不同厂家生产的头孢哌酮钠舒巴坦钠注射用粉针剂通用性近红外定量模型的建立

不同厂家生产的头孢哌酮钠舒巴坦钠注射用粉针剂通用性近红外定量模型的建立

逄焕欢, 冯艳春, 张学博, 胡昌勤^*

1.中国药品生物制品检定所, 北京 100050;
2.吉林省药品检验所, 吉林长春 130062

收稿日期:2007-08-15 修回日期:2008-01-10 出版日期:2008-03-15 发布日期:2008-03-15
通讯作者: 胡昌勤*

Construction of universal quantitative models for the determination of cefoperazone sodium/sulbactam sodium for injection from different manufacturers using near-infrared reflectance spectroscopy

Huan-Huan Pang, Yan-Chun Feng, Xue-Bo Zhang, Chang-Qin Hu^*

1. National Institute for the Control of Pharmaceutical and Biological Products, Beijing 100050, China;
2. Jilin Institute of Drug Control, Changchun 130062, China

Received:2007-08-15 Revised:2008-01-10 Online:2008-03-15 Published:2008-03-15
Contact: Chang-Qin Hu*

摘要/Abstract

摘要：

用光纤和积分球测量的近红外漫反射光谱分别建立可以测定不同厂家生产的头孢哌酮钠舒巴坦钠注射用粉针剂的定量分析模型。建立这两个模型共使用了6批市场销售的样品和42批实验室自制样品,头孢哌酮钠的浓度范围是30%~70%, 舒巴坦钠的浓度范围是60%~20%。型号为EQUINOX55型近红外光谱仪用于模型的建立。对于头孢哌酮钠, 积分球模型的交叉验证均方根误差(RMSECV)和预测均方根误差(RMSEP)分别为1.79%和2.85%; 光纤模型的结果是2.93%和2.92%。对于舒巴坦钠, 积分球模型的RMSECV和RMSEP分别为1.86%和3.08%; 光纤模型的结果是2.23%和3.01%。根据ICH的指导原则和参考文献12, 从专属性、线性、准确度、精密度和粗放性以及模型传递等几个方面对模型进行了评价。我们的研究表明, 建立非破坏性的通用性快速定量分析模型用以分析不同厂家生产的粉针剂样品是可行的。所以, 近红外方法能被作为一种有效的方法快速、非破坏性的监督检查市场上流通的产品。

关键词: 近红外漫反射光谱, 近红外漫反射光谱, 近红外漫反射光谱, 非破坏性定量, 非破坏性定量, 非破坏性定量, 定量模型, 定量模型, 定量模型, 通用性模型, 通用性模型, 通用性模型, 头孢哌酮钠舒巴坦钠, 头孢哌酮钠舒巴坦钠, 头孢哌酮钠舒巴坦钠, 假药, 假药, 假药

Abstract:

To develop near-infrared (NIR) reflectance spectroscopic methods for the quantitative analysis of cefoperazone sodium/sulbactam sodium from different manufacturers for injection powder medicaments. Various powders of cefoperazone sodium/sulbactam sodium were directly analyzed by non-destructive NIR reflectance spectroscopy using the spectrometer EQUINOX55. Two quantitative methods via integrating sphere (IS) and fiberoptic probe (FOP) models were explored from 6 batches of commercial samples and 42 batches of laboratory samples at a content ranging from 30% to 70% for cefoperazone and 60% to 20% for sulbactam. The root mean square errors of cross validation (RMSECV) and the root mean square errors of prediction (RMSEP) of IS were 1.79% and 2.85%, respectively, for cefoperazone sodium, and were 1.86% and 3.08%, respectively, for sulbactam sodium; and those of FOP were 2.93% and 2.92%, respectively, for cefoperazone sodium, and were 2.23% and 3.01%, respectively, for sulbactam sodium. Based on the ICH guidelines and Ref. 12, the quantitative models were then evaluated in terms of specificity, linearity, accuracy, precision, robustness and model transferability. The non-destructive quantitative NIR methods used in this study are applicable for rapid analysis of injectable powdered drugs from different manufacturers.

Key words: NIR diffuse reflectance spectroscopy, NIR diffuse reflectance spectroscopy, Non-destructive determination, Non-destructive determination, Cefoperazone sodium/sulbactam sodium, Cefoperazone sodium/sulbactam sodium, Injection powder medicament, Injection powder medicament, Validation, Validation, Counterfeit medicine, Counterfeit medicine

中图分类号:

R917.4

Supporting: Foundation item: National Key Technologies R&D Program Foundation of China (Grant No. 2006BAK04A11).
^*Corresponding author. Tel.: 86-10-67095308; fax: 86-10-65115148

逄焕欢, 冯艳春, 张学博, 胡昌勤^*

. 不同厂家生产的头孢哌酮钠舒巴坦钠注射用粉针剂通用性近红外定量模型的建立[J]. .

Huan-Huan Pang, Yan-Chun Feng, Xue-Bo Zhang, Chang-Qin Hu^*. Construction of universal quantitative models for the determination of cefoperazone sodium/sulbactam sodium for injection from different manufacturers using near-infrared reflectance spectroscopy[J]. .