应用高效液相色谱-飞行时间质谱及离子阱质谱分析磷酸苯丙哌林中的杂质  

Analysis of Impurity in Benproperine Phosphate Bulk Drug by High Performance Liquid Chromatography-Time of Flight Mass Spectrometry and Ion Trap Mass Spectrometry

作　　者：董宇[1] 王晓黎[1] 曲建国[1] 

机构地区：[1]辽宁省食品药品检验所,沈阳110023

出　　处：《中国药学杂志》2012年第19期1585-1587,共3页Chinese Pharmaceutical Journal

摘　　要：目的应用高效液相色谱-飞行时间质谱及高效液相色谱-离子阱质谱分析磷酸苯丙哌林原料药中的杂质。方法采用Waters C18柱,以乙腈-0.01 mol.L-1醋酸铵溶液(冰醋酸调节pH值至3.3)(60∶40)为流动相,分离杂质与磷酸苯丙哌林,采用飞行时间质谱测定杂质精确相对分子质量,采用离子阱质谱获得其质谱碎片。结果通过精确相对分子质量确定杂质的分子组成为C21H25NO2,为苯丙哌林氧化产物,通过分析质谱碎片和生产工艺,推测了杂质的结构。结论飞行时间质谱和离子阱质谱相结合,可以在化合物结构确认方面发挥重要作用。OBJECTIVE To analyze the impurity in benproperine phosphate bulk drug by high performance liquid chromatogra- phy-time of flight mass spectrometry （TOF-MS） and ion trap mass spectrometry （IT-MS）. METHODS The impurity and benprop- erine phosphate were separated on a Waters C18 column with a mobile phase of aeetonitrile-0.01 mol . L-1 ammonium acetate solution （adjusted to pH 3.3 with glacial acetic acid） （60： 40）. The exact molecular weight of the impurity was obtained by TOF-MS and the fragments were obtained by IT-MS. RESULTS The molecular formula of the impurity was identified as C21 H25 NO2 which was the oxide of benproperine phosphate. The structure was analyzed by fragments and the process of preparation of benproperine phosphate. CONCLUSION TOF-MS and IT-MS are powerful tools for the identification of compounds.

关 键 词：高效液相色谱法 飞行时间质谱 离子阱质谱 磷酸苯丙哌林 杂质 

分 类 号：R917[医药卫生—药物分析学]