Maximizing two-dimensional liquid chromatography peak capacity for the separation of complex industrial samples

Zhu, Koudi; Pursch, Matthias; Eeltink, Sebastiaan; Desmet, Gert

doi:10.1016/j.chroma.2019.460457

Cited by 15 publications

(10 citation statements)

References 59 publications

(57 reference statements)

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“…In a study aimed at maximizing peak capacity, an aromatic amine oligomer sample was separated by 2DLC using up to six 15 cm long pentafluorophenyl columns in first dimension and a 5 cm RPLC column in second dimension. 141 A theoretical maximum peak capacity of 11,000 was achieved and more than 900 resolved peaks were detected in the sample. Other work involved separation of relatively low molecular weight glycerol ethoxylates, glycerol propoxylates, glycerol-ethoxylate-co-propoxylates, and castor oil-based ethoxylates by comprehensive 2DLC comprising HILIC × RPLC and the separation was coupled to high resolution mass spectrometry (Q-TOF) for detection and identification of the individual oligomers.…”

Section: ■ Multidimensional Separations Of Polymers and Oligomersmentioning

confidence: 98%

“…Multidimensional separations of oligomers often produce impressive numbers of well-separated and identifiable components in the distribution, and a number of examples were published in recent years. In a study aimed at maximizing peak capacity, an aromatic amine oligomer sample was separated by 2DLC using up to six 15 cm long pentafluorophenyl columns in first dimension and a 5 cm RPLC column in second dimension . A theoretical maximum peak capacity of 11,000 was achieved and more than 900 resolved peaks were detected in the sample.…”

Section: Multidimensional Separations Of Polymers and Oligomersmentioning

confidence: 99%

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Recent Advances in Separation-Based Techniques for Synthetic Polymer Characterization

et al. 2020

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Section: ■ Multidimensional Separations Of Polymers and Oligomersmentioning

confidence: 98%

Section: Multidimensional Separations Of Polymers and Oligomersmentioning

confidence: 99%

Recent Advances in Separation-Based Techniques for Synthetic Polymer Characterization

et al. 2020

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“…Other orthogonal separation systems, including 2D-NPLC × RPLC [16], 2D-SEC × RPLC [17][18][19], 2D-chiral × chiral [20], and 2D-achiral × chiral [21], temperatureresponsive LC × RPLC [22], countercurrent chromatography × RPLC [23], IEC × assay-based RPLC [24], SFC × RPLC [25], IPC × RPLC [26], and IEC × SEC [27] have also been developed and applied toward the analysis of biosamples. Moreover, advanced strategies [28][29][30] were proposed for the development of a more systematic, less tedious, and less reliant on user expertise 2D-LC method. Notably, the introduction of a new stationary phase with unique selectivity has become a popular strategy for the construction of new 2D-LC systems [9,31].…”

Section: Introductionmentioning

confidence: 99%

Comprehensive profiling of Sanguisorba officinalis using offline two‐dimensional mixed‐mode liquid chromatography × reversed‐phase liquid chromatography, tandem high‐resolution mass spectrometry, and molecular network

Dai

Zhang

Xiong

et al. 2022

J of Separation Science

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The profiling of natural products is important in modern biological sciences and new drug development. However, the separation and characterization of complex herbal extracts are significantly challenging for researchers in the biochemical field. Herein, an offline two-dimensional mixed-mode liquid chromatography × reversed-phase liquid chromatography system is developed. Our system exhibits high orthogonality and is composed of a newly prepared stationary phase in the first dimension and a traditional C 18 phase in the second dimension, and is operated in combination with a high-resolution mass spectrometry and molecular network. Sanguisorba officinalis L. is studied using the proposed method owing to its bioactivity. With the aid of orthogonal separation, the ionization of the individual components is improved. The number of detected compounds and separated peaks are significantly increased when one-dimensional liquid chromatography is upgraded to two-dimensional liquid chromatography.In addition, 270 compounds (127 of which are tentatively characterized as new compounds, and further confirmation is needed) are successfully characterized based on their fragmentation patterns under the guidance of molecular network, while only 95 compounds are characterized using one-dimensional liquid chromatography and high-resolution mass spectrometry. The results indicate that the developed offline two-dimensional mixed-mode liquid chromatography ×

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“…Heterogeneities and chemical complexity associated with such molecules include a high-order structure, composition, conformation, complex mixtures, closely related components along with post-translational modifications, and other chemical changes that occur during bioprocesses . Chromatography is at the center of all facets of pharmaceutical analysis and purification; robust analytical and preparative chromatographic methods are badly needed to accelerate drug research and development efforts. − …”

Section: Introductionmentioning

confidence: 99%

Mapping the Separation Landscape in Two-Dimensional Liquid Chromatography: Blueprints for Efficient Analysis and Purification of Pharmaceuticals Enabled by Computer-Assisted Modeling

et al. 2020

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Recent developments in two-dimensional liquid chromatography (2D-LC) now make separation and analysis of very complex mixtures achievable. Despite being such a powerful chromatographic tool, current 2D-LC technology requires a series of arduous method development activities poorly suited for a fast-paced industrial environment. Recent introductions of new technologies including active solvent modulation and a support for multicolumn 2D-LC are helping to overcome this stigma. However, many chromatography practitioners believe that the lack of a systematic way to effectively optimize 2D-LC separations is a missing link in securing the viability of 2D-LC as a mainstay for industrial applications. In this work, a computer-assisted modeling approach that dramatically simplifies both offline and online 2D-LC method developments is introduced. Our methodology is based on mapping the separation landscape of pharmaceutically relevant mixtures across both first (1 D) and second (2 D) dimensions using LC Simulator (ACD/Labs) software. Retention models for 1 D and 2 D conditions were built using a minimal number of multifactorial modeling experiments (2 × 2 or 3 × 3 parameters: gradient slope, column temperature, and different column and mobile phase combinations). The approach was first applied to online 2D-LC analysis involving achiral and chiral separations of complex mixtures of enantiomeric species. In these experiments, the retention models proved to be quite accurate for both the 1 D and 2 D separations, with retention time differences between experiments and simulations of less than 3.5%. This software-based concept was also demonstrated for offline 2D-LC purification of drug substances.

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Maximizing two-dimensional liquid chromatography peak capacity for the separation of complex industrial samples

Cited by 15 publications

References 59 publications

Recent Advances in Separation-Based Techniques for Synthetic Polymer Characterization

Recent Advances in Separation-Based Techniques for Synthetic Polymer Characterization

Comprehensive profiling of Sanguisorba officinalis using offline two‐dimensional mixed‐mode liquid chromatography × reversed‐phase liquid chromatography, tandem high‐resolution mass spectrometry, and molecular network

Mapping the Separation Landscape in Two-Dimensional Liquid Chromatography: Blueprints for Efficient Analysis and Purification of Pharmaceuticals Enabled by Computer-Assisted Modeling

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