毛细管气相色谱法测定哌拉西林中残留溶剂

Determination of residual solvents in piperacillin by capillary gas chromatography

目的建立气相色谱法分离测定哌拉西林中残留溶剂二氯甲烷、丙酮与乙酸乙酯。方法以HP-624毛细管柱为色谱柱(30 m×0.53 mm×3.00μm),载气为氮气,采用氢火焰离子化检测器,进样口温度为140℃,检测器温度为250℃,采用程序升温(60℃,保持12 min,以20℃.min-1升至240℃),采用顶空进样法,进样量1.0 ml。结果在本色谱系统中,二氯甲烷、丙酮与乙酸乙酯互不干扰,分离度及检出灵敏度均符合要求,最小检出浓度分别为1.43,0.20,0.20 mg.L-1。结论本方法可测定哌拉西林中残留溶剂量,方法简单、准确。

Ahn To determine the contents of residual volatile organic solvents：dichloromethane, acetone and ethyl acetate in piperacillin by GC. Methods HP-624 （30m×0.53mm×3.00μm） sillica capillary column was used. The carrier gas was nitrogen. The injection port and detector temperatures were 140℃ and 250℃ respectively. Headspace injection method initial temperature was kept at 60℃ for 12 min, and then the temperature was raised to 240℃ at the rate of 20℃ · min^- 1. Results The three residual volatile organic solvents were separated completely. The resolution and sensitivity were acceptable. The limits of detection were 1.43, 0.20 and 0.20 mg · L^-1, respectively. Conclusion The method is simple, rapid, precise,and suitable for determination of residual volatile solvents in piperacillin.