Rapid purification and scale-up of honokiol and magnolol using high-capacity high-speed counter-current chromatography

Rapid purification and scale-up of honokiol and magnolol using high-capacity high-speed counter-current chromatography
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DOI:
10.1016/j.chroma.2006.09.098
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发表时间:
2007-02-23
影响因子:
4.1
通讯作者:
Sutherland, Ian A.
Sutherland, Ian A.
中科院分区:
化学2区
文献类型:
--
作者:
Chen, Lijuan;Zhang, Qiang;Sutherland, Ian A.

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本文采用高容量高速逆流色谱法(high-capacity HSCCC)对厚朴中主要活性成分厚朴酚和厚朴酚进行了分离纯化。采用分析型大容量HSCCC系统地研究了溶剂选择工艺、样品上样量和流速的优化。在分析规模下快速获得的优化参数用于在MAXI-DE离心机中使用中试规模大容量HSCCC进行1000倍放大的制备运行。成功地分离了43 g粗样品,并用高效液相色谱法对其进行了分析。该大规模单步制备工艺在20 min内分别获得了16.9 g和19.4 g的厚朴酚和厚朴酚,纯度分别为98.6%和99.9%。这是首次使用高效逆流色谱法纯化多种谷物级生物活性化合物,纯化时间小于1b,且最终产物浓度如此之高(厚朴酚10.8 g/l,厚朴酚7.0 g/l)。(c) 2007 Elsevier B.V.版权所有
In this paper, a rapid separation approach has been developed using high-capacity high-speed counter-current chromatography (high-capacity HSCCC) to isolate and purify honokiol and magnolol, which are the main bioactive constituents from Houpu. The optimization of the solvent selection process, sample loading volume and flow rate is systematically studied using analytical high-capacity HSCCC. The optimized parameters obtained rapidly at analytical scale were used for a 1000 x scale-up preparative run using pilot scale high-capacity HSCCC in a MAXI-DE centrifuge. A crude sample of 43 g was successfully separated and the fractions were analysed by high-performance liquid chromatography (HPLC). This large scale preparative single step run yielded 16.9 and 19.4 g of honokiol and magnolol with purities of 98.6 and 99.9%, in only 20 min. This is the first time that high-performance counter-current chromatography has been used to purify multiple grain grade bioactive compounds in less than 1b and at such high concentrations of final products (10.8 g/l for magnolol and 7.0 g/l for honokiol). (c) 2007 Elsevier B.V. All rights reserved.