薯蓣皂甙元的分光光度法测定

本文以黄姜为主要对象研究了薯蓣皂甙元的定量测定方法，以香荚兰醛－高氯酸为显色剂，冰醋酸为溶剂，使皂甙元显色，用分光光度法在波长为５３０ｎｍ处测定薯蓣皂甙元的含量。从植物中提取的皂甙元不需分离可直接测定。在１．００～２０．００ｍｇ／Ｌ范围内呈良好的线性关系。     

Comparison of ultrasound and microwave assisted extraction of diosgenin from Trigonella foenum graceum seed

From the recent market trend, there is a huge demand for the bioactive compounds from various food matrices that could be capable enough to combat the emerging health effects in day-to-day life. Fenugreek is a well-known spice from ancient times for its medicinal and health benefits. In the present study, two methods of green extraction microwave (MAE) and ultrasound (UAE) assisted were studied in regard of extraction of fenugreek diosgenin. In this study, solvent type (acetone, ethanol, hexane and petroleum ether), solvent concentration (40, 60, 80 and 100%) and treatment time (1.5, 3.0, 4.5 and 6.0 min and 30, 40, 50 and 60 min for MAE and UAE method respectively) was varied to observe the effect of these parameters over extract yield and diosgenin content. The results of this study revealed that treatment time, type of solvent and its concentration and method adopted for extraction of diosgenin has significant effect. In relation with better yield extract and diosgenin content, the yield of fenugreek seed extract was 7.83% with MAE and 21.48% with UAE of fenugreek seed powder at 80% ethanol concentration at 6 and 60 min respectively. The content of diosgenin was observed in fenugreek seed powder extract was 35.50 mg/100 g in MAE and 40.37 mg/100 g in UAE with 80% ethanol concentration at 6 and 60 min respectively. The overall range of yield of fenugreek extract was varied from 1.04% to 32.48% and diosgenin content was 15.82 mg/100 g to 40.37 mg/100 g of fenugreek seed powder including both extraction methods. This study revealed that UAE would impose better ways for preparing fenugreek extract and observing diosgenin content from fenugreek seeds.     

Diosgenin aus Yams als Hormonvorstufe

Diosgenin as a sapogenin is the aglycone of the saponine dioscin. It is occuring in plants such as yam, from which it is isolated on industrial scale since the 1940ies. Plant diosgenin is a starting substance for the synthesis of human, i.e. animal, hormones and “the pill”, which as a hormonal contraception represents a revolution in the control of human sexuality. History, isolation and spectroscopy of this complex sapogenin are reported. This article extends the briskly discussed feature “50 years pill in Germany” (Streller & Roth, ChiuZ, 2011 [( 1 ) ]) by a particular compound example. It belongs to the series on isolation and spectroscopy of natural products in this journal.     

An improved synthesis of pennogenin

An improved synthesis of pennogenin, a bioactive component of Chinese herb “Chonglou” (Paris), is described. A ring-switching process opened the ring E of diosgenin and allowed the use of a hydroxyl-directed diboration/oxidation to introduce C17α-OH, hence eliminating the use of OsO₄. This strategy might be rendered to synthesize similar steroids with C17α-OH.     

一系列薯蓣皂甙元-α-L鼠李糖基-(1→2)和(1→4)-β-D葡萄糖甙的1H和13C NMR归属

用同核和异核二维核磁共振方法全归属了一系列合成的薯蓣皂甙元-α-鼠李糖基-β-D葡萄糖甙的¹H和¹³C核磁共振谱线.这些薯蓣葡萄糖甙是薯蓣皂甙元-β-D葡萄糖甙(1),薯蓣皂甙元-α-L鼠李糖基(1→2)-β-D葡萄糖甙(2),薯蓣皂甙元-α-L鼠李糖基(1→4)-β-D葡萄糖甙(3),薯蓣皂甙元[-α-鼠李糖基-(→2)]-α-L鼠李糖基→-(1→4)-β-D葡萄糖甙(4)以及薯蓣皂甙元[-α-L鼠李糖基-(1→2)]-β-D阿拉伯糖基-(1→4)-β-D葡萄糖甙(5).     

一系列薯蓣皂甙元-β-D葡萄糖基-(1→2)和(1→3)-β-D葡萄糖甙的1H和13C NMR归属

用同核和异核二维核磁共振方法全归属了一系列合成的薯蓣皂甙元-β-D葡萄糖甙的¹H和¹³C核磁共振谱线.这些薯蓣葡萄糖甙是薯蓣皂甙元-β-D葡萄糖甙(1),薯蓣皂甙元-β-D葡萄糖基-(1→2)-β-D葡萄糖甙(2),薯蓣皂甙元,-β-D葡萄糖基-(1→3)-β-D葡萄糖甙(3),薯蓣皂甙元[-β-D葡萄糖基-(1→2)-β-D葡萄糖基(1→3)-β-D葡萄糖甙(4)以及薯蓣皂甙无[-α-L鼠李糖基-(1→2)]-β-D葡萄糖基-(1→3)-β-D葡萄糖甙(5).     

分光光度法测定薯蓣皂苷元

采用高氯酸反应使薯蓣皂苷元显色 ,对影响显色反应的主要因素进行了考察 ,于 41 0nm波长处对穿山龙中薯蓣皂苷元的含量进行测定 ,测定结果与高效液相色谱法相近。方法的线性范围为 3.1 2～2 1 .84μg mL ,适用于薯蓣皂苷元提取过程中的常规检测     

七叶一枝花中薯蓣皂苷的分离及结构鉴定研究

本文利用高效液相色谱-串联质谱联用方法研究了七叶一枝花中的薯蓣皂苷。实验采用高效液相色谱分离了七叶一枝花中的3种薯蓣皂苷;通过与电喷雾质谱联用获得了这几种化合物的分子量信息;再用MS/MS获得了这几种化合物进一步的结构信息。采用此方法可快速分析鉴定从七叶一枝花中分离得到的薯蓣皂苷。     

一系列薯蓣皂甙元-β-D葡萄糖基-(1→2)和(1→3)-β-D葡萄糖甙的1H和13C NMR归属

用同核和异核二维核磁共振方法全归属了一系列合成的薯蓣皂甙元-β-D葡萄糖甙的1H和13C核磁共振谱线．这些薯蓣葡萄糖甙是薯蓣皂甙元-β-D葡萄糖甙（1）,薯蓣皂甙元-β-D葡萄糖基-（1→2）-β-D葡萄糖甙（2）,薯蓣皂甙元,-β-D葡萄糖基-（1→3）-β-D葡萄糖甙（3）,薯蓣皂甙元[-β-D葡萄糖基-（1→2）-β-D葡萄糖基（1→3）-β-D葡萄糖甙（4）以及薯蓣皂甙无[-α-L鼠李糖基-（1→2）]-β-D葡萄糖基-（1→3）-β-D葡萄糖甙（5）．     

薯蓣皂甙元的极谱催化波及其应用

采用线性扫描极谱技术,研究了薯蓣皂甙元(C27H42O3,简称皂素)的极谱催化波及应用。结果表明,在pH=5.3±0.5的BR缓冲溶液、0.1mol/LKCl和8×10-3mol/LH2O2的底液中,皂素产生极谱催化波,其一阶导数波的峰电位在-1.05V(vs.SCE)处,峰电流与皂素浓度在1.0×10-8～8.0×10-8mol/L范围内有良好的线性关系,线性回归方程:i′P=7.322×108c+3.919(μA/s),相关系数r=0.9984,检出限为1.0×10-8mol/L;该波为不可逆吸附、平行催化波。建立了测定皂素的新分析方法,并测定了黄姜中皂素的含量。