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采用高速逆流色谱结合制备型高效液相色谱法从五味子茎中纯化六种木脂素。

Purification of six lignans from the stems of Schisandra chinensis by using high-speed counter-current chromatography combined with preparative high-performance liquid chromatography.

作者信息

Zhu Lijie, Li Bin, Liu Xiuying, Huang Guohui, Meng Xianjun

机构信息

College of Food, Shenyang Agricultural University, Shenyang 110866, People's Republic of China; College of Chemistry, Chemical Engineering and Food Safety, Food Science Research Institute, Bohai University, Jinzhou 121013, People's Republic of China.

College of Food, Shenyang Agricultural University, Shenyang 110866, People's Republic of China.

出版信息

Food Chem. 2015 Nov 1;186:146-52. doi: 10.1016/j.foodchem.2014.09.008. Epub 2014 Sep 10.

Abstract

A method for the preparative purification of lignans from Schisandra chinensis was established using a combination of high-speed counter-current chromatography (HSCCC) and preparative high-performance liquid chromatography (HPLC). The crude extracts obtained from S. chinensis by using 70% ethanol were separated on a macroporous resin column and then eluted with a graded ethanol series. A two-phase solvent system consisting of n-hexane-ethyl acetate-methanol-water (1:1:1:1, v/v) was used for HSCCC, and a mobile phase of acetonitrile-water (50:50, v/v) was used for preparative HPLC. The results obtained using HSCCC were compared with those obtained using preparative HPLC, and their advantages were further integrated to improve the separation efficiency. Six known lignans were identified by electrospray ionisation mass spectrometry and (1)H nuclear magnetic resonance (NMR) and (13)C NMR analyses; the purities of all the compounds were more than 91%.

摘要

建立了一种结合高速逆流色谱(HSCCC)和制备型高效液相色谱(HPLC)从五味子中制备纯化木脂素的方法。用70%乙醇从五味子中获得的粗提物在大孔树脂柱上分离,然后用梯度乙醇系列洗脱。HSCCC使用正己烷 - 乙酸乙酯 - 甲醇 - 水(1:1:1:1,v/v)组成的两相溶剂系统,制备型HPLC使用乙腈 - 水(50:50,v/v)的流动相。将HSCCC获得的结果与制备型HPLC获得的结果进行比较,并进一步整合它们的优点以提高分离效率。通过电喷雾电离质谱、¹H核磁共振(NMR)和¹³C NMR分析鉴定了六种已知木脂素;所有化合物的纯度均超过91%。

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