Determination of Residual Solvents in Ceftazidime Bulk Drug by Headspace Gas Chromatography
Objective To establish a headspace gas chromatography(GC)method for the determination of residual organic solvents in ceftazidime bulk drug.Methods The residual solvents were determined by headspace GC on an Agilent DB-624(60 m×0.32 mm,1.8 μm)capillary column with an FID detector.The carrier gas was nitrogen at a flow rate of 1.5 ml/min.The injection volume was 1.0 ml and the split ratio was 5:1.The inlet temperature was 200℃and the detector temperature was 280℃,and programmed heating was adopted:the initial temperature was kept at 40℃for 10 min,raised to 100℃at the rate of 10℃/min,raised to 160℃at the rate of 30℃/min and kept for 3 min,then raised to 230℃at the rate of 40℃/min and kept for 3 min.The headspace condition is equilibrated at 80℃for 30 min.Results The solvents to be detected were well separated.There were good linear relationships within the investigated concentration ranges(r=0.9999).The average recoveries were 95%-108%,with RSDs(n=9)no more than 2.0%.The results of intermediate precision tests were good,with RSDs(n=12)less than 2.0%.Conclusion This method is simple to operate and can accurately detect the organic solvent residues in ceftazidime bulk drug.
ceftazidimeresidual solventheadspace gas chromatograph
万方数据
维普
