摘要
目的采用液相色谱-串联质谱联用技术(LC-MS/MS)分析厄贝沙坦及其制剂的杂质谱。方法采用色谱柱ZORBAX SB-C18(4.6 mm×150 mm,3.5μm),以体积分数0.1%甲酸溶液(用氨水调节pH值至3.5)-乙腈(体积比62∶38)为流动相,等度洗脱,对厄贝沙坦及其制剂中有关物质进行分离,采用电喷雾-飞行时间质谱法(ESI-TOF-MS/MS)测定各有关物质分子结构信息,并结合对照品质谱结构信息确证有关物质结构。结果厄贝沙坦与其有关物质在该色谱条件下分离良好,共检出16个有关物质,通过对照品确证其中10个有关物质的结构。结论本实验建立的LC-MS/MS方法能够有效分离鉴定厄贝沙坦及其制剂中有关物质,为其质量控制和工艺优化提供参考依据。
OBJECTIVE To analyze the impurity profile of irbesartan and its preparations by LC-MS/MS.METHODS ZORBAX SB-C18 column(4.6 mm×150 mm,3.5μm)was used for the separation of the related substances with a mixture of 0.1%formic acid solution(adjusted to pH 3.5 with ammonia)and acetonitrile(62∶38)as the mobile phase by isocratic elution.The structures of the related substances were speculated by ESI-TOF-MS/MS and verified further by reference substances.RESULTS Irbesartan and its related substances were separated under the established chromatographic condition,and a total of 16 related substances were detected.The structures of 10 related substances were verified by reference substances.CONCLUSION The established LC-MS/MS method is effective for separation and identification of the related substances of irbesartan and its preparations,and the results obtained are valuable for its quality control and manufacturing process.
作者
张文慧
程冬
陆益红
赵述强
裘旭华
ZHANG Wenhui;CHENG Dong;LU Yihong;ZHAO Shuqiang;QIU Xuhua(NMPA Key Laboratory for Impurity Profile of Chemical Drugs,Jiangsu Institute for Food and Drug Control,Nanjing 210019,China;China Pharmaceutical University,Nanjing 210019,China)
出处
《中国药学杂志》
CAS
CSCD
北大核心
2024年第7期612-626,共15页
Chinese Pharmaceutical Journal
基金
2022年国家药品抽检计划第60号厄贝沙坦项目资助。
