Novel analytical method development and validation for the determination of residual solvents in amlodipine besylate by gas chromatography

摘要

The purpose of this research study was to develop and optimize an accurate and precise GC method for the determination of Residual solvents (n-Hexane, Methanol, Isopropyl Alcohol, Toluene, O-Xylene, DMF & Acetic acid) in Amoldipine besylate using the DB-FFAP, 30 m x 0.53mm ID, 1.0 μm column as stationary phase. The injection volume of samples taken is 1 μl. The split ratio of the injection was 1:10. The temperature maintained at the injector and detector was to be 220ºC and 260ºC respectively. Nitrogen gas having make up flow 40 ml/ minute and having column flow 2.8 ml/minute used as mobile phase and the detection was by FID. The flow of hydrogen and Air was maintained at 30ml/min and 300ml/min respectively. The diluent used is Dimethyl Sulfoxide. All solvents well resolved each other with diluents peak RT at 21 min in total run time of 24.25 min. The RTs observed for the Residual solvents n-Hexane, Methanol, Isopropyl Alcohol, Toluene, O-Xylene, DMF & Acetic acid are 3.03, 6.20, 6.87, 10.27, 14.57, 17.49 &19.54 respectively. The method was validated as meets the all regulations of System suitability, Specificity, Method Precision, Linearity, LOD & LOQ, Precision of LOQ and Accuracy/Recovery under ICH specifications.