环丙基乙炔的含量测定方法及主要杂质鉴定

Method of quantitative measurement for cyclopropyl-acetylene and identification of its main trace impurity

目的：分离并分析环丙基乙炔（CPA）生产过程中产生的主要杂质，鉴定其结构，并建立纯度测定方法。方法：采用气相色谱一质谱联用法对环丙基乙炔产品进行了分析，通过对质谱和核磁共振数据进行结构鉴定，采用气相色谱法对环丙基乙炔产品建立了纯度测定方法。结果：气相色谱CPA的最低检测限为1．74mg，CPA在2．88～14．1mg·ml-1范围内线性关系良好，RSD为1．89％。气相色谱质谱推测该杂质为异丙烯基乙炔，核磁共振确认杂质结构为异丙烯基乙炔结构。结论：异丙烯基乙炔为环丙基乙炔生产过程中生成的副产物，对成药品质影响较大。

Objective To separate and analye the main impurity of by-product in cyclopropyl-acetylene,and identi- fy the structure of main trace impurity, thus to establish an analyzing method. Method The main trace impurity was an- alyzed by the gas chromatography-mass spectrometry method and compared to standard mass spectrometry and employed NMR spectrometry. The gas chromatography method was developed by area normalization method. Result The trace im- purity was identified to be isopropenyl-ancetylene, the analyzing method was proven to be accurate and feasible. Conclu- sion The main trace impurity, a by-product in cyclopropyl-acetylene, is highly affedting the quality of cyclopropyl-a- cetylene product.