Static Head Space Gas Chromatographic Method For Quantitative Determination Of Residual Solvents In Canagliflozin API

The pharmaceutical industry is facing a unnerving challenge in the control of impurities; Residual solvents play as an important role in the synthesis of drugs substances; according to the good manufacturing process measuring residual solvents is an integral part of impurities profile assessment for pharmaceutical products and is mandatory for the release testing of all active pharmaceutical ingredients. In synthesing process of canagliflozin API many solvents being used, to analyses these solvent a sensitive static head space gas chromatography (GC HS) with flame ionization detector (FID) method was developed successfully and validated for residual solvents determination of Canagliflozin API. The head space parameters and chromatographic condition, such as split ratio, flow rate and oven program temperature, were optimized to enhance sensitivity and chromatographic resolution. The optimized parameters are 1-methyl-2-pyrrolidone as diluent, equilibration temperature for head space 40°C for 8 min, Oven temperature program 40°C to 200°C with 20°C ramping, Nitrogen carrier gas and DB-624, 30m length and 0.32mm ID, film thickness 1.8 mm a capillary column used. The proposed method was found to be suitable for the determination of ten different residual solvents. The validation results indicate that method is specific, sensitive, accuracy linear and robust, The obtained recovery ranging from 80% to 120% and regression coefficient was higher than 0.999 for all the solvent.