当前位置: X-MOL 学术J. Sep. Sci. › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Purification of triterpenoid saponins and 25R/25S‐inokosterone from Achyranthes bidentata Bl. by high‐speed countercurrent chromatography coupled silver nitrate coordination
Journal of Separation Science ( IF 2.8 ) Pub Date : 2024-04-12 , DOI: 10.1002/jssc.202300901
Tong Niu 1, 2 , Jinqian Yu 1, 2 , Zhenqiang Wang 3 , Chuangchuang Wang 3 , Yingjian Guo 3 , Jian Li 4 , Xiao Wang 1, 2, 3
Affiliation  

An effective method by high‐speed countercurrent chromatography coordinated with silver nitrate for the preparative separation of sterones and triterpenoid saponins from Achyranthes bidentata Blume was developed. Methyl tert‐butyl ether/n‐butanol/acetonitrile/water (4:2:3:8, v/v/v/v) was selected for 20‐hydroxyecdysone (compound 1), chikusetsusaponin IVa methyl ester (compound 4), 2′‐glycan‐11‐keto‐pigmented saponin V (compound 5), as well as a pair of isomers of 25S‐inokosterone (compound 2) and 25R‐inokosterone (compound 3), which were further purified by silver nitrate coordinated high‐speed countercurrent chromatography. What is more, dichloromethane/methanol/isopropanol/water (6:6:1:4, v/v/v/v) was applied for calenduloside E (compound 6), 3β‐[(O‐βd‐glucuronopyranosyl)‐oxy]‐oleana‐11,13‐dien‐28‐oic acid (compound 7), zingibroside R1 (compound 8) and chikusetsusaponin IVa (compound 9). Adding Ag+ to the solvent system resulted in unique selectivity for 25R/25S isomers of inokosterone, which increased the complexing capability and stability of Ag+ coordinated 25S‐inokosterone, as well as the α value between them. These results were further confirmed by the computational calculation of geometry optimization and frontier molecular orbitals assay. Comprehensive mass spectrometry and nuclear magnetic resonance analysis demonstrated the structures of the obtained compounds.

中文翻译:


牛膝中三萜皂苷和25R/25S-肌醇酮的纯化。高速逆流色谱耦合硝酸银配位



高速逆流色谱联用硝酸银制备分离中药甾酮和三萜皂苷的有效方法牛膝布鲁姆被开发出来。 20-羟基蜕皮激素(化合物1)、竹节皂苷IVa甲酯(化合物4)选择甲基叔丁基醚/正丁醇/乙腈/水(4:2:3:8,v/v/v/v), 2′-聚糖-11-酮色素皂苷 V(化合物 5),以及一对 25 的异构体S ‐肌醇酮(化合物 2)和 25右‐肌醇酮(化合物 3),通过硝酸银配合的高速逆流色谱进一步纯化。此外,将二氯甲烷/甲醇/异丙醇/水(6:6:1:4,v/v/v/v)应用于金盏花苷E(化合物6),3 β ‐[(O‐ β ‐ d -吡喃葡萄糖醛酸基)-氧基]-齐墩果-11,13-二烯-28-油酸(化合物7)、姜苷R1(化合物8)和竹节皂苷IVa(化合物9)。添加银+该溶剂系统对 25 种化合物具有独特的选择性右/25 S肌酮酮的异构体,增加了Ag的络合能力和稳定性+协调 25 S ‐肌醇酮,以及α他们之间的价值。这些结果通过几何优化和前沿分子轨道分析的计算进一步得到证实。综合质谱和核磁共振分析证明了所得化合物的结构。
更新日期:2024-04-12
down
wechat
bug