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Validation of residual solvents using gas chromatography with head space in active pharmaceutical ingredient

K.Balamurugan, K.Gokulakrishnan, M.Jamesdevaprabu, A.Vijayakumar

Anew, simple, specific, accurate and precise GC-HSmethod was developed for determination of residual solvents in zonisamide (anti-epileptic active pharmaceutical ingredient): Methanol, Diethyl ether, Isopropyl Alcohol, Ethylacetate, 1,1,2-Trichloroethene and toluene are the residual solvents present in zonisamide.Agilent DB-624 fused silica capillary column 30mï‚´ 0.53mmI.D with a phase thickness of 3.0µ. The split/split less injector was maintained at 140ï‚°C with a split injection 1:5 ratio and temperature of the FID was set to 250ï‚°C. The carrier gaswas nitrogen at a constant flowrate of 5ml/min. the column oven temperature programinvolved an initial temperature of 40ï‚°Cfor 20min; thiswas increased at 10ï‚°C/min to 240ï‚°Cand hold for 20 min. HS sampling was performed with a AOC 5000 headspace sampler (SHIMADZU). The method was validated for precision, ruggedness, linearity, Limit of detection and limit of quantification and recovery according to the International Conference on Harmonization (ICH) guidelines.