依帕列净中新型工艺相关杂质的分离与结构鉴定。
Isolation and characterization of novel process-related impurities in empagliflozin.
机构信息
Key Laboratory of Chemical Biology and Traditional Chinese Medicine (Ministry of Educational of China), Key Laboratory of Phytochemistry R&D of Hunan Province, and Key Laboratory of the Assembly and Application of Organic Functional Molecules of Hunan Province, College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha, Hunan, 410081, China.
Key Laboratory of Theoretical Organic Chemistry and Functional Molecules, Ministry of Education, School of Chemistry and Chemical Engineering, Hunan University of Science and Technology, Xiangtan, Hunan, 411201, China.
出版信息
J Pharm Biomed Anal. 2021 May 10;198:114001. doi: 10.1016/j.jpba.2021.114001. Epub 2021 Mar 6.
Empagliflozin is an effective sodium glucose cotransporter-2 (SGLT2) inhibitor to improve glycemic control in adults with type 2 diabetes. During the manufacture of empagliflozin, three unknown impurities were discovered in pilot batches ranging from 0.05 % to 0.15 % by LC analysis. These unknown impurities were isolated from the crystallization mother liquor by column chromatography and semi-preparative LC, and their structures were elucidated by comprehensive analysis of HRMS, 1D-NMR (H, C) and 2D-NMR (H-H COSY, HSQC, HMBC) spectroscopy data. The plausible mechanistic pathways to the formation of these three impurities were also discussed.
恩格列净是一种有效的钠-葡萄糖协同转运蛋白 2（SGLT2）抑制剂，可改善 2 型糖尿病成人的血糖控制。在恩格列净的生产过程中，通过 LC 分析发现中试批次中有 0.05%至 0.15%的三种未知杂质。这些未知杂质通过柱层析和半制备 LC 从结晶母液中分离出来，并通过高分辨质谱、一维 NMR（H、C）和二维 NMR（H-H COSY、HSQC、HMBC）光谱数据的综合分析来阐明其结构。还讨论了形成这三种杂质的可能的机理途径。
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