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

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)...

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Bibliographic Details
Published in:Journal of pharmaceutical and biomedical analysis 2009-02, Vol.49 (2), p.525-528
Main Authors: Ashok, Chaudhari, Golak, Maikap, Adwait, Deo, Krishna, Vivek, Himani, Agrawal, Umesh, Peshawe, Amol, Gawande, Srinivas, Sompalli, Sharad, Mane, Deepali, Jadhav, Atul, Chaudhari
Format: Article
Language:English
Subjects:
Analysis
Analytical, structural and metabolic biochemistry
Anthraquinones - chemistry
Anti-Inflammatory Agents - chemistry
Biological and medical sciences
Chromatography, High Pressure Liquid - methods
Diacerein
Drug Contamination
Fundamental and applied biological sciences. Psychology
General pharmacology
Isolation
LC–MS
Mass Spectrometry - methods
Medical sciences
Molecular Structure
Molecular Weight
NOESY
Nuclear Magnetic Resonance, Biomolecular - methods
Pharmacology. Drug treatments
Preparative chromatography
Spectrometry, Mass, Electrospray Ionization - methods
Spectrophotometry, Infrared - methods
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Summary: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.
ISSN:0731-7085
1873-264X
DOI:10.1016/j.jpba.2008.11.015