Key Laboratory of Tibetan Medicine Research, Northwest Institute of Plateau Biology, Chinese Academy of Sciences, Xining, Qinghai, China.
University of Chinese Academy of Science, Beijing, China.
J Sep Sci. 2017 Oct;40(19):3808-3816. doi: 10.1002/jssc.201700675. Epub 2017 Aug 30.
An offline preparative two-dimensional reversed-phase liquid chromatography/hydrophilic interaction liquid chromatography coupled with hydrophilic interaction solid-phase extraction method was developed for the preparative isolation of flavonoid glycosides from a crude sample of Sphaerophysa salsula. First, the non-flavonoids were removed using an XAmide solid-phase extraction cartridge. Based on the separation results of three different chromatographic stationary phases, the first-dimensional preparation was performed on an XAqua C18 prep column, and 15 fractions were obtained from the 5.2 g target sample. Then, three representative fractions were selected for additional purification on an XAmide preparative column to further isolate the flavonoid glycosides. In all, eight flavonoid glycosides were isolated in purities over 97%. The results demonstrated that the two-dimensional liquid chromatography method used in this study was effective for the preparative separation of flavonoid glycosides from Sphaerophysa salsula. Additionally, this method showed great potential for the separation of flavonoid glycosides from other plant materials.
建立了离线制备二维反相液相色谱/亲水相互作用液相色谱-亲水相互作用固相萃取法，用于从沙拐枣粗提物中制备分离黄酮糖苷。首先，使用 XAmide 固相萃取小柱去除非黄酮类化合物。根据三种不同色谱固定相的分离结果，在 XAqua C18 制备柱上进行一维制备，从 5.2g 目标样品中得到 15 个馏分。然后，选择三个代表性馏分在 XAmide 制备柱上进行进一步纯化，以进一步分离黄酮糖苷。总共分离出 8 个纯度超过 97%的黄酮糖苷。结果表明，本研究中使用的二维液相色谱法对从沙拐枣中制备分离黄酮糖苷是有效的。此外，该方法在分离其他植物材料中的黄酮糖苷方面具有很大的潜力。
