Abstract

CATEGORISATION OF OXIDATIVE DEGRADATION IMPURITIES AND ONE PROCESS IMPURITY OF SUVOREXANT BY LC-MS/MS, HR-MS AND 1D AND 2D NMR; AUTHENTICATION OF SUVOREXANT INGREDIENT AND DEVELOPMENT IMPURITIES BY HPLC AND UPLC

Hari Prasad Vanam, E. A. Lohit, P. Kumar and A. Saranga Pani*

ABSTRACT

During the oxidative (10% H202) degradation of Suvorexant, around 1.0% of one impurity and less than 1.0% four impurities were found by a new High Performance Liquid chromatography assay and related substance method. The mass numbers of 1.0 % impurity was 469[M+H]+, remaining four impurities were 172[M+H]+, 467[M+H]+, 483[M+H]+, 485[M+H]+. The 469[M+H]+, 485[M+H] and 172[M+H]+ impurities were characterized by using the LC-MS/MS, HR-MS and 1D, 2D NMR spectroscopic data and 172[M+H]+ impurities was prepared synthetically and co-injected. The retention time was matching with the unknown degradants impurity in HPLC. The developed Mass compatible HPLC and UPLC methods were validated for process impurities and drug substance as per ICH Q2 R1 guidelines.

Keywords: Characterization, Mass spectrometry, 1D and 2D NMR, Validation, HPLC, UPLC.