高效液相色谱-串联质谱检测苹果醋中非法添加物西布曲明及其去甲基衍生物

摘要

To develop a detection method for sibutramine,N-desmethyl sibutramine and N,N-di-desmethyl sibutramine in apple vinegar using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).The chromatography is performed using an ACQUITY UPLC(R)BEH C18 (1.7 μm,2.1 mm×100 mm) column with a mobile phase consisting of acetonitrile and 0.1％ acetic acid-10 mmol/L ammonium acetate.Qualitative analysis of sibutramine,N-desmethyl sibutramine and N,N-di-desmethyl sibutramine is conducted under full-scan model,and quantitative analysis in the multiple reaction monitoring (MRM) model.The results show that the calibration curve for the analyte shows good linearity in the range of 2～ 24 ng/mL.The limit of detection is sibutramine of 15.8 μg/kg,N-desmethyl sibutramine of 18.0μg/kg,N,N-di-desmethyl sibutramine of 58.6 μg/kg,and the recoveries obtained by standard addition method are 86％ ～99.6％.Conclution:This method is simple,specific and accurate with a high sensitivity.It can be used for the illegal addition of sibutramine,N-desmethyl sibutramine and N,N-di-desmethyl sibutramine added in apple vinegar.%采用高效液相色谱-串联质谱法对苹果醋中非法添加化学成分西布曲明、N-单去甲基西布曲明和N,N-双去甲基西布曲明进行检测.建立了以ACQUITY UPLC(R)BEH C18柱(1.7 μm,2.1mm×100 mm)为色谱柱,以乙腈、含0.1％乙酸的10 mmol/L乙酸铵为流动相.通过HPLC-MS/MS系统中全扫描模式对西布曲明及其去甲基衍生物进行定性分析,多反应监测模式对其进行定量分析.结果表明:西布曲明、N-单去甲基西布曲明和N,N-双去甲基西布曲明在2～24 ng/mL内具有良好线性,检出限分别为15.8,18.0,58.6 μg/kg,加标回收率均在86％～99.6％.结论:该方法操作方便、专属性强、灵敏度高、准确度高,可用于苹果醋中西布曲明及其去甲基衍生物的检测.