Massspectrometry(QuEChERS-HPLC-MS/MS)method for the determination of fipronil,fipronil-desulfinyl,fipronil-sulfide,fipronil-sulfone,chlorbenzuron,chlorfluazuron,hexaflumuron,triflumuron in honeybee,honey and bee pollen,and apply to the real samples determination.[Methods]The pesticide residues in samples were extracted with acetonitrile,purified by C_(18),PSA sorbent.It was determined by electrospray ionization negative ion mode(ESI-)multi-reactions monitoring(MRM)and quantitative measurement by means of external standard method.[Results]The linear range of this method was 0.1-100μg/L,the correlation coefficient was greater than 0.999,and the limit of quantitation was 1-10μg/kg(S/N=10).At the spiked concentration ranged from 1-50μg/kg,the recoveries were76.2-117.9%,and the relative standard deviations weres less than 22.5%.[Conclusions]The method is simple,rapid,sensitive and stable.It is suitable for determination of the above five pesticides and fipronil metabolites in honeybees and bee products.

关 键 词：蜜蜂 蜂蜜 蜂花粉 农药 残留检测 

分 类 号：TQ450.2[化学工程—农药化工]