Halloysite nanotubes-based hybrid silica monolithic spin tip for hydrophilic solid-phase extraction of sulbactam, cefoperazone, and cefuroxime in whole blood

J Chromatogr A. 2024 Jun 21:1725:464943. doi: 10.1016/j.chroma.2024.464943. Epub 2024 Apr 25.

Abstract

In this study, we proposed a novel method utilizing polyethyleneimine (PEI)-modified halloysite nanotubes (HNTs)-based hybrid silica monolithic spin tip to analyze hydrophilic β-lactam antibiotics and β-lactamases inhibitors in whole blood samples for the first time. HNTs were incorporated directly into the hybrid silica monolith via a sol-gel method, which improved the hydrophilicity of the matrix. The as-prepared monolith was further modified with PEI by glutaraldehyde coupling reaction. It was found that the PEI-modified HNTs-based hybrid silica monolith enabled a large adsorption capacity of cefoperazone at 35.7 mg g-1. The monolithic spin tip-based purification method greatly reduced the matrix effect of whole blood samples and had a detection limit as low as 0.1 - 0.2 ng mL-1. In addition, the spiked recoveries of sulbactam, cefuroxime, and cefoperazone in blank whole blood were in the range of 89.3-105.4 % for intra-day and 90.6-103.5 % for inter-day, with low relative standard deviations of 1.3-7.2 % and 4.9-10.5 %, respectively. This study introduces a new strategy for preparing nanoparticles incorporated in a hybrid silica monolith with a high adsorption capacity. Moreover, it offers a valuable tool to monitor sulbactam, cefoperazone, and cefuroxime in whole blood from pregnant women with the final aim of guiding their administration.

Keywords: Halloysite nanotubes; Hybrid silica monolith; Whole blood; β-lactam antibiotic; β-lactamases inhibitor.

MeSH terms

  • Adsorption
  • Anti-Bacterial Agents / blood
  • Anti-Bacterial Agents / chemistry
  • Cefoperazone* / blood
  • Cefoperazone* / chemistry
  • Cefuroxime* / blood
  • Cefuroxime* / chemistry
  • Chromatography, High Pressure Liquid / methods
  • Clay / chemistry
  • Humans
  • Hydrophobic and Hydrophilic Interactions*
  • Limit of Detection*
  • Nanotubes* / chemistry
  • Polyethyleneimine / chemistry
  • Reproducibility of Results
  • Silicon Dioxide* / chemistry
  • Solid Phase Extraction* / methods
  • Sulbactam* / blood
  • Sulbactam* / chemistry

Substances

  • Cefoperazone
  • Sulbactam
  • Silicon Dioxide
  • Cefuroxime
  • Clay
  • Anti-Bacterial Agents
  • Polyethyleneimine