Dispersive Solid-Phase Extraction using Magnetic Carbon Nanotube Composite for the Determination of Emergent Mycotoxins in Urine Samples.

Campillo Campillo,Arroyo-Manzanares Arroyo-Manzanares,Peñalver-Soler Peñalver-Soler,Viñas Viñas

doi:10.3390/toxins12010051

Abstract

Dispersive magnetic solid-phase extraction (DMSPE) has received growing attention for sample treatment preconcentration prior to the separation of analytes due to its many advantages. In the present work, the potential of DMSPE for the determination of emergent mycotoxins (enniatins A, A1, B and B1, and beauvericin) is investigated for the first time. Different magnetic nanoparticles were tested and a magnetic multiwalled carbon nanotube (Fe3O4@MWCNT) composite was selected for the extraction and preconcentration of the five target mycotoxins in human urine samples before their analysis by ultrahigh performance liquid chromatography coupled to high resolution mass spectrometry (UHPLC-HRMS). The nanocomposite was characterized by energy dispersive X-ray spectrometry, scanning electron microscopy, Fourier transform infrared spectrophotometry, and X-ray diffraction. Several parameters affecting the adsorption and desorption of DMSPE steps were optimized and the method was fully validated. Due to a matrix effect, matrix-matched calibration curves were necessary to carry out quantification. In this way, limits of quantification of between 0.04 and 0.1 μg/L, relative standard deviation values lower than 12% and recoveries between 89.3% and 98.9% were obtained. Finally, a study of the reuse of the Fe3O4@MWCNT composite was carried out, confirming that it can be reused at least four times.

Highlights

Mycotoxins are low molecular weight noxious secondary metabolites produced by toxicogenic strains of some mould species that mainly belong to the genera Aspergillus, Fusarium, Penicillium, Alternaria, and Claviceps
high resolution mass spectrometry (HRMS) has been demonstrated for the first time
The proposed method based on Dispersive magnetic solid‐phase extraction (DMSPE) has multiple advantages over other sample treatments, such as the enhancement of the mass transfer, the improvement of the extraction efficiency, and the reduction of organic volume solvent in the desorption step, avoiding filtration or centrifugation steps

Summary

Introduction

Mycotoxins are low molecular weight noxious secondary metabolites produced by toxicogenic strains of some mould species that mainly belong to the genera Aspergillus, Fusarium, Penicillium, Alternaria, and Claviceps. Approximately 400 different mycotoxins have been described, the most common are aflatoxins (B1, B2, G1, and G2), ochratoxin A, fumonisins, trichothecenes, zearalenone, and patulin. Mycotoxins can contaminate animal feed, food, or the raw materials used for their production, originating diseases and disorders, both in humans and animals. Mycotoxins can bioaccumulate in fluids, tissues and organs, especially the liver and kidney, as well as affect the nervous, endocrine, and immune systems. Due to their toxicity, the European Union has established or recommended maximum permissible contents for some of these contaminants in various foods [1,2,3].

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