【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。更多还原

【Abstract】 [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.更多还原