液相色谱-质谱联用技术测定头孢他啶中未知杂质的结构

Analyzing the structure of an unknown impurity in ceftazidime by liquid chromatogram-mass spectrometry

目的应用液相色谱-电喷雾离子化质谱法分析头孢他啶原料药中的杂质,并初步确定了一未知杂质的结构。方法采用C18色谱柱;以乙腈-乙酸铵水溶液(15∶85)为流动相;检测波长255nm;以电喷雾电离源正离子模式进行质谱数据采集。结果获得头孢他啶和未知杂质的液相色谱图以及液相色谱峰对应的一级质谱图,对谱图进行分析归纳,推测头孢他啶样品中未知杂质的结构为头孢他啶结构中羧酸的甲酯化产物。结论本方法灵敏、可靠、快速,对头孢他啶的生产、质量监控具有指导意义。

OBJECTIVE To analysis an unknown impurity in ceftazidime with liquid chromatogram and electrospray ionization mass spectrometry, and the structure of one impurity was initially confirmed. METHODS Hypersil-column of Cl8 with mobile phases of CH3CN-ammonium acetate solution （15：85） was used：The detection wavelength was set at 255 nm;Electrospray ionization source was applied and the mass data about MS ＋ was collected. RESULTS The first order mass spectrum of ceftazidime and its unknown impurity were determined, it was induced that the impurity was the methylester of ceftazidime.CONCLUSION The method is sensitive, rapid and credible technique in production and quality control of ceftazidime.