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

Studies on the Determination of Diosgenin in Total Saponin of Dioscorea nipponica Makino by Capillary Gas Chromatography

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(Methylsiloxane)不锈钢毛细管柱 ,柱箱温度 2 70℃ ,柱头压 12 3 7kPa ,汽化室温度 330℃ ,检测器温度 310℃ ,载气 (N2 )流速 2 0mL·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 35 2～ 175 8ng范围内峰面积与其浓度线性关系良好 (r=0 9996 ) ,样品平均回收率为 95 6 5 % ,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。

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,1237 kPa as column pressure,330 ℃ as inlet heater,310 ℃ as detector heater, 20 mL·min -1 as N\-2 flow and 40∶1 as split ratio.Results:It can separate diosgenin and its primary impurity.The calibration curve was linear (r=0999 6) within the range of 352～1 758 ng for diosgenin.The average recovery and precision (RSD) for diosgenin were 9565% (n=5) and 10%(n=5) respectively.Conclusions:The method is not derivatived and the result of separation is good.The analysis is accurate,satisfactory.