Industrial Scale-Up of Countercurrent Chromatography

Sutherland, Ian; Booth, A. J.; Brown, Les; Kemp, Bruce E.; Kidwell, Huw; Games, David E.; Graham, A. S.; Guillon, G G; Hawes, David J.; Hayes, M.; Janaway, Lee; Lye, Gary J.; Massey, Peter R.; Preston, Caroline M.; Shering, P.; Shoulder, T; Strawson, C.; Wood, Philip

doi:10.1081/jlc-100104362

Cited by 26 publications

(8 citation statements)

References 9 publications

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“…For all columns, a linear decrease with an increase in flow rate was observed within the studied range. This is in line with similar studies from literature for both, CCC [5,18,33,[35][36][37][38][39][40] and CPC [14,16,20,22,24,38,41] of different column sizes and geometries within a certain flow rate range. However, it should be noted that this only applies up to a certain flow rate.…”

Section: Stationary Phase Retentionsupporting

confidence: 93%

Evaluation of Inter-Apparatus Separation Method Transferability in Countercurrent Chromatography and Centrifugal Partition Chromatography

Roehrer

Minceva

2019

Separations

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In the countercurrent chromatography and centrifugal partition chromatography, separation method transfer and scale-up is often described as an easy and straightforward procedure. Separation methods are usually developed on lab scale columns and subsequently transferred using linear scale-up factors to semi-preparative or preparative columns of the same column design. However, the separation methods described in the literature have been developed on various columns of different design and size. This is accompanied by differences in the separation behavior of the columns and therefore makes separation method transfer difficult. In the current study, the separation performances of different columns were evaluated and compared. Linear correlations of stationary phase retention and column efficiency as a function of flow rate were found to be applicable for the calculation of separation resolution in the typical operating range of each column. In this context, a two-point short-cut approach for a fast column characterization is recommended. This allows a quick prediction of the separation method transferability between columns, which saves experimental time and effort. In the current study, the transferability between five different columns from lab scale countercurrent chromatography (CCC) (18 mL) to semi-preparative centrifugal partition chromatography (CPCs) (250 mL) with different cell numbers and design is investigated.Separations 2019, 6, 36 2 of 16 often differ significantly in column design as well as size. Consequently, suitable operating parameters (e.g., flow rate, rotational speed) and separation performances (e.g., stationary phase retention, column efficiency) between the columns are also different. Therefore, efficient and systematic strategies are needed to quickly transfer separation methods between different apparatuses.In conventional liquid chromatography (LC), e.g., High-performance liquid chromatography (HPLC), clear rules exist on how to transfer batch separation methods between columns. Here, columns are of cylindrical shape and packed with a solid stationary phase. The design parameters are column diameter, length and stationary phase particle size. In general, sample load, i.e., the feed sample concentration and relative volumetric column loading, is kept constant and the same or a better number of theoretical stages is aimed for. To achieve these criteria when transferring a separation method, usually the particle size and the column length are kept the same, while the cross sectional area and the mobile phase flow rate are adjusted in order to guarantee the same mobile phase velocity in both columns [6]. In literature, this approach was studied also for applicability in CCC and CPC. The same mobile phase linear velocity was used in both columns when transferring the separation method between columns [7]. However, this is difficult, especially in CPC, since the cross-sectional area of the CPC cells is not constant and changes along the cells of different geometries. It was shown, that an av...

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Section: Stationary Phase Retentionsupporting

confidence: 93%

Evaluation of Inter-Apparatus Separation Method Transferability in Countercurrent Chromatography and Centrifugal Partition Chromatography

Roehrer

Minceva

2019

Separations

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“…Equation 25 is used to predict the retention of the stationary phase of all the solvent systems in Table 3 (literature data). The comparison of the predicted and literature data13, 14, 29–31 is shown in Figure 11.…”

Section: Resultsmentioning

confidence: 99%

Retention of the stationary phase for high‐speed countercurrent chromatography

Zhao

2007

AIChE Journal

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in Wiley InterScience (www.interscience.wiley.com).High-speed countercurrent chromatography (HSCCC) is an emerging technique for preparative purification of a wide variety of solutes. Retention of the stationary phase is a crucial variable which is used for the derivation of the column efficiency, peak resolution, and solute retention. A mathematical model was proposed to describe the influences of operation conditions (flow rate, rotation speed), physical properties (density difference, viscosity, and interfacial tension), and instrument parameters (tube diameter, revolution radius) on the retention of the stationary phase, by building on the flow behavior of the two phases in the coiled column, laminar flow or droplet flow. The model parameters, together with the critical value at which the transition between the laminar flow and droplet flow occurs, were determined by the analysis of experimental data of the retention of the stationary phase measured in this work. Furthermore, the proposed model was used to predict the literature data of retention of the stationary phase for seven HSCCC apparatuses including preparative, semi-preparative, and analytical types, with the coiled column material of PTFE and stainless steel, and for 16 two-phase systems with 151 data points. The agreement between the predicted and the literature data is quite good with the total absolute deviation (AAD%) of 2.96% and the maximum deviation of 12.8%.

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“…The HPCCC method was selected as a contemporary separation tool allowing to facilitate the transfer of the analytical conditions to a preparative, industrial scale. HPCCC is also characterized by the absence of a (conventional) stationary phase, which reduces the losses caused by the absorption of active compounds (Sutherland, 2007).…”

Section: Introductionmentioning

confidence: 99%