穿龙薯蓣总皂苷中薯蓣皂苷元含量的毛细管气相色谱法研究

摘要

Objective：The method of the determination of diosgenin in total saponins of Dioscorea nipponica Makino is developed.Methods:This method used HP-1(Methyl siloxane) capillary column with 270 ℃ as oven heater,123.7 kPa as column pressure,330 ℃ as inlet heater,310 ℃ as detector heater, 2.0 mL*min-1 as N2 flow and 40∶1 as split ratio.Results:It can separate diosgenin and its primary impurity.The calibration curve was linear (r=0.999 6) within the range of 352～1 758 ng for diosgenin.The average recovery and precision (RSD) for diosgenin were 95.65% (n=5) and 1.0%(n=5) respectively.Conclusions:The method is not derivatived and the result of separation is good.The analysis is accurate,satisfactory.%目的：建立毛细管气相色谱法测定穿龙薯蓣总皂苷中薯蓣皂苷元的含量。方法：采用HP-1(Methyl siloxane)不锈钢毛细管柱，柱箱温度270 ℃，柱头压123.7 kPa，汽化室温度330 ℃，检测器温度310 ℃，载气(N2)流速2.0 mL*min-1，分流比40∶1，对穿龙薯蓣总皂苷中薯蓣皂苷元含量进行测定。结果：能将薯蓣皂苷元及其主要杂质进行分离，薯蓣皂苷元在352～1 758 ng范围内峰面积与其浓度线性关系良好(r=0.999 6)，样品平均回收率为95.65%，精密度RSD为1.0%(n＝5)。结论：该法测定样品无需衍生化，分离效果好，分析快速准确。