Determination of Residual Solvents in Fasudil Hydrochloride by Headspace GC

OBJECTIVE To develop a headspace gas chromatography method for determining residual organic solvents-methanol, dichloromethane, ethanol in fasudil hydrochloride. METHODS Headspace gas chromatography was added using an Agilent HP-INNOWAX capillary column(30 m´0.32 mm, 0.5 µm ) with temperature programming. The initial column temperature was 35 ℃ maintained for 12 min and then raised (40 ℃·min-¹) to 200 ℃ for 5 min with nitrogen gas as carrier and FID as detector. The flow of carrier is 1.0 mL·min^-1. The injection port and detector temperature were 200 ℃ and 250 ℃, respectively. RESULTS With external standard method, the average recoveries of methanol, dichloromethane and ethanol were 96.21%, 77.96% and 95.56%, respectively. And three solvent residuals in samples were less than the limits of Ch.P. CONCLUSION The method can be used for the determination of residual solvents in fasudil hydrochloride.