Levothyroxine sodium revisited: A wholistic structural elucidation approach of new impurities via HPLC-HRMS/MS, on-line H/D exchange, NMR spectroscopy and chemical synthesis

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• 作者：M. Ruggenthaler^a ; ^b ; J. Grass^a ; W. Schuh^a ; C.G Huber^b ; R.J. Reischl^b ; ^{roland.reischl@sbg.ac.at}
• 关键词：Levothyroxine ; Thyroid hormone ; Pharmaceutical impurities ; On-line H/D Exchange ; HDX ; LC-MS
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2017
• 出版时间：20 February 2017
• 年：2017
• 卷：135
• 期：Complete
• 页码：140-152
• 全文大小：1518 K
• 卷排序：135

文摘

A multitude of levothyroxine sodium impurities new to literature are characterized via HPLC-HRMS/MS and On-line H/D exchange. 5 major LT4 impurities are identified via synthesis or isolation of the reference substance and characterization with 1D and 2D-NMR. CID fragmentation mechanisms of identified levothyroxine sodium impurities are discussed. New subclasses of levothyroxine sodium impurities are introduced originating from the alternative synthetic route of this API.