目的:建立手性固定相液相色谱串联质谱(LC-MS/MS)同时分离4个β受体阻滞剂的方法。方法:以Chiralcel OD-H(250 mm×4.6 mm,5μm)为手性柱,通过电喷雾离子化(ESI),采用多反应检测(MRM)方式进行正离子检测,普萘洛尔、美托洛尔、阿替洛尔、比索洛尔检测离子分别为m/z 260.2→116.0,m/z 268.4→116.0,m/z 267.2→145.0,m/z 326.2→116.0,在23 min内同时完成4个对映体的分离。结果:考察了流动相组成、柱温及流速对拆分的影响,并优化了实验条件,最终获得同时分离4个β受体阻滞剂的LC-MS/MS方法。针对药物的结构特点和固定相的种类,探讨了手性分离机理。结论:本方法很大程度上提高了分离效率,具有简便、高效及重复性好等特点,可用于该类药物的常规及生物样品分析。 Objective: To establish a method for the simultaneous separation of four β-blockers by liquid chromatography-tandem mass spectrometry (LC-MS / MS). METHODS: Chiralcel OD-H (250 mm × 4.6 mm, 5 μm) was used as a chiral column for positive ion detection by electrospray ionization (ESI) and multi-reaction detection (MRM) The measured ions of lol, atenolol and bisoprolol were m / z 260.2 → 116.0, m / z 268.4 → 116.0, m / z 267.2 → 145.0, m / z 326.2 → 116.0, respectively. Enantiomeric separation. Results: The effects of mobile phase composition, column temperature and flow rate on the resolution were investigated. The experimental conditions were optimized and the LC-MS / MS method for simultaneous separation of four β-blockers was also obtained. According to the structural characteristics of the drug and the type of stationary phase, the chiral separation mechanism was discussed. Conclusion: The method greatly improves the separation efficiency, with the characteristics of simple, efficient and reproducible, and can be used for routine and biological sample analysis of such drugs.