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高速逆流色谱不同旋转模式从姜粗提取物中直接大规模制备低极性姜酚类化合物的有效策略。

An efficient strategy for large-scale preparation of low polarity gingerols directly from ginger crude extract by high-speed countercurrent chromatography with different rotation mode.

机构信息

Key Laboratory of Comprehensive and Highly Efficient Utilization of Salt Lake Resources, Qinghai Institute of Salt Lakes, Chinese Academy of Sciences, Xining, P. R. China.

College of Pharmacy, Jinan University, Guangzhou, P. R. China.

出版信息

J Sep Sci. 2023 Oct;46(19):e2300320. doi: 10.1002/jssc.202300320. Epub 2023 Aug 4.

Abstract

This study presents an efficient strategy for large-scale preparation of low polarity gingerols directly from ginger crude extract by high-speed countercurrent chromatography with different rotation mode. The ultrasonic-assisted extraction conditions were optimized by response surface methodology and the results showed the major low polarity gingerols could be well enriched under the optimized extraction conditions. Then the crude extract without any pretreatment was directly separated by high-speed countercurrent chromatography with different rotation mode using n-hexane/ethyl acetate/methanol/water (6:4:6:4, v/v/v/v) as the solvent system. In about 400 min, five major gingerols including 150 mg of [6]-gingerol, 50 mg of [8]-gingerol, 20 mg of [6]-shogaol, 43 mg of [6]-dehydrogingerdione, and 40 mg of [10]-gingerol were obtained from 1.2 g of crude extract in a single run with repeated injection. Their structures were identified by H-NMR spectroscopy.

摘要

本研究提出了一种从姜粗提取物中直接通过高速逆流色谱以不同旋转模式大规模制备低极性姜烯醇的有效策略。通过响应面法优化了超声辅助提取条件,结果表明主要的低极性姜烯醇可以在优化的提取条件下得到很好的富集。然后,在没有任何预处理的情况下,使用正己烷/乙酸乙酯/甲醇/水(6:4:6:4,v/v/v/v)作为溶剂系统,通过不同旋转模式的高速逆流色谱直接分离粗提取物。在大约 400 分钟内,从 1.2 g 粗提取物中单次运行和重复进样中,得到了 150 mg [6]-姜烯醇、50 mg [8]-姜烯醇、20 mg [6]-姜辣素、43 mg [6]-脱氢姜二酮和 40 mg [10]-姜烯醇等五种主要的姜烯醇,其结构通过 H-NMR 光谱鉴定。

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