Approaches to find complementary separation conditions for resolving complex mixtures by high-performance liquid chromatography

Ortiz-Bolsico, C.; Torres-Lapası́o, J.R.; García-Álvarez-Coque, M.C.

doi:10.1016/j.chroma.2012.01.034

Cited by 9 publications

(3 citation statements)

References 15 publications

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“…The chromatographic separation of complex mixtures of closely related species is becoming increasingly important in pharmaceutical and biomedical research, reflecting the ever-increasing complexity of both fundamental biology and the therapeutics used to treat disease. − Multidimensional separation techniques have emerged as a preferred tool for dealing with complex samples, with new liquid chromatography–mass spectrometry hybrid techniques laying the foundation for the ongoing omics revolution in biomedicine. − Recent years have seen a rapid growth in the use of multidimensional chromatography for the study of complex mixtures, with two-dimensional (2D) chromatography emerging as a valuable tool for pharmaceutical, biomedical research, and other disciplines. − However, this technique continues to evolve rapidly as it moves from the realm of isolated studies by experts using custom equipment to the realm of routine use by nonspecialists using platform technology solutions.…”

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confidence: 99%

Ultrafast Chiral Chromatography as the Second Dimension in Two-Dimensional Liquid Chromatography Experiments

Barhate

Regalado²,

Contrella³

et al. 2017

Anal. Chem.

107

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Chromatographic separation and analysis of complex mixtures of closely related species is one of the most challenging tasks in modern pharmaceutical analysis. In recent years, two-dimensional liquid chromatography (2D-LC) has become a valuable tool for improving peak capacity and selectivity. However, the relatively slow speed of chiral separations has limited the use of chiral stationary phases (CSPs) as the second dimension in 2D-LC, especially in the comprehensive mode. Realizing that the recent revolution in the field of ultrafast enantioselective chromatography could now provide significantly faster separations, we herein report an investigation into the use of ultrafast chiral chromatography as a second dimension for 2D chromatographic separations. In this study, excellent selectivity, peak shape, and repeatability were achieved by combining achiral and chiral narrow-bore columns (2.1 mm × 100 mm and 2.1 mm × 150 mm, sub-2 and 3 μm) in the first dimension with 4.6 mm × 30 mm and 4.6 mm × 50 mm columns packed with highly efficient chiral selectors (sub-2 μm fully porous and 2.7 μm fused-core particles) in the second dimension, together with the use of 0.1% phosphoric acid/acetonitrile eluents in both dimensions. Multiple achiral × chiral and chiral × chiral 2D-LC examples (single and multiple heart-cutting, high-resolution sampling, and comprehensive) using ultrafast chiral chromatography in the second dimension are successfully applied to the separation and analysis of complex mixtures of closely related pharmaceuticals and synthetic intermediates, including chiral and achiral drugs and metabolites, constitutional isomers, stereoisomers, and organohalogenated species.

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confidence: 99%

Ultrafast Chiral Chromatography as the Second Dimension in Two-Dimensional Liquid Chromatography Experiments

Barhate

Regalado²,

Contrella³

et al. 2017

Anal. Chem.

107

View full text Add to dashboard Cite

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“…the solvent content) was compared under isocratic elution using the same training set. In order to optimise parallel columns of different nature, a previous approach (developed to search complementary mobile phases [20]) was adapted. The performance of the different configurations was evaluated through the limiting resolutions and the percentage of separation capability of the chromatographic systems reached at the optimal conditions.…”

Section: Discussionmentioning

confidence: 99%

“…Also, along the last decade, we have reported a different separation approach, based on the complementarity concept, which has succeeded in the resolution of highly complex samples [20]. In this approach, a separation condition focuses on the resolution of some compounds in the sample, while the other compounds remain unresolved, but are optimally resolved in a second (or subsequent) condition(s).…”

Section: Introductionmentioning

confidence: 98%