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Advances in Hydrophilic Interaction Liquid Chromatography

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A special issue of Molecules (ISSN 1420-3049). This special issue belongs to the section "Analytical Chemistry".

Deadline for manuscript submissions: closed (31 May 2023) | Viewed by 11526

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Dr. Xavier Subirats

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Guest Editor

Faculty of Chemistry, University of Barcelona, Barcelona, Spain
Interests: chromatographic retention modeling; HILIC; lipophilicity; solubility; acidity; subrogation of biological systems

Special Issue Information

Dear Colleagues,

Hydrophilic interaction liquid chromatography (HILIC) is a powerful technique for the separation of polar and ionized analytes, particularly in the context of samples of biological interest. In the last decade, the development of HILIC methodologies and applications has surged, not only in the fields of pharmaceutical, environmental and food analysis, but also in the complex omics sciences, such as metabolomics, genomics, proteomics and glycomics. After reversed-phase chromatography, HILIC is in fact the liquid chromatographic mode with the highest number of applications. It combines polar stationary phases with organic-solvent-rich mobile phases, leading to a complementary selectivity to the reversed phase.

To facilitate these various applications, several manufacturers include in their commercial catalogues a good number of columns with different polar packing materials (zwitterionic, aminopropyl, amide, diol, bare silica, etc.), but retention mechanisms in HILIC are very complex and not yet completely understood. It is generally accepted that retention is mainly based on the partition of analytes between the mobile phase and a water-rich layer sorbed (or semi-sorbed) on the packing material, but hydrogen bonding and dipole–dipole or electrostatic interactions with the bonded phase may also take place. A better understanding of HILIC retention mechanisms could help method development and boost the number of applications.

This Special Issue aims to both disseminate new methodologies and applications for the resolution (bio)analytical problems and present recent advances in retention modelling in HILIC.

Dr. Xavier Subirats
Guest Editor

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Keywords

hydrophilic interaction liquid chromatography
HILIC
biomolecules
omics
column characterization
selectivity

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Published Papers (5 papers)

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Research

12 pages, 2335 KiB

Open AccessArticle

Hydrophilic Partitioning or Surface Adsorption? A Quantitative Assessment of Retention Mechanisms for Hydrophilic Interaction Chromatography (HILIC)

by Yong Guo and Dominik Baran

Molecules 2023, 28(18), 6459; https://doi.org/10.3390/molecules28186459 - 6 Sep 2023

Cited by 4 | Viewed by 1235

Abstract

Retention mechanisms in HILIC have been investigated and reported in literature. However, the current understanding of retention mechanisms is qualitative and lacks quantitative details. Previously, mechanism elucidation was based on indirect evidence, and unambiguous assignment of retention mechanisms has not been reported based on direct data. This study aims to quantitatively determine the contributions of two major retention mechanisms in HILIC, hydrophilic partitioning and surface adsorption to the overall retention of neutral compounds. Using the methodologies we developed previously, the phase ratio for adsorbed water layer and distribution coefficients were measured and used to calculate the retention factors contributed by hydrophilic partitioning. The methodology allows the determination of the contribution of surface adsorption simultaneously. The evaluation of five test compounds demonstrates that the retention may be controlled by hydrophilic partitioning, surface adsorption or both depending on compound characteristics. Quantitative assessment of retention mechanisms also makes it possible to better understand the effect of acetonitrile on retention in HILIC. Full article

(This article belongs to the Special Issue Advances in Hydrophilic Interaction Liquid Chromatography)

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10 pages, 637 KiB

Open AccessArticle

Determination of Glycerol, Propylene Glycol, and Nicotine as the Main Components in Refill Liquids for Electronic Cigarettes

by Paweł Kubica

Molecules 2023, 28(11), 4425; https://doi.org/10.3390/molecules28114425 - 29 May 2023

Cited by 2 | Viewed by 3276

Abstract

Refill liquids for electronic cigarettes are an important area of research due to the health safety and quality control of such products. A method was developed for the determination of glycerol, propylene glycol, and nicotine in refill liquids using liquid chromatography, coupled with tandem mass spectrometry (LC-MS/MS) in multiple reaction monitoring (MRM) mode with electrospray ionisation (ESI). Sample preparation was based on a simple dilute-and-shoot approach, with recoveries ranging from 96 to 112% with coefficients of variation < 6.4%. Linearity, limits of detection and quantification (LOD, LOQ), repeatability, and accuracy were determined for the proposed method. The proposed sample preparation and the developed chromatographic method using hydrophilic interaction liquid chromatography (HILIC) were successfully applied for the determination of glycerol, propylene glycol, and nicotine in refill liquid samples. For the first time, the developed method using HILIC-MS/MS has been applied for the determination of the main components of refill liquids in a single analysis. The proposed procedure is rapid and straightforward and is suitable for quick determination of glycerol, propylene glycol, and nicotine. The nicotine concentrations corresponded to the labelling of samples (it varied from <LOD—11.24 mg/mL), and the ratios of propylene glycol to glycerol were also determined. Full article

(This article belongs to the Special Issue Advances in Hydrophilic Interaction Liquid Chromatography)

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20 pages, 4034 KiB

Open AccessArticle

Reversed HILIC Gradient: A Powerful Strategy for On-Line Comprehensive 2D-LC

by Soraya Chapel, Florent Rouvière, Davy Guillarme and Sabine Heinisch

Molecules 2023, 28(9), 3907; https://doi.org/10.3390/molecules28093907 - 5 May 2023

Cited by 2 | Viewed by 2105

Abstract

The aim of the present work is to evaluate the possibilities and limitations of reversed hydrophilic interaction chromatography (revHILIC) mode in liquid chromatography (LC). This chromatographic mode consists of combining a highly polar stationary phase (bare silica) with a gradient varying from very low (1–5%) to high (40%) acetonitrile content (reversed gradient compared to HILIC). The retention behavior of revHILIC was first compared with that of reversed-phase LC (RPLC) and HILIC using representative mixtures of peptides and pharmaceutical compounds. It appears that the achievable selectivity can be ranked in the order RPLC > revHILIC > HILIC with the two different samples. Next, two-dimensional liquid chromatography (2D-LC) conditions were evaluated by combining RPLC, revHILIC, or HILIC with RPLC in an on-line comprehensive (LC × LC) mode. evHILIC × RPLC not only showed impressive performance in terms of peak capacity and sensitivity, but also provided complementary selectivity compared to RPLC × RPLC and HILIC × RPLC. Indeed, both the elution order and the retention time range differ significantly between the three techniques. In conclusion, there is no doubt that revHILIC should be considered as a viable option for 2D-LC analysis of small molecules and also peptides. Full article

(This article belongs to the Special Issue Advances in Hydrophilic Interaction Liquid Chromatography)

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21 pages, 8830 KiB

Open AccessArticle

In-Depth Performance Analysis and Comparison of Monolithic and Particulate Zwitterionic Hydrophilic Interaction Liquid Chromatography Polymer Columns

by Haibin Li, Zhengjin Jiang, Gert Desmet and Deirdre Cabooter

Molecules 2023, 28(7), 2902; https://doi.org/10.3390/molecules28072902 - 23 Mar 2023

Cited by 3 | Viewed by 1768

Abstract

The kinetic performance of different zwitterionic hydrophilic interaction liquid chromatography polymer columns is evaluated and compared in-depth. For this purpose, two lab-made monolithic columns, synthesized with different crosslinkers, and a commercial particle packed column are considered. It is found that performance evaluation techniques, such as comparing plate height curves or fitted A-, B- and C-terms, obtained by fitting experimental plate height data to a plate height model, are complicated by the determination of a reliable characteristic length. This is due to the very different morphology of these column types, and the heterogeneity of the monolithic columns. The occurrence of a convective flow through the packed particle column further complicates the interpretation of the obtained fitting parameters, as part of the C-term is wrongfully attributed to the A-term. Therefore, the use of the kinetic plot method is suggested for the comparative evaluation of these columns, as kinetic plots do not require the determination of a characteristic length, nor rely on any fitting parameters. With the kinetic plot method, it is demonstrated that the lab-made monolithic columns outperform the packed particle column for plate counts between 10,000 and 800,000. This is attributed to the higher column efficiency of these columns, due to their small domain and skeleton sizes, and their high permeability, resulting from their high external porosity and the occasional occurrence of preferential flow paths. Full article

(This article belongs to the Special Issue Advances in Hydrophilic Interaction Liquid Chromatography)

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16 pages, 2283 KiB

Open AccessArticle

Evaluation of Hold-Up Volume Determination Methods and Markers in Hydrophilic Interaction Liquid Chromatography

by Lídia Redón, Xavier Subirats and Martí Rosés

Molecules 2023, 28(3), 1372; https://doi.org/10.3390/molecules28031372 - 1 Feb 2023

Cited by 7 | Viewed by 2467

Abstract

Common methods for hold-up time and volume determination in Reversed-Phase Liquid Chromatography (RPLC) have been tested for Hydrophilic Interaction Liquid Chromatography (HILIC). A zwitterionic ZIC-HILIC column has been used for the testing. The pycnometric determination method, based on differences in column weight when filled with water or organic solvent, provides the overall volume of solvent inside the column. This includes the volume of eluent semi-sorbed on the packing of the column, which acts as the main stationary phase. The homologous series approach, based on the retention behavior of homologues in relation to their molecular volume, allows the determination of accurate hold-up volumes. However, the application of this method is time-consuming. In some cases, large neutral markers with poor dipolarity/polarizability and hydrogen bonding interactions can be used as hold-up volume markers. This is the case of dodecylbenzene and nonadecane-2-one in clearly HILIC behaving chromatographic systems, the use of decanophenone as a marker can be even extended to the boundary between HILIC and RPLC. The elution volume of the marker remains nearly unaffected by the concentration of ammonium acetate in the mobile phase up to 20 mM. The injection of pure solvents to produce minor base-line disturbance as hold-up markers is strongly discouraged, since solvent peaks are complex to interpret and depend on the ionic strength of the eluent. Full article

(This article belongs to the Special Issue Advances in Hydrophilic Interaction Liquid Chromatography)

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