顶空毛细管气相色谱法测定门冬氨酸洛美沙星原料中6种有机溶剂残留量

Determination of Six Residual Organic Solvents in Lomefloxacin Aspartate by Headspace Capillary Gas Chromatography

目的建立顶空毛细管气相色谱(GS)法测定门冬氨酸洛美沙星原料中乙醇、丙酮、正丙醇、乙酸乙酯、N,N-二甲基甲酰胺、二甲基亚砜6种有机溶剂的残留量。方法采用气相色谱法,色谱柱为DB-624石英毛细管柱(30.0 m×0.53 mm,3.0μm),载气为氮气,进样口温度为220℃,FID检测器温度为250℃;柱温:40℃保持5 min,以15℃·min^(-1)升温速率升至200℃保持5 min;顶空进样条件:顶空瓶温度为80℃,平衡时间为35 min,分流比3∶1,溶剂为水。结果 6种有机溶剂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。结论该方法简便、快捷,灵敏度高,结果准确可靠,适用于门冬氨酸洛美沙星原料中有机溶剂残留量的检测。

OBJECTIVE To establish a method of headspace capillary gas chromatography for the content determination of six residual organic solvents（ ethanol,acetone,n-propanol,ethyl acetate,N,N-dimethylformamide,dimethyl sulfoxide） in lomefloxacin aspartate. METHODS The residual organic solvents in lomefloxacin aspartate were separated by DB-624 capillary column（ 30.0 m×0.53 mm,3.0 μm） with the FID detector. The carrier gas was nitrogen. The injector temperature and detector temperature were controlled at 220 ℃ and 250 ℃,respectively. The column temperature was maintained at 40 ℃ for 5 min,then raised at a rate of 15 ℃per min to 200 ℃ and maintained 5 min. The sample was dissolved in water. The containers of head-space injector were in equilibrium at 80 ℃ for 35 min,the splitting-ratio was 3 ∶1. RESULTS The measure 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 simple,rapid,sensitive,accurate and reliable. It is suitable for the content determination of residual organic solvents in lomefloxacin aspartate.