Selection of operating parameters on the basis of hydrodynamics in centrifugal partition chromatography for the purification of nybomycin derivatives

Adelmann, S.; Baldhoff, Tobias; Koepcke, B.; Schembecker, Gerhard

doi:10.1016/j.chroma.2012.11.031

Cited by 32 publications

(25 citation statements)

References 23 publications

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“…However, at a certain flow rate, the stationary phase retention drastically decreased, which was observable for the selected ATPS between 9 and 11 mL min −1 . This behavior could be noticed for several other ATPS and some aqueous-organic systems [24,25]. It is known from earlier studies, that the stationary phase retention may be slightly lower using the separation rotor (20 discs, 1320 chambers) in contrast to the single disc rotor (66 chambers) used for the hydrodynamic measurements.…”

Section: Selection Of Operating Parametersmentioning

confidence: 73%

“…The rotor is built up of 20 discs, containing 1320 chambers and 200 mL internal volume in total. The peripheral setup is as described in further studies [24,25]: solvent supply is done by two SD-1 pumps (Agilent, Santa Clara (CA), USA), one for each phase. Six-port valves (Knauer, Berlin, Germany; type: Smartline S6, 3-channel) were used to select the phase to be pumped to the CPC and for sample injection.…”

Section: Cpc Experimentsmentioning

confidence: 99%

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Separation of active laccases from Pleurotus sapidus culture supernatant using aqueous two-phase systems in centrifugal partition chromatography

Schwienheer

Zeiner

Merz

2015

Journal of Chromatography B

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Section: Selection Of Operating Parametersmentioning

confidence: 73%

Section: Cpc Experimentsmentioning

confidence: 99%

Separation of active laccases from Pleurotus sapidus culture supernatant using aqueous two-phase systems in centrifugal partition chromatography

Schwienheer

Zeiner

Merz

2015

Journal of Chromatography B

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“…The columns differ in type, size and design, but also in the typical operating range in terms of relative centrifugal acceleration (g-field) and mobile phase flow rate. Hence, the column performance is different in every single column as a result of differences in flow pattern, mass transfer area and solute residence time distribution [16,[19][20][21][22]26,27]. The different column characteristics can be described by a different stationary phase retention, column efficiency and peak resolution.…”

Section: Approach Of Column Characterization-based Separation Methods mentioning

confidence: 99%

“…Hence, this approach can only be directly applied, if a higher separation resolution occurs on the column where the method is intended to be transferred.According to literature, columns of same size but different design or cell geometries behave differently as a function of operating conditions such as flow rate and rotational speed (g-field) [14][15][16][17][18]. Differences in stationary phase retention and column efficiency have a clear influence on the separation resolution and process performances, including product purity, recovery, achievable productivity, and solvent consumption [16,[19][20][21][22][23][24]. Hence, a reliable and easy strategy for the separation method transfer between columns independent of their size and type is needed that considers the separation performances of different column designs.…”

mentioning

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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“…Therefore, adsorption effects of the stationary phase material, artifact formation, tailing of solute peaks, and contamination can be eliminated . HSCCC and HPCPC are hydrodynamic and hydrostatic operations, respectively . Owing to the differences in the underlying principles of HSCCC and HPCPC, the compounds separated by HSCCC and HPCPC using the same two‐phase solvent system are usually different.…”

Section: Introductionmentioning

confidence: 99%

Extraction and separation of lactate dehydrogenase inhibitors from Poria cocos (Schw.) Wolf based on a hyphenated technique and in vitro methods

Zhang

et al. 2017

J of Separation Science

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Stroke is one of the most common diseases worldwide. Lactate dehydrogenase inhibitors are widely used in the treatment of ischemic stroke, with natural products considered a promising source of lactate dehydrogenase inhibitors. In this study, ultrafiltration liquid chromatography coupled with mass spectrometry was used for the screening and identification of lactate dehydrogenase inhibitors from Poria cocos. Five lactate dehydrogenase inhibitors were selected: dehydropachymic acid, pachymic acid, dehydrotrametenolic acid, trametenolic acid, and eburicoic acid. The inhibitors were extracted and isolated with purities of 96.75, 98.15, 97.25, 95.46, and 94.88%, respectively, by using a new "hyphenated" strategy of microwave-assisted extraction coupled with counter-current chromatography and centrifugal partition chromatography by a two-phase solvent system of n-hexane/ethyl acetate/ethanol/water at the volume ratio 0.965:1.000:0.936:0.826 v/v/v/v. The bioactivity of the isolated compounds was assessed using the 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide assay in PC12 cells. The results also showed that the hyphenated technique of microwave-assisted extraction coupled with counter-current chromatography and centrifugal partition chromatography was an efficient method for the continuous extraction and online isolation of chemical constituents from medicinal herbs. Furthermore, the research route based on the activity screening, extraction, separation, and activity verification of the compounds offered advantages of efficiency, orientation, and objectivity.

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Selection of operating parameters on the basis of hydrodynamics in centrifugal partition chromatography for the purification of nybomycin derivatives

Cited by 32 publications

References 23 publications

Separation of active laccases from Pleurotus sapidus culture supernatant using aqueous two-phase systems in centrifugal partition chromatography

Separation of active laccases from Pleurotus sapidus culture supernatant using aqueous two-phase systems in centrifugal partition chromatography

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

Extraction and separation of lactate dehydrogenase inhibitors from Poria cocos (Schw.) Wolf based on a hyphenated technique and in vitro methods

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