国产头孢匹胺注射剂的质量分析

摘要

目的 评价国内不同厂家生产的头孢匹胺注射剂的质量现状及存在问题.方法 依据现行法定标准进行样品检验,统计分析检验结果,分析国产头孢匹胺注射剂的总体质量水平,比较不同生产企业产品质量.结果 本次抽验涉及12家生产企业的112批次样品(注射用头孢匹胺24批次,注射用头孢匹胺钠88批次),按法定标准检验结果均符合规定,合格率100％.标准检验发现13个现行标准均为局颁注册标准,存在限度不统一、安全性项目(如苯甲酸钠量、碳酸钠量、聚合物量)缺失问题.探索性研究对工艺合理性进行了评价,提示溶媒结晶工艺得到的头孢匹胺钠盐注射剂相对更安全,质量更可控.采用LC/MS等方法首次建立了该品种杂质谱,并对杂质来源进行了归属及结构确认.新建碳酸钠和苯甲酸钠含量测定方法;建立有关物质Ⅱ检查方法.结论 目前国内头孢匹胺注射剂整体质量较好,但存在边缘产品,尤其是存在多种工艺,质量标准有待统一提高,并增加碳酸钠含量、苯甲酸钠含量和有关物质Ⅱ等安全性项目.%Objective To evaluate the suitability of the statutory standard and the quality status of the cefpiramide for injection of different domestic manufacturers.Methods According to the current statutory standards for sample inspections,the statistical analysis,and test results,analyze the overall quality of domestic cefpiramide for injection,and compare the quality of different production enterprises.Results This testing involved 112 batches of samples (24 batches of cefpiramide for inection and 88 batches of cefpiramide sodium for injection) from twelve production enterprises.According to the legal standard,the inspection results were in conformity with the provisions and the qualified rate was 100％.The standard test found that the 13 current standards were all registered standards.However,the limits were not uniform,and safety items (such as sodium benzoate,sodium carbonate,polymer content) were missing.Exploratory studies were conducted to evaluate the rationality of the process.It was suggested that the injection of cefpiramide sodium salt obtained by the solvent crystallization process was relatively safer and more controllable in quality.The impurity spectrum of this variety was established for the first time by LC/MS.The source and the structure of the impurity were identified.New methods for the determination of sodium carbonate and sodium benzoate and the related substances Ⅱ examination method were established.Conclusions At present,the quality of domestic cephalosporin injection is good,but there were edge products.Especially there were a variety of processes.The quality standards need to be improved,and the safety items such as the sodium carbonate content,the sodium benzoate content,and related substances Ⅱ should be included.