柱前手性衍生化-正相高效液相色谱法拆分甲基麻黄碱对映异构体

Enantiospecific analysis of methylephedrine by normal-phase HPLC with precolumn derivatization

目的 建立一种用柱前手性衍生化 正相高效液相色谱法分析甲基麻黄碱对映异构体的方法。方法 以 (- ) 氯甲酸薄荷醇酯作为手性衍生化试剂 ,(- ) 甲基麻黄碱与 (+) 甲基麻黄碱衍生化后生成一对非对映异构体。选用LichrosorbSi 6 0柱 ,以正己烷 异丙醇 三乙胺 (体积比为 94∶6∶0 .0 2 )为流动相 ,在 2 2 0nm下检测。结果 非对映异构体色谱峰的保留时间分别为 3.6min和 4 .3min。经电喷雾离子阱多级质谱分析验证了衍生物结构。结论 本方法操作简单、重现性好 。

OBJECTIVE: To develop a high-performance liquid chromatographic method for the determination d (-)-and (+)-enantiomers of methylephedrine. METHODS: The derivatization with (-)-menthyl chloroformate was followed by normal-phase chromatography with a mobile phase of n-hexane / 2-propanol / triethylamine (94:6:0.02) at a flow rate of 1.3 mL &middot min-1 and the detection wavelength was set at 220 nm. RESULTS: The electrospray ionization-quadrupole ion trap mass spectrometer was applied to verify the structure of derivatives of methylephedrine. The retention times for the (-)- and (+)-methylephedrine diastereomeric derivatives were 3.6 min and 4.3 min respectivdy. CONCLUSION: The presented study provided a simple and reproducible method for the enantiomeric quality control of (-)-methylephedrine.