Exploratory Purification of Compounds from Aqueous Extracts of Pinus massoniana Lamb. by Two-Dimensional Preparative Liquid Chromatography

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• 作者：Fan Yang ; Manxi Zhao ; Xiuli Zhang ; Qiang Li ; Yuansheng Xiao ; Xiao Ke…
• 关键词：Two ; dimensional preparative LC ; Orthogonal ; RP × HILIC ; RP × RP ; Separation strategy
• 刊名：Chromatographia
• 出版年：2017
• 出版时间：January 2017
• 年：2017
• 卷：80
• 期：1
• 页码：39-43
• 全文大小：
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chromatography; Proteomics; Pharmacy; Laboratory Medicine;
• 出版者：Springer Berlin Heidelberg
• ISSN：1612-1112
• 卷排序：80

文摘

An off-line orthogonal two-dimensional preparative liquid chromatography method was developed for isolation of high-purity compounds from aqueous extracts of Pinus massoniana Lamb., which has efficient therapeutic properties in recipes of traditional Chinese medicines. A polar-enhanced reversed-phase (RP) column, XAqua C18 was selected for the first-dimensional separation. A HILIC column and a hydrophobic RP column were both explored in the second dimension. The preparation results indicated hydrophilic RP × HILIC mode would provide better separation efficiency for polar complexes, i.e., the second-dimensional separation was finished in less than 30 min and high-purity compounds were obtained. In this work, 16 fractions were collected efficiently in the first dimension with a recovery up to 96%, and six compounds with high purity and enough quantity were identified by NMR and high resolution mass spectrometry, including epicatechin, betuloside, taxifolin-3-O-xyloside, cedrusin-4-O-glucoside, massonianoside C and massonianoside D, and five are glycosides, including flavonoid glycosides, lignanoid glycosides and an arylbutanoid glycoside. Betuloside was first reported in the preparation of Pinus massoniana Lamb. This work demonstrated a flexible strategy of compromise in between time and resolution for selecting solvent and column to enhance preparative efficiency of polar complex systems.