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建立了高效液相色谱-串联质谱联用测定蜂王浆中甲硝唑(MTZ)、二甲硝唑(DM Z)和洛硝哒唑3(RNZ)种硝基咪唑类残留的方法。使用氢氧化钠溶液溶解样品后,以乙酸乙酯液液萃取提取蜂王浆样品中的硝基咪唑类残留物。该法简便快捷,适合大批量样品处理。采用氘代二甲硝唑作为内标和利用高选择性反应监测(H-RSM)技术,降低了基质干扰,增加了定量的准确性。实验结果表明DM Z检测下限可以达到1.0μg/kg,MTZ和RNZ检测下限可以达到0.5μg/kg(S/N大于5);DM Z定量下限可以达到2.0μg/kg,MTZ和RNZ定量下限可以达到1.0μg/kg(S/N大于10)。线性范围为2.0~200μg/L,添加回收率为96.6%~110.6%(内标校正),相对标准偏差(RSD)为2.1%~7.4%。
A high performance liquid chromatography-tandem mass spectrometry (LC-MS / MS) method was developed for the determination of nitroimidazole residues in metronidazole (MTZ), metronidazole (DMZ) and ritonadiazole 3 (RNZ) After the sample was dissolved in sodium hydroxide solution, the nitroimidazole residue in the sample of royal jelly was extracted by liquid-liquid extraction with ethyl acetate. The method is simple and fast, suitable for high-volume sample processing. Using deuterodomectron as internal standard and using highly selective reaction monitoring (H-RSM) techniques, matrix interference is reduced and quantitative accuracy is increased. The results showed that the detection limit of DMZ could reach 1.0μg / kg, the detection limit of MTZ and RNZ could reach 0.5μg / kg (S / N greater than 5), the lower limit of DMZ could reach 2.0μg / kg, the lower limit of MTZ and RNZ Reached 1.0 μg / kg (S / N greater than 10). The linear range was 2.0 ~ 200 μg / L, and the recoveries were 96.6% ~ 110.6% (internal standard calibration). The relative standard deviations (RSDs) ranged from 2.1% to 7.4%.