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摘 要: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270℃,柱头压123.7kPa,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352~1758ng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95.65%,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。
Studies on the Determination of Diosgenin in Total Saponin of Dioscorea nipponica Makino by Capillary Gas Chromatography DU Shu-hu(Anhui
Institute of Medical Sciences,Hefei 230061) Abstract: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.
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作者单位:都述虎(安徽省医学科学研究所合肥
230061) 王晓华(安徽省医学科学研究所合肥 230061) 夏重道(安徽省医学科学研究所合肥 230061) 刘文英(中国药科大学药物分析教研室南京 210009) 参考文献: [1]FANG Yi-wei(方一苇),ZHAO
Jia-jun(赵家俊),HE Yu-zhen(贺玉珍).Elucidation of the chemical
structures of two steroid sapogenins of Dioscorea nipponica Makino(穿龙薯蓣中两种水难溶性甾体皂苷的结构研究).Acta
Pharm Sin(药学学报),1982,17(5):387(in Chinese) 收稿日期:2000年5月8日 出版日期:2001年3月31日 |
原载于《药物分析杂志》2001 Vol.21 No.2 P.116-119
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