UMR CNRS 7312, Université de Reims Champagne-Ardenne, Bât. 18, Moulin de la Housse, BP 1039, 51687 Reims Cedex 2, France.
J Chromatogr A. 2012 Jul 20;1247:18-25. doi: 10.1016/j.chroma.2012.05.046. Epub 2012 May 17.
The aim of this article was to evaluate the influence of the column design of a hydrostatic support-free liquid-liquid chromatography device on the process efficiency when the strong ion-exchange (SIX) development mode is used. The purification of p-hydroxybenzylglucosinolate (sinalbin) from a crude aqueous extract of white mustard seeds (Sinapis alba L.) was achieved on two types of devices: a centrifugal partition chromatograph (CPC) and a centrifugal partition extractor (CPE). They differ in the number, volume and geometry of their partition cells. The SIX-CPE process was evaluated in terms of productivity and sinalbin purification capability as compared to previously optimized SIX-CPC protocols that were carried out on columns of 200 mL and 5700 mL inner volume, respectively. The objective was to determine whether the decrease in partition cell number, the increase in their volume and the use of a "twin cell" design would induce a significant increase in productivity by applying higher mobile phase flow rate while maintaining a constant separation quality. 4.6g of sinalbin (92% recovery) were isolated from 25 g of a crude white mustard seed extract, in only 32 min and with a purity of 94.7%, thus corresponding to a productivity of 28 g per hour and per liter of column volume (g/h/LV(c)). Therefore, the SIX-CPE process demonstrates promising industrial technology transfer perspectives for the large-scale isolation of ionized natural products.
本文旨在评估在采用强离子交换（SIX）开发模式时，无支撑静压液体-液体色谱装置的柱设计对工艺效率的影响。通过两种设备：离心分配色谱仪（CPC）和离心分配萃取器（CPE），从白芥子粗水提物中纯化对羟基苄基葡萄糖硫苷（西玛宾）。它们在分相单元的数量、体积和几何形状上有所不同。与之前在 200 mL 和 5700 mL 柱内体积的 CPC 柱上分别优化的 SIX-CPC 方案相比，评估了 SIX-CPE 工艺的生产力和西玛宾纯化能力。目的是确定减少分相单元数量、增加其体积以及采用“双单元”设计是否会通过应用更高的流动相流速而在保持恒定分离质量的同时显著提高生产力。从 25 g 白芥子粗提取物中分离出 4.6 g 西玛宾（回收率为 92%），仅用时 32 min，纯度达到 94.7%，因此，每小时每升柱体积（g/h/LV(c)）的生产力为 28 g。因此，SIX-CPE 工艺为大规模分离离子化天然产物的工业化技术转移提供了有前景的应用。
