氯麻黄碱的检验研究

Determination of Chloroephedrine

目的研究氯麻黄碱的定性分析方法。方法通过使用红外光谱(IR)、气相色谱质谱联用仪(GC-MS)、超高效液相色谱-四级杆-飞行时间质谱仪(HPLC-QTOFMS)对氯麻黄碱进行检验研究。结果氯麻黄碱高温下转换为1,2-二甲基-3-苯基-氮丙啶,不适合用气相色谱质谱分析。HPLC-QTOFMS检验氯麻黄碱,可避免氯麻黄碱在检验中途因高温转化成1,2-二甲基-3-苯基-氮丙啶。结论本文建立的HPLC-QTOFMS分析方法可对氯麻黄碱定性分析。氯麻黄碱含量大于20%的氯麻黄碱和麻黄碱混合物中氯麻黄碱可用红外检测进行筛查。

Objective To establish methods for qualitative analysis of chloroephedrine. Methods Different methods were used to analyze chloroephedrine. Solid sample was dissolved with methanol and the solution was analyzed by Fourier transform infrared spectrometer （FTIR）, gas chromatography-mass spectrometer （GC-MS） and high performance liquid chromatography-quadrupole time-of-flight mass spectrometry （HPLC-QTOFMS）, respectively. Results 1,2-dimethyl-3- phenylaziridine, not chloroephedrine was detected with GC-MS. Transformation of chloroephedrine to 1, 2-dimethyl-3- phenylaziridine was observed during GC-MS analysis due to the high temperature of inlet. However, such interference was prevented while using LC-MS or FTIR. Chloroephedrine and 1, 2-dimethyl-3-phenylaziridine could be separated and determined by LC-MS. Exact ion m/z of chloroephedrine was 184.0888, and 148.1121 for that of 1, 2-dimethyl-3- phenylaziridine. In addition, retention time of chloroephedrine and 1, 2-dimethyl-3-phenylaziridine were different in LC-MS. Conclusions GC-MS is not fit for the determination of chloroephedrine, because chloroephedrine is unstable and transformed to l, 2-dimethyl-3-phenylaziridine by high temperature of inlet. HPLC-QTOFMS is competent for qualitative determination of chloroephedrine and the transformation could be avoidable. FTIR is capable of qualitative determination of highly pure chloroephedrine.