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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

来源:中国色谱网 作者:都述虎 王晓华 夏重道 刘文英 2007-5-18

摘要: New Page 1 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。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352~1758......


New Page 1

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。


关键词:穿龙薯蓣总皂苷 薯蓣皂苷元 毛细管气相色谱法


分类号:R927 文献标识码:A

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

DU Shu-huAnhui Institute of Medical Sciences,Hefei 230061) 
WANG Xiao-huaAnhui Institute of Medical Sciences,Hefei 230061) 
XIA Chong-daoAnhui Institute of Medical Sciences,Hefei 230061) 
LIU Wen-yingDepartment of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009) 

AbstractObjectiveThe 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 401 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 3521 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.


Keywords
total saponins of Dioscorea nipponica Makino,diosgenin,capillary column gas chromatography

 

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)
[2]ZHAO Jing-chan(赵景婵),GUO Zhi-an(郭治安),CHENG Xiao-fei(成小飞),et al.A normal-phase high performance liquid chromatographic method for the determination of diosgenin in Dioscorea nipponica Makino(穿龙薯蓣中薯蓣皂苷元的高效液相色谱法测定).Chin J Pharm Anal(药物分析杂志),2000,20(1):27(in Chinese)
[3]DA Shi-lu(达世禄),TANG Xiang-yi(唐祥怡),DA Hui-ning(达晖宁),et al.Determination of diosgenin in Dioscorea zingiberensis by using reversed-phase high performance liquid chromatography(盾叶薯蓣中薯蓣属植物中的反相高效液相色谱测定). Chin J Chromatogr(色谱),1992,10(2):98(in Chinese)
[4]TAO Li(陶莉),DA Hui-ning(达晖宁),DA Shi-lu(达世禄).Determination of diosgenin in Dioscorea zingiberensis by using gas chromatography(盾叶薯蓣中薯蓣皂甙元的气相色谱测定).Chin Tradit Herb Drugs(中草药),1991,22(6):252(in Chinese)
[5]TANG Shi-rong(唐世蓉),ZHANG Han-qing(张涵庆),DONG Yun-fa(董云发),et al.Content and identification of diosgenin in Dioscorea(薯蓣科植物甾体皂苷元的含量和鉴定).Acta Bot Sin(植物学报),1979,21(2):171(in Chinese)
[6]Cook B K.Determination of diosgenin in Dioscorea deltoidea and Dioscorea sylvatice by using gas-liquid chromatography.Analyst,1970,95(1):95
[7]John C Knight.Analysis of Fenugreek sapogenins by gas-liquid chromatography. J Chromatogr,1977,133:222
[8]ZHOU Ji-ming(周继铭),YANG Jia-zhen(杨家珍),ZHOU Ze-qing(周泽清).Content of diosgenin in Dioscorea from Sichuan region(四川地区薯蓣属植物中薯蓣皂甙元的含量).J Chin Med Mater(中药材),1985,(3):20(in Chinese)
[9]DU Shu-hu(都述虎),XIA Chong-dao(夏重道),FU Tie-jun(付铁军),et al.Studies on hydrolysis conditions of total saponins in Dioscorea nipponica Makino(穿龙薯蓣总皂苷水解条件的优化).Chin Tradit Pat Med(中成药),2000,22(9):608(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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