Open AccessIdentification and Characterization of Forced Degradation Products for Dofetilide using Rapid and Sensitive UPLC-MS/MS Method and HRMS Studies
Author(s) -
M. Ajay Babu,
G. Krishna Mohan,
N. Naresh,
Ch. Krishnam Raju,
Sharad D. Mankumare
Publication year - 2019
Publication title -
asian journal of chemistry/asian journal of chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.145
H-Index - 34
eISSN - 0975-427X
pISSN - 0970-7077
DOI - 10.14233/ajchem.2019.22220
Subject(s) - chemistry , chromatography , degradation (telecommunications) , forced degradation , dofetilide , high performance liquid chromatography , mass spectrometry , reversed phase chromatography , medicine , telecommunications , qt interval , computer science
A simple, rapid and efficient method has been developed and validated using ultra UPLC combined with Q-ToF MS system for recognition and characterization of forced degradation products obtained from dofetilide degradation studies. The dofetilide drug is an antiarrhythmic and belongs to Class III and it was treated with various stress conditions like acidic, basic, oxidative, photolytic and thermal conditions as per ICH guidelines. The main drug shows extensive degradation towards oxidative degradation conditions and single degradation product was identified through chromatogram. Thechromatographic separation among main and its impurities were attained through 2.1 × 150, 1.8 μm column from gradient elution using UPLC and its detection at wavelength 230 nm. The validation was performed for the developed method using various parameters like specificity, linearity and robustness studies. Waters Synapt G2 Q TOF system was used and performed MSn studies to establish mass spectral fragmentation pathway for drug and its degradation products and determined accurate massesstudy. The efficiency of this method was helpful to identify and characterize the drug and degradation products using LC/MSn techniques.