对氨甲苯酸注射液中特定杂质4-甲酰基苯甲酸的研究  

Specific impurity 4-formylbenzoic acid in aminomethylbenzoic acid injection

作　　者：张耀文 于明 李沫 孙苓苓 ZHANG Yao-wen;YU Ming;LI Mo;SUN Ling-ling(Liaoning Inspection,Examination&Certification Centre,Shenyang 110036;Liaoning Institute for Drug Control,Shenyang 110036)

机构地区：[1]辽宁省检验检测认证中心,沈阳110036 [2]辽宁省药品检验检测院,沈阳110036

出　　处：《中南药学》2021年第4期705-709,共5页Central South Pharmacy

基　　金：国家药品监督管理局2020年国家药品抽验任务(编号:73)。

摘　　要：目的研究氨甲苯酸注射液中的特定杂质。方法对样品进行有关物质检查,利用半制备柱从样品中制备杂质,建立UHPLC-Q Exactive Focus MS法对样品中的杂质进行结构鉴定,并以氨甲苯酸为参照物,采用斜率法计算杂质的相对校正因子。结果确定了特定杂质为4-甲酰基苯甲酸,且其在1.244~62.20 ng·mL^(-1)与峰面积线性关系良好,Y=1687X-330.5(r=1.000),相对校正因子为2.88,检测限和定量限分别为0.27 ng·mL^(-1)和1.07 ng·mL^(-1),重复性RSD为0.44%,稳定性RSD为0.50%,加样回收率在97.85%~102.6%(RSD=1.4%)。结论本文利用半制备柱从样品中制备杂质,建立了UHPLC-Q Exactive Focus MS方法对杂质结构进行鉴定及定量分析,进一步完善质量标准。Objective To determine the specific impurity in aminomethylbenzoic acid injection.Methods The related substances were measured in samples,and the impurity was determined with semi-preparative columns.The UHPLC-Q Exactive Focus MS method was used to identify the structure of the impurity in the samples.The relative correction was obtained by HPLC with aminomethylbenzene as the internal standard.Results The specific impurity was 4-formyl benzoic acid.The linearity was good at 1.244~62.20 ng•mL^(-1),Y=1687X-330.5(r=1.000),and the relative correction factor was 2.88.The limit of detection and limit of quantification were 0.27 ng•mL^(-1)and 1.07 ng•mL^(-1),respectively.The repeatability RSD was 0.44%and the stability RSD was 0.50%.The sample recovery was at 97.85%~102.6%(RSD=1.4%).Conclusion A semipreparative column is used to prepare the impurity from the samples.The UHPLC-Q Exactive Focus MS method helps identify the structure of the impurity to further improve the quality standard.

关 键 词：氨甲苯酸注射液 UHPLC-Q Exactive Focus MS 4-甲酰基苯甲酸 校正因子 

分 类 号：R927[医药卫生—药学]