Continuous fractionation of multicomponent mixtures with sequential centrifugal partition chromatography

Goll, Johannes; Minceva, Mirjana

doi:10.1002/aic.15529

Cited by 24 publications

(9 citation statements)

References 17 publications

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“…In this context, individual requirements such as purity, yield, productivity, and solvent consumption can be assessed. For a more comprehensive and reliable model-based optimization of the separation performance, a more extensive characterization of the column like in Section 3.2 with additional pulse injections could be recommended especially for the optimization and fine tuning of operating conditions at preparative or industrial scale [46,47]. Finally, it could be shown that transferability between columns can be determined by performing a two-point short-cut characterization.…”

Section: Short-cut Approach For Evaluation Of Separation Methods Transmentioning

confidence: 99%

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: Short-cut Approach For Evaluation Of Separation Methods Transmentioning

confidence: 99%

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

Roehrer

Minceva

2019

Separations

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“…All in all, the redosing of the stationary phase as a newly developed mode of operation offers some benefits compared to different approaches, addressing the loss of the stationary phase over time. Sequential Centrifugal Chromatography or Continuous Centrifugal Extraction both circumvent the drawbacks in separation efficiency caused by bleeding but require high technical effort for implementation as well as complex operation [22,30,[38][39][40].…”

Section: Reference Experiments Without Redosingmentioning

confidence: 99%

Optimizing Chromatographic Separation with Redosing: Effects on Separation Efficiency of a Model System in Centrifugal Partition Chromatography

Buthmann,

Hohlmann,

Neuwald

et al. 2024

Separations

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This study investigates and optimizes chromatographic separation in a Centrifugal Partition Chromatograph. Therefore, a model system is separated in a single-disc rotor. The occurring loss of the stationary phase lowers the separation efficiency over time. We introduced a new mode of operation, called the redosing of the stationary phase, to counteract this hydrodynamic phenomenon. Experiments with redosing at an optimized operating point demonstrate almost constant separation performance over 12 h, reducing solvent consumption by 45% and increasing chromatographic resolution by 37%. The improvement in retention by 69% contributes to this enhancement. Accordingly, reference experiments without redosing were conducted as a benchmark, highlighting the automated mode’s benefits, as mentioned.

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“…In recent years, researchers have studied the retention behavior of chromatography extensively, and related mathematical models have been established in the CCC [18–21]. In view of the huge potential application prospects of this method in separation, we referred to Berthod's research [22] and established a model of the elution‐extrusion method for continuous sample feed and separation with CCC in this work.…”

Section: Introductionmentioning

confidence: 99%

“…In recent years, researchers have studied the retention behavior of chromatography extensively, and related mathematical models have been established in the CCC [18][19][20][21].…”

Section: Introductionmentioning

confidence: 99%

A model for continuous sample feed and separation with counter‐current chromatography based on elution‐extrusion mode and its application

Sun

Huang

Pei

et al. 2022

J of Separation Science

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A novel and meaningful theoretical model was established with counter-current chromatography based on the elution-extrusion mode for efficient continuous separation. For the experimental verification of the theory, the separation of the binary mixture luteolin/baicalein was studied. The velocity model and volume model of the chromatographic separation behavior of the target compounds in the separation process were given by theoretical analysis. The results showed that this method had obvious advantages in the separation of binary mixtures. In addition, the established model was used to predict and isolate oleuropein from olive leaves. A two-phase solvent system of n-butanol/ethyl acetate/methanol/water (1:19:1:19, v/v/v/v) was chosen for the continuous separation of oleuropein. After optimizing the conditions in this way, a large amount of sample loading was achieved; the volume of injections can reach 48 ml, approximately 35.29% of the volume of the counter-current chromatography column, and oleuropein with a purity of 86.42% was obtained within 80 min. The model provided technical support for the prediction of chromatographic behavior and operating parameters during continuous separation and preparation of counter-current chromatography. It has great application prospects and significance in separation preparation, especially in large-scale industrial preparation.

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Continuous fractionation of multicomponent mixtures with sequential centrifugal partition chromatography

Cited by 24 publications

References 17 publications

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

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

Optimizing Chromatographic Separation with Redosing: Effects on Separation Efficiency of a Model System in Centrifugal Partition Chromatography

A model for continuous sample feed and separation with counter‐current chromatography based on elution‐extrusion mode and its application

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