应用液相色谱-串联质谱联用技术分析厄贝沙坦及其制剂的杂质谱

Analysis of Impurity Profile of Irbesartan and Its Preparations by LC-MS/MS

张文慧 ¹程冬 ²陆益红 ²赵述强 ²裘旭华²

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作者信息

1. 江苏省食品药品监督检验研究院,国家药品监督管理局化学药品杂质谱研究重点实验室,南京 210019;中国药科大学,南京 210009
2. 江苏省食品药品监督检验研究院,国家药品监督管理局化学药品杂质谱研究重点实验室,南京 210019
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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,3.5 μm),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.

Abstract

OBJECTIVE To analyze the impurity profile of irbesartan and its preparations by LC-MS/MS.METHODS ZORB-AX SB-C18 column(4.6 mm × 150 mm,3.5 μm)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 detec-ted.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.

关键词

厄贝沙坦/厄贝沙坦制剂/有关物质/杂质谱/液相色谱-串联质谱联用

Key words

irbesartan/irbesartan preparation/related substance/impurity profile/LC-MS/MS

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基金项目

国家药品抽检计划厄贝沙坦项目(2022)(第60号)

出版年

2024

中国药学杂志

中国药学会

中国药学杂志

CSTPCD北大核心

影响因子：0.957

ISSN：1001-2494

参考文献量3

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