逆流色谱(CCC)已被广泛用作从植物提取物和发酵液中纯化天然产物的制备分离方法。传统上,CCC的吞吐量优化集中在样品浓度和样品体积上。在本文中,样品注射被认为是由三个变量组成:注射流速,后注射流速和样品溶剂。使用从厚朴树皮提取物中纯化和厚朴酚作为案例研究,研究了这些参数的影响,目的是获得超过99%纯度的这种潜在抗癌药物,以提交给中国FDA。建立了一种注射方法,使和厚朴酚的通量增加了46.5%(从3.05g/h增加到4.47g/h),每克和厚朴酚流动相和固定相的溶剂消耗量分别降低了40.0%(从0.68L/g降至0.41L/g)和48.4%(从0.40L/g降至0.21L/g)。这些结果显示了在优化给定的CCC分离时理解整个注入过程的重要性。
Counter-current chromatography (CCC) has been widely used as a preparative separation method to purify natural products from plant extracts and fermentation broths. Traditionally, throughput optimization in CCC has focused on sample concentration and sample volume. In this paper sample injection was considered as consisting of three variables: injection flow rate, post-injection flow rate and sample solvent. The effects of these parameters were studied using a
honokiol purification from a Magnolia officinalis bark extract as a
case study aiming to achieve the highest throughput/yield ratio for greater than 99% purity of this potential anti-cancer drug obtained for submission to the Chinese FDA. An injection method was established that increased the throughput of
honokiol by 46.5% (from 3.05g/h to 4.47g/h), and decreased the solvent consumption of mobile phase and stationary phase per gram of
honokiol by 40.0% (from 0.68L/g to 0.41L/g) and 48.4% (from 0.40L/g to 0.21L/g) respectively. These results show the importance of understanding the whole injection process when optimizing a given CCC separation.