AI Article Synopsis

  • The study involves encapsulating Trimethylated-β-cyclodextrin (TM-β-CD) into polymer monolithic capillary columns for improved nano-liquid chromatography aimed at chiral separations.
  • The monolithic phases were created through a one-pot method using specific monomers and solvents, resulting in chiral stationary phases characterized by various analytical techniques.
  • Results showed that higher concentrations of TM-β-CD led to columns with larger surface area and better enantioseparation efficiency for separating racemic pharmaceuticals, highlighting the effectiveness of this encapsulation strategy.

Article Abstract

Trimethylated-β-cyclodextrin (TM-β-CD) was encapsulated within several polymer monolithic capillary columns for reversed-phase chiral nano-liquid chromatography (nano-LC). The monolithic phases were prepared using the one-pot in situ copolymerization of ethylene glycol dimethacrylate (EDMA), glycidyl methacrylate (GMA) monomers and 1-propanol, 1,4-butanediol as progenic solvents in presence of TM-β-CD solution within fused silica capillaries (150µm I.D.). The obtained chiral monolithic stationery phases were characterized by scanning electron microscopy (SEM), N adsorption/desorption isotherms, wide angle x-ray diffraction (WAXRD), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). The materials characterization demonstrated that monolithic phases with higher concentration of TM-β-CD have relatively larger surface area, smaller pore size and larger total pore volume compared to those with lower concentration TM-β-CD. The prepared columns were tested for their enantioseparation efficiency of a range of racemic pharmaceuticals. The screening results demonstrated the potential of functionalizing polymer monolithic stationary phases with TM-β-CD using the in situ encapsulation approach.

Download full-text PDF

Source
http://dx.doi.org/10.1016/j.talanta.2016.06.027DOI Listing

Publication Analysis

Top Keywords

monolithic capillary
8
capillary columns
8
polymer monolithic
8
monolithic phases
8
concentration tm-β-cd
8
tm-β-cd
5
monolithic
5
trimethyl-β-cyclodextrin-encapsulated monolithic
4
columns preparation
4
preparation characterization
4

Similar Publications

Precise Light-Driven Polarity of Stationary Phase for Regulating Gradient Separation of Liquid Chromatography.

Anal Chem

December 2024

Department of Chemistry, National Demonstration Centre for Experimental Chemistry Education, Yanbian University, Yanji City 133002, Jilin Province, China.

Generally, the traditional stationary phase for liquid chromatography is the key part, but with an in situ immutable property, leading to many separation limitations. Based on the former exploration of photosensitive gas chromatography, we successfully prepared a photosensitive monolithic capillary silica column with high light transmission, taking advantage of the reversible cis-trans isomerism of azobenzene. And the cis-trans isomerism has launched an effective, reversible, and precise control on the liquid chromatographic retention behavior just by photoinduction according to the theoretical basis of a good correlation between photoinduction time, -azobenzene ratio, and chromatographic retention factor () ( > 0.

View Article and Find Full Text PDF

In order to enrich the selection of biological ligands, realize the miniaturization analysis, and broaden the application of monolith materials for active ingredients screening and separating, we sough to construct a lipid raft @capillary monolith microcolumn affinity chromatography model. Single factor experiments and various characterization methods, including scanning electron microscopy (SEM) and thermogravimetric analysis, were employed to investigate the polymerization of the monolith column under different material ratios to determine optimal preparation conditions. Subsequently, the lipid raft from U251 cells was integrated with the monolith materials based on epoxy-based covalent crosslinking principle and characterized through SEM and immunofluorescence methods.

View Article and Find Full Text PDF

We present a novel chip-based device featuring a pinhole emitter for mass spectrometry (MS) coupling with integrated fluidic back-pressure regulation for supercritical mobile phases. This design enables facile coupling of packed capillary columns used for supercritical fluid chromatography (SFC) with atmospheric pressure ionization mass spectrometry. The monolithic microfluidic chips were fabricated using selective laser-induced etching, seamlessly integrating multiple functions, including comb-shaped particle retention structures for column packing and ports for zero-clearance connection with standard fused silica capillaries.

View Article and Find Full Text PDF

Preparation of amyloid N-terminal nonapeptide imprinted monolithic column and evaluation of adsorption properties.

J Pharm Biomed Anal

February 2025

College of Pharmacy, Jiangsu Ocean University, Lianyungang, 222005, China; Jiangsu Key Laboratory of Marine Pharmaceutical Compound Screening, College of Pharmacy, Jiangsu Ocean University, Lianyungang 222005, China. Electronic address:

A novel β-amyloid protein capillary microextraction column was designed and prepared using epitope molecular imprinting technology for specific recognition of trace β-amyloid proteins in complex biological matrices. Using N-terminal nonapeptide of β-amyloid protein as template molecule, choline chloride-MAA and N-hydroxymethyl acrylamide as functional monomers, ethylene glycol dimethacrylate as crosslinker, the imprinted capillary monolithic column was prepared by thermal polymerization in the acetonitrile-water system. The optimal preparation parameters were obtained with the ratio of template: functional monomer: crosslinker at 1:6:16 (mmol/mmol/mmol).

View Article and Find Full Text PDF

Cryogel particles were obtained by freeze-drying and grinding hydrogel monoliths made from 20 % (w/w) whey protein isolate (WP) suspensions prepared at different pH (pH 4.8, 5.7, and 7.

View Article and Find Full Text PDF

Want AI Summaries of new PubMed Abstracts delivered to your In-box?

Enter search terms and have AI summaries delivered each week - change queries or unsubscribe any time!