本文建立了采用液相色谱-串联质谱法测定蜂胶胶囊（以蜂胶为主要原料的保健食品）中多种硝基咪唑类药物（甲硝唑、洛硝哒唑、异丙硝唑、二甲硝基咪唑、羟基甲硝唑、羟甲基甲硝咪唑）残留的检测方法。样品经0.1 mol/L盐酸溶液溶解分散，涡旋混匀，超声提取目标成分，通过HLB SPE小柱净化；采用Waters ACQUITY UPLC® BEH C18（1.7 μm，2.1 m×100 mm）色谱柱进行分离，流动相为0.1%甲酸水溶液-乙腈，梯度洗脱，经三重四级杆串联质谱测定，电喷雾正离子MRM模式检测，离子丰度比定性，外标法定量。结果6种目标分析物线性关系良好，相关系数均大于0.998；在2.5、5.0、10.0 μg/kg三个水平下，回收率为68.12%~92.20%，RSD为1.20%~5.83%；该方法简单可靠，重复性好，推广应用前景较好，能适用于蜂胶保健食品中多种痕量硝基咪唑类药物的同时检测。

In this paper, a method based on liquid chromatography-tandem mass spectrometry for the determination of residues of various nitroimidazoles (metronidazole, lornidazole, isopropynidazole, dimethylnitroimidazole, hydroxymetronidazole, hydroxymethylnitroimidazole) in health food with propolis as the main raw material was established. The samples were dissolved and dispersed with 0.1 mol/L hydrochloric acid solution, mixed well with vortex, then the target components were extracted by ultrasound and purified by HLB SPE column. The extract was separated on a Waters ACQUITY UPLC® BEH C18 column (1.7 μm, 2.1 m×100 mm) with gradient elution using a mobile phase consisting of 0.1% formic acid and acetonitrile. A tandem quadrupole mass spectrometer equipped with electrospray ionization (ESI) source in positive ion mode was employed for the quantitative analysis of the analyte using multiple reaction monitoring (MRM) scanning mode, with ion abundance ratio for qualitative analysis and external standard method for quantitative analysis. Under the optimal conditions, good linearities (R>0.998) were obtained in the related linear ranges. With addition level at 2.5, 5.0, 10.0 μg/kg, the recovery rates were 68.12%~92.20%, the relative standard deviations were 1.20%~5.83%. This method was simple, sensitive, accurate, and reproducible, has great popularization and application value, and could be suitable for the determination of various trace amounts of nitroimidazoles in propolis-derived health foods.

广西食品药品监督管理局科技项目（YJJ16001）；广西中医药大学“岐黄工程”高层次人才团队培育项目（2018002）；广西高等学校高水平创新团队自主计划（桂教2019-52）