顶空毛细管气相色谱法测定加替沙星中的残留溶剂

目的建立顶空毛细管气相色谱方法测定加替沙星中的残留溶剂。方法采用气相色谱法，色谱柱为DB-624（6％氰丙基苯基-94％二甲基聚硅氧烷固定液）石英毛细管柱（30.0m×0．53mm，3．0μm），载气为氮气，进样口温度为200℃，FID检测器温度为250℃；枉温为60℃，保持4min，以20℃／min的升温速率升到200℃，保持2min；顶空进样，平衡温度为105℃，平衡时间为30min，分流比为1：1；溶剂为二甲基甲酰胺。结果被测物均能得到很好的分离，峰面积与质量浓度线性关系良好，精密度和回收率良好。结论顶空毛细管气相色谱法可用于加替沙星原料药中残留溶剂的检测。

Determination of Residual Solvents in Gatifloxacin by CGC

Objective To establish a method of headspace capillary gas chromatography（CGC） for the determination of residual solvents in gatifloxacin. Methods The residual solvents in gatifloxacin were separated by DB- 624 capillary column（30. 0 m ×0. 53 mm,3.0 μm）with the FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature was controlled at 200℃ and 250℃, respectively. The column temperature was maintained at 60℃ for 4 min, then raised at a rate of 20℃ per min to 200℃ and maintained at 200℃ for 2 min. The sample was dissolved in dimethylformamide. The containers of head-space injector were in equilibrium at 10℃ for 30 min, the splitting- ratio was 1 ： 1. Results The measured solvents were separated completely. The calibration curve of each solvent showed a good linear relationship with good precision and accuracy. Conclusion The established method is accurate and reliable. It can be used for the determination of The residual solvents in gatifloxacin.