Review of recent advances in development and applications of organic‐silica hybrid monoliths

Zajickova, Zuzana

doi:10.1002/jssc.202300396

Cited by 7 publications

(2 citation statements)

References 114 publications

(202 reference statements)

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“…On the other hand, silica‐based monoliths with bimodal pore structures and large surface areas have been known to be better suited for the separations of small molecules [4, 5]. Likewise, organo‐silica hybrid monoliths have been mostly applied to the analysis of low molecular weight compounds [6–8]; however, as the field advanced and new hybrid monolithic columns were developed, reports of liquid chromatography (LC) analysis of large biomolecules emerged.…”

Section: Introductionmentioning

confidence: 99%

Characterization of hybrid organo‐silica monoliths for possible application in the gradient elution of peptides

Kosmáková,

Zajickova,

Urban

2023

J of Separation Science

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We characterized thermally polymerized organo‐silica hybrid monolithic capillaries to test their applicability in the gradient elution of peptides. We have used a single‐pot approach utilizing 3‐(methacryloyloxy)propyltrimethoxysilane (MPTMS), ethylene dimethacrylate (EDMA), and n‐octadecyl methacrylate (ODM) as functional monomers. The organo‐silica monolith containing MPTMS and EDMA was compared with the stationary phase prepared by adding ODM to the original polymerization mixture. Column prepared using a three‐monomer system provided a lower accessible volume of flow‐through pores, a higher proportion of mesopores, and higher efficiency. We utilized isocratic and gradient elution data to predict peak widths in gradient elution. Both protocols provided comparable results and can be used for peptide peak width prediction. However, applying gradient elution data for peak width prediction seems simpler. Finally, we tested the effect of gradient time on achievable peak capacity in the gradient elution of peptides with a column prepared with a three‐monomer system providing a higher peak capacity. However, the performance of hybrid organo‐silica monolithic stationary phases in gradient elution of peptides must be improved compared to other monolithic stationary phases. The limiting factor is column efficiency in highly aqueous mobile phases, which needs to be focused on.

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Section: Introductionmentioning

confidence: 99%

Characterization of hybrid organo‐silica monoliths for possible application in the gradient elution of peptides

Kosmáková,

Zajickova,

Urban

2023

J of Separation Science

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“…Alkyne–azide cycloaddition is the most commonly used reaction to immobilize functional groups in different materials . Thiol-ene click reactions are mostly exploited for preparation of silica hybrid or polymer monoliths, as reviewed elsewhere. − …”

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confidence: 99%

Preparation of Monolith for Online Extraction and LC–MS Analysis of β-Estradiol in Serum Via a Simple Multicomponent Reaction

Cerrato,

Aita,

Cavaliere

et al. 2024

Anal. Chem.

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Multicomponent reactions offer efficient and environmentally friendly strategies for preparing monoliths suitable for applications in analytical chemistry. In the described study, a multicomponent reaction was utilized for the one-pot miniaturized preparation of a poly(propargyl amine) polymer inside commercial silica-lined PEEK tubing. The reaction involved only small amounts of reagents and was characterized by atom economy. The resulting monolithic column was incorporated into an autosampler system for the online extraction and cleanup of β-estradiol from human serum. Sample pretreatment was simplified to a simple dilution with methanol and centrifugation to remove proteins. The resulting platform included LC−MS analysis in multiple reaction monitoring for quantitative analysis of β-estradiol. The method was validated in serum, demonstrating practical applicability for the monitoring of fertile women. Recoveries were above 94%, and LOD and LOQ values at 0.008 and 0.18 ng mL −1 , respectively. The developed platform proved to be competitive with previous methods for solidphase microextraction of β-estradiol in serum, with comparable recovery and sensitivity but with the advantage of nearly complete automation. The environmental impact of the process was evaluated as acceptable due to the miniaturization of the monolith synthesis and the automation of extraction. The drawback associated with the LC−MS technique can be reduced by the inclusion of additional analytes in a single investigation. The work demonstrates that multicomponent reactions are versatile, economical, and possibly a green methodology for producing reversed-phase and mixed-mode sorbents, enabling miniaturization of the entire analytical procedure from the preparation of extraction sorbents to analysis.

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Effect of crosslinker/porogen ratio on sponge-nested polymer monoliths for solid-phase extraction

Morales,

Thickett,

Maya

2024

Journal of Chromatography A

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Review of recent advances in development and applications of organic‐silica hybrid monoliths

Cited by 7 publications

References 114 publications

Characterization of hybrid organo‐silica monoliths for possible application in the gradient elution of peptides

Characterization of hybrid organo‐silica monoliths for possible application in the gradient elution of peptides

Preparation of Monolith for Online Extraction and LC–MS Analysis of β-Estradiol in Serum Via a Simple Multicomponent Reaction

Effect of crosslinker/porogen ratio on sponge-nested polymer monoliths for solid-phase extraction

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