摘要
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.
作者
段和祥
陈希
刘绪平
鄢雷娜
DUAN Hexiang;CHEN Xi;LIU Xuping;YAN Leina(Jiangxi Institute for Drug Control,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang,Jiangxi 330029,China)
出处
《今日药学》
CAS
2018年第10期665-667,共3页
Pharmacy Today
基金
江西省食品药品监督管理局科研项目(2016YP18)