Development and Validation of Lc-ms/ms Method for Detection and Characterisation of Forced Degradation Products of Dapagliflozin Propanediol Monohydrate and Vildagliptin: Greenness Assessment Using Agree
Year: 2025
Type: article
Abstract: The goal of current research was to illustrate a method for separating, identifying, and characterizing the degradation products of Vildagliptin and Dapagliflozin Propanediol Monohydrate in bulk using the liquid chromatography-mass spectrometry (LC-MS/MS) methodology. The drugs were exposed to basic, thermal, oxidative, acidic, and photolytic stimuli in line with International Conference on Harmonization guideline Q1A(R2). When exposed to oxidative, basic, and acidic hydrolysis stimuli, the mentioned API showed extensive deterioration. Under both thermal and photolytic stress, the drug products remained stable. Four degradation products were identified and separated. Using acetonitrile: 10 mM ammonium acetate (pH 5) (30:70, v/v) as eluent, the drug and its degradation products were resolved utilising a Zorbax C18 (5µm, 150 × 4.6 mm) column. Vildagliptin and Dapagliflozin Propanediol Monohydrate showed linearity from 5 – 15 and 0.5 – 1.5 μg/ml individually. The % RSD for precision, accuracy, and robustness was found to be less than 2%. The exact mass and MS/MS fragmentation pattern, which were acquired employing LC-ESI-TQMS/MS, serve as the basis for the hypothesized structure of degradation products and the accompanying pathways. Optimizing the manufacturing as well as quality assurance parameters of the drugs under investigation would be made possible by the proposed degradant structures and pathways. Using the AGREE tool, the result score was 0.60. Hence, the method was found to be eco-friendly.
Source: RASAYAN Journal of Chemistry
Authors: S. M. Rathod, C. M. Aakhunji, N. C. Patel
Language: English
Subfield: Analytical Chemistry
Field: Chemistry
Domain: Physical Sciences
Open Access status: diamond
OpenAlex ID: W4411670282