林生文,李玮玲,朱炳辉,陆惠文
Lin Shengwen; Li Weiling 1; Zhu Binghui; Lu Huiwen(Guangdong Province Constitute for Drug Control;

• 1:广东省药品检验所
• 2:中国药科大学分析化学教研室
• 3:广东省药品检验所
• 4:广东省药品检验所 广州510180

摘要(Abstract)：

目的　建立盐酸尼非卡兰原料中有机溶剂残留物的测定方法。方法　采用顶空进样—毛细管气相色谱法 ,色谱柱为用5 %苯基 95 %甲基聚硅氧烷化学交联石英毛细管柱 ( 30m× 0 .5 3mm ,5 μm ) ;柱温 :5 0℃ ,维持 1min ,以每分钟 12℃升温至12 0℃ ,维持 1min ;检测器FID ,温度 2 80℃。用外标法测定盐酸尼非卡兰原料中有机溶剂残留量。结果　建立的色谱方法在所考察的浓度范围内 ,线性关系良好 ,各溶剂回收率符合要求。结论　建立的色谱方法灵敏、准确 ,适用于盐酸尼非卡兰原料中有机溶剂残留量的检测
Objective To establish a method for determination of organic solvent residue in material of nifekalant hydrochloride. Methods Headspace gas chromatography is applied to quantitative analysis. Chromatographic conditions are :CP Sil 8 capillary column(30m×0.53mm);headspace injector;maintain column at a temperature of 50℃ for 1 minute, then raising the temperature at a rate of 12℃ per minute to 120℃ and maintaining it at 120℃ for 1 minute and the temperature of flame ionization detector (FID) at 280℃. Results are obtained by external calibration. Results The calibration curve of organic solvent residue in material of nifekalant hydrochloride has a good linear relationship,The recovery meets the requirement. Conclusion The established method is sensitive and accuracy,it can be applied to determine the organic solvent residue in material of nifekalant hydrochloride.

关键词(KeyWords)： 盐酸尼非卡兰;有机溶剂残留量;顶空-气相色谱法
nifekalant hydrochloride;organic solvent residue;headspace gas chromatographic determination

Abstract:

Keywords:

基金项目(Foundation):

作者(Authors): 林生文,李玮玲,朱炳辉,陆惠文
Lin Shengwen; Li Weiling 1; Zhu Binghui; Lu Huiwen(Guangdong Province Constitute for Drug Control;

参考文献(References)：

• [1]王卫.药品中有机溶剂残留量及其测定[J].天津药学,2001,13(3):26～29.
• [2]国家药典委员会.中华人民共和国药典2000年版二部附录[M].北京:化学工业出版社,2000.64.
• [3]马广慈主编.药物分析方法与应用[M].北京:科学出版社,2000.671.