毛细管气相色谱法测定加替沙星中二甲基亚砜残留量

Determination of Dimethyl Sulfoxide in Gatifloxacin by CGC

目的用毛细管气相色谱方法测定加替沙星中的残留溶剂二甲基亚砜。方法色谱柱为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230℃,FID检测器温度为250℃,柱温为140℃,直接进样,分流比为10∶1,溶剂为二甲基甲酰胺。结果被测物均能得到很好分离,峰面积与质量浓度呈良好的线性关系,精密度和回收率良好。结论该法可用于加替沙星原料药中残留溶剂二甲基亚砜的检测。

Objective To establish a method of capillary gas chromatography（CGC）for the determination of dimethyl sulfoxide（residual solvent） in gatifloxacin. Methods Dimethyl sulfoxide in gatifloxacin was separated by DB-624 capillary column（30.0m×0.53mm,3.0μm） with FID detector. The carried gas was nitrogen. The injector temperature and the detector temperature was controlled at 230℃ and 250℃, respectively. The column temperature was maintained at 140℃. The sample was dissolved in dimethylformamide. The direct injection was used, the splitting - ratio was 10 ： 1. Results The measured solvent were separated completely. The calibration curve of dimethyl sulfoxide 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 dimethyl sulfoxide in gatifloxacin.