Abstract

The aim of this study was to develop magnetic molecularly imprinted nano-conjugate sorbent for effective dispersive solid phase extraction of antazoline (ANT) and its metabolite, hydroxyantazoline (ANT-OH) in analytical method employing liquid chromatography coupled with mass spectrometry method. The core–shell material was characterized in terms of adsorption properties, morphology and structure. The heterogeneous population of adsorption sites towards ANT-OH was characterized by two Kd and two Bmax values: Kd (1) = 0.319 µg L−1 and Bmax (1) = 0.240 μg g−1, and Kd (2) = 34.6 µg L−1 and Bmax (2) = 5.82 μg g−1. The elemental composition of magnetic sorbent was as follows: 17.55, 37.33, 9.14, 34.94 wt% for Si, C, Fe and O, respectively. The extraction protocol was optimized, and the obtained results were explained using theoretical analysis. Finally, the analytical method was validated prior to application to pharmacokinetic study in which the ANT was administrated intravenously to three healthy volunteers. The results prove that the novel sorbent could be useful in extraction of ANT and ANT-OH from human plasma and that the analytical strategy could be a versatile tool to explain a potential and pharmacological activity of ANT and ANT-OH.

Highlights

  • Introduction iationsIn recent years, many advances have been made in the field of biomedical and food analysis mainly due to developments of hyphenated analytical techniques like liquid chromatography coupled with mass spectrometry (LC-MS)

  • Adsorption Properties imprinted polymer) and mag-NIP, the analysis of bindIn order to reveal the adsorption characteristics of mag-molecularly imprinted polymers (MIPs) (magnetic molecularly ing capacities was calculated according to Equation (1) and mag-NIP, the analysis of ANT and ANT-OH)

  • The adsorption properties were evaluated using Freundlich model, binding capacities was calculated according to Equation (1)

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Summary

Introduction

Many advances have been made in the field of biomedical and food analysis mainly due to developments of hyphenated analytical techniques like liquid chromatography coupled with mass spectrometry (LC-MS). Biological matrices contain diverse components with different chemical properties, which greatly hinder the selective extraction of target analytes, reducing the sensitivity of the instrumental analytical methods. Sample pretreatment methods are constantly developing aiming to reduce the matrix effect and improve the method selectivity. One of the most effective method is solid phase extraction (SPE), reliable and cost-effective technique for the selective isolation and concentration of a wide range of analytes and sample matrices [1]. Low selectivity of commercial sorbents used in the pretreatment step limited the applicability of the technique. The molecularly imprinted polymers (MIPs) could be Licensee MDPI, Basel, Switzerland

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