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LC-MS based stability-indicating method for studying the degradation of lonidamine under physical and chemical stress conditions
Journal article   Open access   Peer reviewed

LC-MS based stability-indicating method for studying the degradation of lonidamine under physical and chemical stress conditions

Ankit Kanaiyalal Rochani, Margaret Wheatley, Brian Edward Oeffinger, John Robert Eisenbrey and Gagan Kaushal
Research in pharmaceutical sciences, v 15(4), pp 312-322
01 Jul 2020
PMID: 33312209
url
https://doi.org/10.4103/1735-5362.293509View
Published, Version of Record (VoR)CC BY-NC-SA V4.0 Open

Abstract

Chemistry, Medicinal Life Sciences & Biomedicine Pharmacology & Pharmacy Science & Technology
Background and purpose: Lonidamine is a hexokinase II inhibitor, works as an anticancer molecule, and is extensively explored in clinical trials. Limited information prevails about the stability-indicating methods which could determine the forced degradation of lonidamine under stressed conditions. Hence, we report the use of a rapid, sensitive, reproducible, and highly accurate liquid chromatography and mass spectrometry method to analyze lonidamine degradation. Experimental approach: The Xbridge BEH shield reverse phase C18 column (2.5 mu m, 4.6 x 75 mm) using isocratic 50:50 water: acetonitrile with 0.1% formic acid can detect lonidamine with help of mass spectrometer in tandem with an ultraviolet (UV) detector at 260 nm wavelength. Findings/ Results: A linear curve with r(2) > 0.99 was obtained for tandem liquid chromatography-mass spectrometry (LC-MS)-UV based detections. This study demonstrated (in the present set up of isocratic elution) that LC-MS based detection has a relatively high sensitivity (S/N (10 ng/mL): 220 and S/N (20 ng/mL): 945) and accuracy at lower detection and quantitation levels, respectively. In addition to developing the LC-MS method, we also report that the current method is stability-indicating and shows that lonidamine gets degraded over time under all three stress conditions; acidic, basic, and oxidative. Conclusion and implications: LC-MS based quantitation of lonidamine proved to be a better method compared to high-performance liquid chromatography (HPLC)-UV detections for mapping lonidamine degradation. This is the first report on the stability-indicating method for studying the forced degradation of lonidamine using LC-MS method.

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Collaboration types
Domestic collaboration
Web of Science research areas
Chemistry, Medicinal
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