Suitability of various chromatographic and spectroscopic techniques for analysis and kinetic degradation study of trelagliptin

Wafaa A Zaghary; Shereen Mowaka; Mostafa A Hassan; Bassam M Ayoub

doi:10.1038/s41598-017-17642-1

Suitability of various chromatographic and spectroscopic techniques for analysis and kinetic degradation study of trelagliptin

Sci Rep. 2017 Dec 8;7(1):17255. doi: 10.1038/s41598-017-17642-1.

Authors

Wafaa A Zaghary¹, Shereen Mowaka^{2

3

4}, Mostafa A Hassan^{1

4}, Bassam M Ayoub^{5

6}

Affiliations

¹ Pharmaceutical Chemistry Department, Faculty of Pharmacy, Helwan University, Ein Helwan, Cairo, 11795, Egypt.
² Analytical Chemistry Department, Faculty of Pharmacy, Helwan University, Ein Helwan, Cairo, 11795, Egypt.
³ Pharmaceutical Chemistry Department, Faculty of Pharmacy, The British University in Egypt, El-Sherouk city, Cairo, 11837, Egypt.
⁴ The Center for Drug Research and Development (CDRD), Faculty of Pharmacy, The British University in Egypt, El-Sherouk city, Cairo, 11837, Egypt.
⁵ Pharmaceutical Chemistry Department, Faculty of Pharmacy, The British University in Egypt, El-Sherouk city, Cairo, 11837, Egypt. bassam.ayoub@bue.edu.eg.
⁶ The Center for Drug Research and Development (CDRD), Faculty of Pharmacy, The British University in Egypt, El-Sherouk city, Cairo, 11837, Egypt. bassam.ayoub@bue.edu.eg.

Abstract

Multifaceted comparative analytical methods for trelagliptin (TRL) were investigated, applied to ZAFATEK tablets and HPLC-UV was selected for a degradation kinetic study. UPLC-MS/MS (Method I), UPLC-UV (Method II), HPLC-UV (Method III), UHPLC-UV (Method IV) and direct UV (Method V) methods were developed. Methods (I-V) showed satisfactory results using TRL concentration ranges of 50-800 ng/mL, 2.5-80 μg/mL, 5-100 μg/mL, 5-100 μg/mL and 5-50 μg/mL, respectively. Multiple Reaction Monitoring (MRM) of the transition pairs of m/z 358.176 to 134.127 for TRL and m/z 340.18 to 116.08 for alogliptin (IS) were employed utilizing positive mode Electrospray Ionization (ESI). The degradation kinetic study (Method VI) was carried out using 1 N HCl based on three different temperatures (70 °C, 80 °C and 90 °C). Through the optimized method-3, a good chromatographic separation of TRL from its major degradation product was achieved. Arrhenius plot was used in the kinetic study and the apparent 1^st order degradation rate constant (K), t_1/2, t₉₀, and the activation energies were calculated for each temperature and at 25 °C. The optimized UPLC-MS/MS method is suitable for further TRL assay either in biological fluids or in the presence of impurities.