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盐酸吡格列酮有关物质的色谱-质谱结构鉴定
投稿时间:2017-04-01  修订日期:2017-05-04  点此下载全文
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作者单位E-mail
殷潇雅 中国药科大学 1032546095@qq.com 
汪澄 中国药科大学  
杭太俊 中国药科大学 hangtj@cpu.edu.cn 
明国军 江苏九阳生物制药有限公司  
中文摘要:采用色谱-质谱联用技术鉴定盐酸吡格列酮的有关物质。使用Ultimate XB-C18(250 mm × 4.6 mm, 5 μm) 色谱柱,以甲醇-0.1%乙酸铵缓冲液为流动相,梯度洗脱,对盐酸吡格列酮有关物质进行分离;以电喷雾正离子化-飞行时间质谱法测定各有关物质[M+H]+母离子的准确质量和元素组成,三重四极质谱测定特征碎片离子,对有关物质进行分析鉴定。根据质谱分析结果,结合合成工艺与强制降解机制分析,检测并鉴定出11个主要有关物质(1个合成中间体、6个合成副产物、4个降解产物),可为其生产工艺优化和质量控制提供参考。
中文关键词:盐酸吡格列酮  有关物质  结构鉴定  色谱-质谱联用
 
Identification of the related substances in pioglitazone hydrochloride by hyphenated LC-MS techniques
Abstract:To identify the related substances in pioglitazone hydrochloride by hyphenated LC-MS techniques,an Ultimate XB-C18 (250 mm×4.6 mm, 5 μm) column was used for separation of the related substances with methanol and 0.1% ammonium acetate buffer as the mobile phases in gradient elution. Electrospray positive ionization high resolution TOF/MS was used for the determination of the accurate mass and elemental composition of parent [M+H]+ ions of the related substances, and triple quadrupole tandem mass spectrometry was employed for the product mass spectra determination. Eleven major related substances were detected and identified to be one synthesis intermediate, six by-products and four degradation products, by using LC-MS determination, spectra elucidation, and further synthetic process and stress degradation mechanisms analysis. The results are useful for pioglitazone hydrochloride manufacturing processes optimization and quality control.
keywords:pioglitazone hydrochloride  related substances  structure identification  LC-MS
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