高效液相色谱-串联质谱法测定蜂胶中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星残留量

Determination of lomefloxacin,pefloxacin,ofloxacin and norfloxacin in propolis by high performance liquid chromatography-tandem mass spectrometry

建立了一种适用于蜂胶中洛美沙星、培氟沙星、氧氟沙星、诺氟沙星残留检测的Qu ECh ERS-高效液相色谱串联质谱方法。样品中的蜂胶经叔丁基甲醚溶解,以5%甲酸水溶液提取喹诺酮类药物,并以乙腈、无水Mg SO4、Na Cl为复提取溶剂和盐析剂;通过正交实验,优选了150 mg无水硫酸镁、50 mg N-丙基乙二胺、50 mg封端十八烷基键合硅胶的组合为吸附剂,有效减少复杂基体的干扰。试样溶液经HPLC-MS/MS测定,内标法定量。4种喹诺酮类药物线性范围为2.0~100 ng/m L,相关系数均大于0.9997;方法检出限和定量限分别为0.75μg/kg和2.0μg/kg,平均回收率为67.4%~96.2%,相对标准偏差RSD(n=6)为1.6%~8.6%。方法可用于蜂胶中4种禁用喹诺酮类药物残留的风险监测。

A method for the determination of lomefloxacin,pefloxacin,ofloxacin and norfloxacin in propolis was developed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Four kinds of quinolones(QNs)were extracted by 5%formic acid after the dissolution of the sample with methyl tert-butyl ether(MTBE).The sample extracts were re-extracted by acetonitrile with magnesium sulfate andsodium chloride.The optimized conditions for clean-up reagents were 150 mg anhydrous magnesium sulfate,50 mg octadecylsilane and 50 mg N-propylethylenediamine according to the orthogonal test.The detection of QNs were carried out by HPLC-MS/MS and the quantification was performed by the internal standard method.The calibration curves of QNs showed a good linearity in the range of 2.0-100 ng/m L with r≥0.9997.The limit of detection and the limit of quantification were 0.75μg/kg and 2.0μg/kg,respectively.Recoveries of samples spiked at three levels were between 67.4%and 96.2%with relative standard deviations of 1.6%-8.6%.The method was suitable for the determination of lomefloxacin,pefloxacin,ofloxacin and norfloxacin in propolis.