Isolation and structural elucidation of two impurities from a diacerein bulk drug

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• 作者：Chaudhari Ashok ; Maikap Golak ; Deo Adwait ; Vivek Krishna ; Agrawal Himani ; Peshawe Umesh ; Gaw ; e Amol ; Sompalli Srinivas ; Mane Sharad ; Jadhav Deepali ; Chaudhari Atul
• 关键词：Diacerein ; LC– ; MS ; Preparative chromatography ; Isolation ; NOESY
• 刊名：Journal of Pharmaceutical and Biomedical Analysis
• 出版年：2009
• 出版时间：20 February 2009
• 年：2009
• 卷：49
• 期：2
• 页码：525-528
• 全文大小：303 K

文摘

Two impurities were found in the crude sample of diacerein. The level of these impurities 1.14 % and 1.24 % were detected by isocratic reverse-phase high performance liquid chromatography (HPLC). The molecular weights of the impurities were determined by liquid chromatography–mass spectroscopy (LC–MS) analysis. These impurities were isolated from crude sample of diacerein by reverse-phase preparative liquid chromatography. These impurities were characterized as 5-acetoxy-4-hydroxy-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid (Impurity-1) and 4-acetoxy-5-hydroxy-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid (Impurity-2) respectively. Structural elucidation of both the impurities were carried out by ¹H NMR, ¹³C NMR, DEPT, 1D NOESY, MS and IR spectroscopy.