中国药典2015年版中诺氟沙星胶囊有关物质测定方法的改进研究

Improvement of the Determination Method of Related Substances of Norfloxacin Capsules in Chinese Pharmacopoeia(2015 Edition)

关键词:  中国药典2015年版  诺氟沙星胶囊  有关物质  质量可控性

Key words:  ChP2015  norfloxacin capsules  related substances  quality controllability

摘要:

目的 考察中国药典2015年版中诺氟沙星胶囊有关物质测定方法的质量可控性，并对现行方法进行改进。方法 分别采用中国药典2015年版和EP9.3版的方法对浙江省各地区抽样的57批诺氟沙星胶囊的有关物质进行检查，对结果进行比较研究；并对中国药典2015年版方法的合理性进行探讨。结果 57批抽样样品按EP9.3版有关物质测定方法检查，结果有5批样品检出杂质E超出限度（0.15%），1批杂质K为限度边缘（0.15%），而根据中国药典2015年版方法检查结果，57批样品全部合格。现行的中国药典2015年版诺氟沙星胶囊有关物质测定方法专属性不强，杂质E被包含在主峰之中难于检出；现行标准有关物质测定方法中不同品牌的C₁₈色谱柱以及流动相条件对测定结果影响较大，选择Waters Sunfire C₁₈色谱柱，调整流动相的比例和梯度条件可以使杂质E与诺氟沙星主峰很好地分离，样品的测定结果也与EP9.3方法的测定结果一致，能达到控制杂质E、杂质K以及其他杂质的目的。结论 目前浙江省市场上的诺氟沙星胶囊中杂质E有超标的情况，但根据中国药典2015年版的现行有关物质测定方法难以检出，难以有效控制药品的质量，需修订提高。

Abstract:

OBJECTIVE To study quality controllability of determination method of related substances of norfloxacin capsules in Chinese Pharmacopoeia(2015 Edition)(ChP2015) and to improve the current method. METHODS The related substances of 57 batches of norfloxacin capsules samples from all regions of Zhejiang province were determined according to ChP2015 method and EP9.3 method, and the results were compared. The rationality of the ChP2015 method was discussed. RESULTS The tested results of 57 batches of samples according to EP9.3 method showed that the contents of impurity E of 5 batches of samples exceeded the limit(0.15%), and the impurity K of 1 batch of sample was on the edge of the limit(0.15%). While the results of 57 batches of samples all met the requirements according to ChP2015 method. The method of related substances of Norfloxacin capsules in ChP2015 was not specific, and the impurity E included in the main peak was difficult to detect. The determination results were affected by the columns of different brand and the mobile phase conditions in ChP2015 method of related substances. Using Waters Sunfire C₁₈ column and adjusting the proportion and gradient condition of the mobile phase could make the impurity E well separated from the main peak of norfloxacin, the determination results of samples were in accordance with EP9.3 method, and it could control the impurity E, K and other impurities. CONCLUSION The contents of impurity E of norfloxacin capsules exceed the standard on the current market of Zhejiang province, and it can not be detected according to ChP2015 method. The determination method of related substances of norfloxacin capsules in ChP2015 can not control the quality of the drug effectively and need to be revised and improved.