Department of Chemistry, Changchun Normal University, Changchun 130032, China; Guelph Food Research Centre, Agriculture and Agri-Food Canada, 93 Stone Road West, Guelph, Ontario, Canada N1G 5C9.
Guelph Food Research Centre, Agriculture and Agri-Food Canada, 93 Stone Road West, Guelph, Ontario, Canada N1G 5C9.
Food Chem. 2008 May 15;108(2):702-10. doi: 10.1016/j.foodchem.2007.10.082. Epub 2007 Nov 6.
Five phenylethanoid glycosides (PhGs), echinacoside, cistanoside A, acteoside, isoacteoside and 2'-acetylacteoside, were isolated and purified from Cistanche deserticola for the first time by high-speed counter-current chromatography (HSCCC) using two biphasic systems, one consisting of ethyl acetate-ethanol-water (5:0.5:4.5, v/v/v) and another of ethyl acetate-n-butanol-ethanol-water (0.5:0.5:0.1:1, v/v/v/v). A total of 28.5mg of echinacoside, 18.4mg of cistanoside A, 14.6mg of acteoside, 30.1mg of isoacteoside and 25.2mg of 2'-acetylacteoside were purified from 1412mg of the n-butanol extract of C. deserticola, each at over 92.5% purity as determined by HPLC. The structures were identified by their retention time, UV, LC-ESI-MS in the negative ion mode, and confirmed by NMR experiments. The characteristic LC-ESI-MS(n) fragmentation pattern of the five compounds is discussed, and found to be a very specific and useful tool for the structural identification of PhGs from this important medicinal plant.
首次采用高速逆流色谱（HSCCC）法，利用两种双相体系（乙酸乙酯-乙醇-水（5:0.5:4.5，v/v/v）和乙酸乙酯-正丁醇-乙醇-水（0.5:0.5:0.1:1，v/v/v/v）），从肉苁蓉中分离和纯化了 5 种苯乙醇苷类化合物（PhGs），分别为毛蕊花糖苷、肉苁蓉苷 A、麦角甾苷、异麦角甾苷和 2′-乙酰麦角甾苷。从 1412mg 的肉苁蓉正丁醇提取物中，共分离纯化出 28.5mg 的毛蕊花糖苷、18.4mg 的肉苁蓉苷 A、14.6mg 的麦角甾苷、30.1mg 的异麦角甾苷和 25.2mg 的 2′-乙酰麦角甾苷，经 HPLC 测定纯度均超过 92.5%。通过保留时间、紫外、LC-ESI-MS 在负离子模式下以及 NMR 实验确定了它们的结构。讨论了这 5 种化合物的特征 LC-ESI-MS(n) 裂解模式，发现它是鉴定该重要药用植物中 PhGs 结构的非常特异和有用的工具。
