Derivatization Method as a Residual Solvent of Acetic Acid by GC-MS Method in Empagliflozin Drug Substance: Development and Evaluation

The existing study is concerned with isolating unknown impurities from the bulk drug of Empagliflozin. The bulk drug Empagliflozin, Column: Agilent Technologies DB-FFAP 30mx 0.530mm, 1.0-micron, Instrument: PerkinElmer, GC 2014, for GC-MS Column: Agilent Technologies, Elite 5-MS, 30mm X 0.25 mm, 1.0-micron Instrument: Perkin Elmer, Carrier gas: Helium Source Temp.: 230°C, Transfer line: 250°C Inlet Temp.: 180°C, Diluent: Methanol Source energy: 70eV IR and 1HNMR. Column: DB-624,30m x 0.53mm x 3.0 um or equivalent oven Temperature. The injector and detector temperatures were 200°C and 240°C. For a 0.2 ml injection volume and 0.1-minute injection period, the (LOD) Limit of detection and (LOQ) Quantitation were 25 ppm and 76 ppm, respectively. In the Empagliflozin samples, the % recovery for acetic acid varied from 94.10 to 96.31. The devised technique was verified by specificity, linearity, accuracy, quantitation limit, precision, accuracy, and robustness by the principles set out by the International Council on Harmonisation. The IR shows that the Acetic acid impurity was unknown and confirmed. by GC-MS and NMR spectra. An unknown impurity was identified during bulk drug analysis. It was isolated and characterized using various analytical techniques, such as IR, NMR, GC, and GC-MS. Acetic acid, a genotoxic residual solvent, was identified as an unknown impurity and needs to be quantified and validated for routine analytical work. Residual solvents are undesirable compounds (solvents) produced or employed during the production of pharmaceutical formulations, excipients, or drugs, that don't seem to be eliminated by reasonable means in the final product. Method validation was carried out using GC-Column due to better separation in GC-HS mode. The validated method was proven specific, accurate, precise, and sensitive. The advanced and validated process can be implemented to determine and quantify Acetic acid in Empagliflozin bulk drug.