Low-Speed Rotary Countercurrent Chromatography Using a Convoluted Multilayer Helical Tube for Industrial Separation

Abstract

An industrial-scale countercurrent chromatographic system was developed using a slowly rotating helical device which can be automated and left unattended during the operation. It uses a multilayer coiled column consisting of long convoluted Teflon tubing of 0.85 cm i.d., which provides sufficient retention of the stationary phase under a relatively high flow rate. The column is mounted on a seal-less continuous-flow rotary device which eliminates various complications such as leakage and clogging as often caused by the use of a conventional rotary seal. Using a multilayer coiled column with a 10-L capacity, 150 g of crude tea extract was successfully purified, yielding 40 g of epigallocatechin gallate of over 92.7% purity at a recovery rate of 82.6%. The present system can be scaled up for a kilogram-scale separation.

Preparative Separation of Phenolic Constituents in the Fruits of Luffa cylindrica (L.) Roem using Slow Rotary Countercurrent Chromatography

“…Slow rotary countercurrent chromatography (SRCCC) [3,4] employs a nonplanetary low rotation column (20 -150 rpm), which permits the system to be left unattended during the long time separation. The advantage of SRCCC is that the separation can be scaled up to an industrial level.…”

Isolation of 6,9,12,15-Hexadecatetraenoic Fatty Acid (16:4n-1) Methyl Ester from Transesterified Fish Oil by HSCCC

“…For instance, HSCCC in the first step could be linked with silver ion HPLC for the separation of cis-/trans-isomers [32]. Although the sample capacity of HSCCC was high, an upscale of the method is one of the major current goals [16,33]. First steps were made by introducing slow rotating CCC which may be used for the separation of up to kilogram amounts [16].…”

Tubing modifications for countercurrent chromatography (CCC): Stationary phase retention and separation efficiency

“…Preferentially, a solvent system should possess a low mean viscosity η M , a high interfacial tension σ and density difference Δρ to achieve high S f [32,33]. Taking into account the different behavior of solvent systems in CCC [26], three different and routinely used two-phase solvent systems were selected (one hydrophobic, one intermediate and one hydrophilic). The non-aqueous hydrophobic system (HACN) was made of n-hexane/acetonitrile (1:1, v/v).…”

“…More recently, a similar approach was followed for the improvement of the spiral tube support assembly for CCC (specially developed for the separation of extremely polar compounds with polar solvent systems) by changing the shape of the tubing through compressions perpendicularly along the length of the tubing [21][22][23]. Convoluted tubing was introduced to improve the retention of the stationary phase during the scale-up of slow-rotary CCC by Du and Winterhalter and it has been successfully applied in the purification of natural products [24][25][26][27]. In addition, Yang et al investigated novel geometric designs of tubing in the rarely used and noncommercialized toroidal zigzag CCC apparatus and observed improved peak resolution [28,29].…”