盐酸尼非卡兰有机溶剂残留量测定

Determination of organic solvent residue in material of nifekalant hydrochloride

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 。

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.