药用辅料苯甲酸苄酯有关物质HPLC检测方法的建立  

Investigation on the HPLC method of benzyl benzoate related substances in pharmaceutical excipients

作　　者：杜凯 朱晓月 王琳 张喆 胡琴 DU Kai;ZHU Xiaoyue;WANG Lin;ZHANG Zhe;HU Qin(Beijing Institute for Drug Control and Research,Key Laboratory of Genetics Research and Evaluation of the State Administration of Drugs,Beijing Key Laboratory of Traditional Chinese Medicine Component Analysis and Biological Evaluation,Beijing 102206,China)

机构地区：[1]北京市药品检验研究院,国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京102206

出　　处：《中国药品标准》2024年第3期299-302,共4页Drug Standards of China

基　　金：国家药典委员会药品标准提高课题(2018Y061)。

摘　　要：目的:建立苯甲酸苄酯有关物质的高效液相色谱方法,对该辅料质量标准提出修订建议。方法:用苯基硅烷键和硅胶为填充剂,以甲醇-1%-醋酸(60∶40)为流动相,检测波长为254 nm,流速1.0 mL·min^(-1),进样量20μL。结果:根据破坏试验结果,并兼顾分离度要求,确定了苯甲酸苄酯有关物质的色谱条件,并进行了方法学验证。有关物质中杂质苯甲酸和苯甲醛的检测限分别为0.2μg·mL^(-1)和0.01μg·mL^(-1),苯甲酸和苯甲醛的校正因子分别为1.0和0.1。按新建方法对4家企业6批次苯甲酸苄酯样品进行有关物质检查,均检出苯甲醛杂质,杂质含量在0.02%~0.1%。杂质总量在0.02%~0.9%。结论:新建立的方法可增订入苯甲酸苄酯的质量标准中,并根据给药途径的不同,制定不同的杂质限度,以便更好的控制药品质量。Objective:To establish an HPLC method for benzyl benzoate related substances and propose revision suggestions for the quality standard of this excipient.Methods:Phenylsilane bond and silica gel were used as fillers,and methanol-1%acetic acid(60∶40)was used as the mobile phase at the flow rate of 1.0 mL·min^(-1).The detection wavelength was 254 nm and the injection amount was 20μL.Results:Based on the results of the destruction test and taking into account the separation requirements,the chromatographic conditions for benzyl benzoate related substances were confirmed and methodological validation was conducted.The detection limits for benzoic acid and benzaldehyde in related substances were 0.2μg·mL^(-1)and 0.01μg·mL^(-1).The correction factors for benzoic acid and benzaldehyde were 1.0 and 0.1,respectively.According to the newly established method,six batches of benzyl benzoate samples from four enterprises were inspected for related substances,and benzaldehyde was detected with content from 0.02%to 0.1%.The total amount of impurities was from 0.02%to 0.9%.Conclusion:The newly established method can be added to the quality standards of benzyl benzoate,and different impurity limits can be formulated according to the different administration routes in order to better control drug quality.

关 键 词：苯甲酸苄酯 质量标准 有关物质 高相液相色谱法 修订建议 

分 类 号：R921.2[医药卫生—药学]