目的：分析和鉴定注射用头孢哌酮钠他唑巴坦钠中的未知降解杂质。方法采用液相色谱-质谱（ LC-MS／MS）法，采用强制降解的破坏条件，制备杂质含量较高的受试样品；以0.1%的甲酸水溶液为流动相A，乙腈为流动相 B，采 C18色谱柱进行梯度洗脱；以电喷雾串联质谱电离源正离子模式进行质谱数据采集，对热降解破坏样品进行LC-MS／MS测定。结果获得注射用头孢哌酮钠他唑巴坦钠的液相色谱图，以及与液相色谱图对应的一级、二级质谱图，对谱图进行分析归纳，推测注射用头孢哌酮钠他唑巴坦钠中2个未知杂质为头孢哌酮杂质 A进一步水解的产物，并推导了降解途径。结论本方法灵敏、可靠、快速，对头孢哌酮钠及其制剂的生产、质量监控具有指导意义。%ABSTRACT:OBJECTIVE To establish a HPLC/MS/MS method for the analysis and identification of unknown impurities in cefoperazone sodium and tazobactam sodium for injection.METHODS LC-MS/MS was performed on C18 column with mobile phase was 0.1%formic acid solution and acetonitrile.After stress degradation on high tem-perature,the sample was tested and data was collected in positive ion modes with ESI as ion resource.RESULTS The first and second mass spectrum of cefoperazone and its unknown impurities were determined,it was concluded that the impurities were hydrolyzates of cefoperazone impurity A according the degradation pathway.CONCLUSION The method is sensitive, rapid and credible technique in production and quality control of cefoperazone and its preparations.
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