Determination of Seven Kinds of Residual Solvents in Bicalutamide by GC / 中国药师

ABSTRACT

Objective:To establish a headspace GC method for the determination of 7 kinds of residual solvents in bicalutamide, including dichloromethane, n-hexane, tetrahydrofuran, ethanol, ether, acetone and ethyl acetate. Methods: The residual solvents in the substance were determined by GC equipped with an FID detector and linked with an Agilent DB-624 capillary column (30. 0 m × 0. 25 mm × 1. 4 m). The inlet temperature was 200℃ and the FID detector temperature was 250℃. The column temperature was raised by programthe initial temperature was 35℃, maintained for 13 min, raised to 180℃ with a rate of 100℃/min, and maintained for 5 min. The carrier gas was nitrogen and the flow rate was 1. 2 ml·min-1. The heated temperature of the headspace oven was 90℃, the heated time lasted 30 min, and the injection volume was 1. 0 ml. The solution medium was dimethyl sulphoxide (DMSO). Results:Each solvent could be completely separated, and the calibration curve of each solvent showed good linear relationship with good accuracy. Conclusion:The method can be applied for the determination of residual solvents in bicalutamide.