Physicochemical characterization of ezetimibe and its impurities

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• 作者：Katarzyna Filip^a ; ^{k.filip@ifarm.eu} ; Krzysztof Ba&#x144 ; kowski^a ; ^{k.bankowski@ifarm.eu} ; Katarzyna Sidoryk^a ; ^{k.sidoryk@ifarm.eu} ; Joanna Zagrodzka^a ; ^{j.zagrodzka@ifarm.eu} ; Marta &#x141 ; aszcz^a ; ^{m.laszcz@ifarm.eu} ; Kinga Trzci&#x144 ; ska^a ; ^{k.trzcinska@ifarm.eu} ; Anna Szyprowska^a ; ^{a.szyprowska@ifarm.eu} ; Piotr Cmoch^a ; ^b ; ^{p.cmoch@ifarm.eu} ; Wioleta Maruszak^a ; ^{w.maruszak@ifarm.eu}
• 关键词：Ezetimibe ; Stereoisomer ; Impurity ; Physicochemical characterization ; NMR
• 刊名：Journal of Molecular Structure
• 出版年：2011
• 出版时间：5 April 2011
• 年：2011
• 卷：991
• 期：1-3
• 页码：162-170
• 全文大小：1463 K

文摘

The physicochemical characterization of major degradation and process-related impurities associated with the synthesis of ezetimibe was performed. The possibility of forming the undesirable (R,R,S) stereoisomer of ezetimibe has been mentioned in literature (Vinod KK, Suhail A, Bhupendra T, Nitin G US 2010/0010212 A1, Ind-Swift Laboratories Limited WO 2008/096372), but no study of its structure determination has been published yet. This paper discusses the structure elucidation of the (R,R,S) stereoisomer as well as ezetimibe degradation product on the bases of NMR, IR and MS data. Other potential impurities of ezetimibe are also described. A selective and stability-indicating high-performance liquid chromatography method with dual UV detection was developed for the determination of chemical and stereochemical purity of ezetimibe. The characterization of particle size and shape for ezetimibe and its stereoisomer is also described.