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目的:建立顶空毛细管气相色谱方法测定克拉维酸钾原料中的残留溶剂丙酮。方法:色谱柱为HP-FFAP石英毛细管柱(25 mm×0.32 mm;0.5μm),FID为检测器载气为氮气。检测器温度:180℃;进样口温度:150℃;柱温:60℃。顶空进样,平衡温度为100℃,平衡时间为20 min,分流比为5:1。丁酮为内标物。结果:丙酮的线性范围是2～200μg·ml~(-1),r= 0.999 5,平均回收率分别为99.2%,99.3%及100.5%。结论:该法可用于克拉维酸钾原料中残留溶剂丙酮的检测。
Objective: To establish a headspace capillary gas chromatographic method for the determination of residual solvent acetone in potassium clavulanate. Methods: HP-FFAP silica capillary column (25 mm × 0.32 mm; 0.5 μm) was used as the chromatographic column. FID was the carrier gas of nitrogen gas. Detector temperature: 180 ° C; inlet temperature: 150 ° C; column temperature: 60 ° C. Headspace injection, the equilibrium temperature of 100 ℃, the balance time of 20 min, split ratio of 5: 1. Methyl ethyl ketone as an internal standard. Results: The linear range of acetone was 2 ~ 200μg · ml ~ (-1), r = 0.999 5, the average recoveries were 99.2%, 99.3% and 100.5% respectively. Conclusion: This method can be used for the determination of residual solvent acetone in potassium clavulanate.