High throughput HPLC/MS purification in support of drug discovery

Goetzinger, Wolfgang; Zhang, X.; Bi, Grace; Towle, Marc H.; Cherrak, Djamel E; Kyranos, James N.

doi:10.1016/j.ijms.2004.02.024

Cited by 34 publications

(22 citation statements)

References 22 publications

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“…Since the first commercial instrument became available in the 1990s [5], supercritical fluid chromatography (SFC) has become an increasingly important purification tool to obtain enantiomerically pure compounds, especially in the early drug discovery stage due to its high speed and separation efficiency compared to LC [6][7][8][9][10][11][12][13]. In addition, the reduction of solvent to be removed from the purified sample, as well as reduced solvent waste after chromatographic separation, makes SFC extremely attractive to discovery-purification laboratories in the pharmaceutical industry [14,15].…”

Section: Introductionmentioning

confidence: 99%

Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatographic mobile phases

Gahm

Tan

Liu

et al. 2008

Journal of Pharmaceutical and Biomedical Analysis

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Section: Introductionmentioning

confidence: 99%

Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatographic mobile phases

Gahm

Tan

Liu

et al. 2008

Journal of Pharmaceutical and Biomedical Analysis

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“…In our approach, the waste line is connected to a second UV detector and the eluant is monitored prior to discharging it in the waste system. The overall efficiency of the collection process can be monitored for each sample in real time by comparing the trace of the UV immediately after the HPLC column with the chromatographic trace from the waste UV (Goetzinger et al, 2004).…”

Section: Purification Of Ncesmentioning

confidence: 99%

Mass spectrometry analysis of new chemical entities for pharmaceutical discovery

Fang

Miao

Tidswell

et al. 2007

Mass Spectrometry Reviews

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In this Section, we review the applications of mass spectrometry for the analysis and purification of new chemical entities (NCEs) for pharmaceutical discovery. Since the speed of synthesis of NCEs has dramatically increased over the last few years, new high throughput analytical techniques have been developed to keep pace with the synthetic developments. In this Section, we review both novel, as well as modifications of commonly used mass spectrometry techniques that have helped increase the speed of the analytical process. Part of the review is devoted to the purification of NCEs, which has undergone significant development in recent years, and the close integral association between characterization and purification to drive high throughput operations. At the end of the Section, we review potential future directions based on promising and exciting new developments.

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“…CCC is a support-free liquid-liquid partition method which eliminates irreversible adsorption of samples onto the solid support, providing a wider range of selection of two-phase solvent systems and yielding high purity and recovery [11–15]. Being an amplification mode of analytic HPLC, preparative RP-HPLC has become a powerful tool due to its shorter isolation time, excellent efficiency and high recovery [16–19]. Because of these remarkable characteristics, these two chromatographic methods play an important role in current biochemical researches.…”

Section: Introductionmentioning

confidence: 99%

Comparative Studies on Performance of CCC and Preparative RP-HPLC in Separation and Purification of Steroid Saponins from Dioscorea Zingiberensis C.H.Wright

Zhang

Liang

Zhang

et al. 2015

J Steroids Hormon Sci

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Steroid saponins from Dioscorea zingiberensis C.H.Wright were separated for the first time using two chromatographic methods for comparison: counter-current chromatography (CCC) coupled with evaporative light scattering detector (ELSD) and preparative reversed phase high-performance liquid chromatography (RP-HPLC) with an ultraviolet detector. Ethyl acetate-n-butanol-methanol-water (4:1:2:4, v/v) was chosen as the two-phase solvent system for CCC, while the acetonitrile-water (25:75 for the first step and15:85 for the second step, v/v) was used as the mobile phase in the preparative RP-HPLC. The following five steroid saponins were purified by theses two chromatographic methods, in one-step operation by CCC and by two-step operation in preparative RP-HPLC: 1) 26-O-β-D- glucopyranosyl-(25R)-furost-5-en-3β, 22ζ, 26-triol-3-O-[β-D-glucopyranosyl-(1→3)-β-D-glucopyranosyl-(1→4)-α-L-rhamnopyranosyl-(1→2)]-β-D-glucopyranoside (compound A), 2) 26-O-β-D-glucopyranosyl-(25R)-furost-5-en-3β, 22ζ, 4) 26-triol-3-O-[β-D-glucopyranosyl-(1→3)-α-L-rhamnopyranosyl-(1→2)]-β-D-glucopyranoside (compound B), 3) 26-O-β-D-glucopyranosyl-(25R)-furost-5-en-3β, 22ζ, 26-triol-3-O-[α-L-rhamnopyranosyl-(1→4)]-β-D-glucopyranoside (compound C), 4) 26-O-β-D-glucopyranosyl-(25R)-furost-5, 20(22)-diene-3β, 26-diol-3-O-{α-L-rhamnopyranosyl-(1→4)-[β-D-glucopyranosyl-(1→3)-β-D-glucopyranosyl-(1→2)]}-β-D-glucopyranoside (compound D) and 5) 26-O-β-D-glucopyranosyl-(25R)-furost-5, 20(22)-diene-3β, 26-diol-3-O-[β-D-glucopyranosyl-(1→4)-α-L-rhamnopyranosy-(1→2)]-β-D-glucopyranoside (compound E). The purities of these five steroid saponins separated by both methods were over 95%, and structural identification of these compounds was performed by ESI-MS, and 13C NMR. Comparison of these two established approaches revealed that CCC required a longer separation time but with less solvent consumption, whereas preparative RP-HPLC gave a shorter separation time but with higher solvent consumption. These results demonstrated that either of these two methods of different separation mechanism is feasible, economical and efficient for rapid preparative isolation and purification of steroid saponins from Dioscorea zingiberensis C.H.Wright.

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High throughput HPLC/MS purification in support of drug discovery

Cited by 34 publications

References 22 publications

Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatographic mobile phases

Purification method development for chiral separation in supercritical fluid chromatography with the solubilities in supercritical fluid chromatographic mobile phases

Mass spectrometry analysis of new chemical entities for pharmaceutical discovery

Comparative Studies on Performance of CCC and Preparative RP-HPLC in Separation and Purification of Steroid Saponins from Dioscorea Zingiberensis C.H.Wright

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