762 © The Author(s) 2021. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com Journal of Chromatographic Science, 2021, Vol. 59, No. 8, 762–769 https://doi.org/10.1093/chromsci/bmaa136 Advance Access Publication Date: 13 January 2021 Article Article Quality and Stability Profile Assessment of the Recent Antidiabetic Omarigliptin by Using Different Chromatographic Methods Mahmoud A. Tantawy 1,2, *, Amal M. Hassan 3 , Maha A. Hegazy 1 and Khadiga M. Kelani 1,3 1 Analytical Chemistry Department, Faculty of Pharmacy, Cairo University, Kasr el Aini Street, 11562, Cairo, Egypt, 2 Chemistry Department, Faculty of Pharmacy, October 6 University, 6 October City, 12585, Giza, Egypt, and 3 Analytical Chemistry Department, Faculty of Pharmacy, Modern University for Technology and Information, El-hadaba El-Wosta, Mokatam, 5th district, 11571, Cairo, Egypt *Author to whom correspondence should be addressed. Email: matantawy@hotmail.com Received 13 August 2020; Revised 11 November 2020; Accepted 16 December 2020 Abstract In a contribution to stability profiling of the recent antidiabetic drug, omarigliptin (OMR), two stability-indicating chromatographic methods were developed and validated. Stability profiling was performed for OMR under different stress conditions as acidic, alkaline, oxidative, photolytic and thermal degradations. Structures elucidation to all formed degradation products were identified using IR and mass spectrometry. Thin Layer Chromatography (TLC) and High-Performance Liquid Chromatography (HPLC) were used. In TLC-densitometric method, aluminum TLC plates precoated with silica gel G.F 254 were used as stationary phase along with methanol: ethyl acetate: 33% ammonia (2:8:1,v/v/v ) as mobile phase. The obtained chromatograms were scanned at 254 nm over concertation range of 5–70 μg band −1 for OMR. The second chromatographic method was an HPLC one with diode array detection and RP-C18 column with isocratic elution. Mobile phase used was composed of phosphate buffer pH 3.5: acetonitrile (80, 20, v/v ), delivered at flow rate of 1.0 mL min −1 . Diode array detector was adjusted at 230 nm with linearity range of 15–180 μg mL −1 for OMR. Several factors affecting TLC and HPLC efficiency have been carefully studied. The developed methods were validated according to International Conference on Harmonization guidelines and successfully applied for assessment of OMR in bulk powder and tablets. Introduction Diabetes mellitus (DM) is considered one of the most common health disorders in the world (1). As indicated by World Health Organi- zation (WHO), there are more than 422 million people suffering from this disease; moreover, in 2016, 1.6 million deaths were directly caused by DM (2). There are two main types of DM: type 1 and type 2. Both types of diabetes are chronic. Several drugs have been developed for treatment of type 2 DM. Dipeptidyl peptidase-4 (DPP- 4) inhibitors are among the most important classes used for DM treatment (3, 4). Stability studies are essential for shelf life prediction of phar- maceutical products as well as verification of quality, safety and efficacy (5). Additionally, they help in identification of the possible degradation pathways under different stress conditions (6). Stability- indicating methods are then developed for detection and quantifica- tion of intact drugs along with their degradation product (s) without any interference (7–10). Omarigliptin (OMR) is chemically designated as (2R,3S,5R)- 2-(2,5-difluorophenyl)-5- [2-(methylsulfonyl)-2,6-dihydropyrrolo [3,4-c]pyrazol-5(4H)- yl]tetrahydro-2H-pyran-3-amine] (11). It is Downloaded from https://academic.oup.com/chromsci/article/59/8/762/6090333 by guest on 03 April 2023