Microdetermination of diosgenin from fenugreek (Trigonella foenum-graecum) seeds.
Microdetermination of diosgenin from fenugreek (Trigonella foenum-graecum) seeds.
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DOI：
10.1021/jf000467t
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发表时间：
2000-10
影响因子：
6.1
通讯作者：
Wesley G. Taylor;James L. Elder;P. Chang;Ken W. Richards
中科院分区：
文献类型：
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作者：
Wesley G. Taylor;James L. Elder;P. Chang;Ken W. Richards
通过毛细管气相色谱分析 100 mg 种子材料样品中的薯蓣皂苷元 [(25R)-spirost-5-en-3-ol] 和异构螺甾二烯伪影，研究了琥珀胡芦巴甾体糖苷的硫酸水解。用 80% 乙醇提取后，当在含有 60-80% 2-丙醇的水中以 1 摩尔 (M) 浓度制备的硫酸中进行水解时，薯蓣皂苷元的回收率最高。与之前使用盐酸水溶液的方法相比，所选择的在 70% 2-丙醇中使用硫酸在 100 ℃ 水解 2 小时的条件减少了二烯的形成，但并没有完全消除这些伪影。在硫酸水解之前用各种醇/水混合物提取甾体皂苷得到类似的薯蓣皂苷元回收率。将定量方法应用于 Amber、Quatro 和 ZT-5 葫芦巴的实验样品，使用 10 mg 粉碎种子子样品（用石油醚脱脂并在 60 摄氏度下干燥），得出薯蓣皂苷元含量分别为 0.55、0.42 和 0.75%。加拿大胡芦巴育种品系 ZT-5 的水解种子提取物中异菝葜皂苷元和菝葜皂苷元的含量非常低。
Sulfuric acid hydrolysis of steroidal glycosides of Amber fenugreek was studied by capillary gas chromatographic analysis of diosgenin [(25R)-spirost-5-en-3-ol] and isomeric spirostadiene artifacts from 100 mg samples of seed material. Following extraction with 80% ethanol, highest recoveries of diosgenin occurred when hydrolyses were conducted in sulfuric acid, prepared at 1 molar (M) concentration in water containing 60-80% 2-propanol. Compared to a previous method with aqueous hydrochloric acid, the selected conditions of hydrolysis at 100 degrees C for 2 h with sulfuric acid in 70% 2-propanol reduced diene formation but did not completely eliminate these artifacts. Extraction of steroidal saponins with various alcohol/water mixtures prior to sulfuric acid hydrolysis gave similar recoveries of diosgenin. Application of the quantitative method to experimental samples of Amber, Quatro, and ZT-5 fenugreek, using 10 mg subsamples of crushed seed that had been defatted with petroleum ether and dried at 60 degrees C, gave diosgenin levels of 0.55, 0.42, and 0.75%, respectively. Levels of smilagenin and sarsasapogenin were very low in hydrolyzed seed extracts from ZT-5, a Canadian breeder line of fenugreek.