NH2-MIL-53(Al) Polymer Monolithic Column for In-Tube Solid-Phase Microextraction Combined with UHPLC-MS/MS for Detection of Trace Sulfonamides in Food Samples.

Qian-Chun Zhang,Xiao-Lan Zhang,Jun-Yi Liang,Xing-Yi Wang,Li Jiang,Yu-Guo Zheng,Guang-Ping Xia

doi:10.3390/molecules25040897

Qian-Chun Zhang, Xiao-Lan Zhang + Show 5 more

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https://doi.org/10.3390/molecules25040897

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Abstract

In this study, a novel monolithic capillary column based on a NH2-MIL-53(Al) metal–organic framework (MOF) incorporated in poly (3-acrylamidophenylboronic acid/methacrylic acid-co-ethylene glycol dimethacrylate) (poly (AAPBA/MAA-co-EGDMA)) was prepared using an in situ polymerization method. The characteristics of the MOF-polymer monolithic column were investigated by scanning electron microscopy, Fourier-transform infrared spectroscopy, X-ray photoelectron spectroscopy, X-ray diffractometry, Brunauer-Emmett-Teller analysis, and thermogravimetric analysis. The prepared MOF-polymer monolithic column showed good permeability, high extraction efficiency, chemical stability, and good reproducibility. The MOF-polymer monolithic column was used for in-tube solid-phase microextraction (SPME) to efficiently adsorb trace sulfonamides from food samples. A novel method combining MOF-polymer-monolithic-column-based SPME with ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was successfully developed. The linear range was from 0.015 to 25.0 µg/L, with low limits of detection of 1.3–4.7 ng/L and relative standard deviations (RSDs) of < 6.1%. Eight trace sulfonamides in fish and chicken samples were determined, with recoveries of the eight analytes ranging from 85.7% to 113% and acceptable RSDs of < 7.3%. These results demonstrate that the novel MOF-polymer-monolithic-column-based SPME coupled with UHPLC-MS/MS is a highly sensitive, practical, and convenient method for monitoring trace sulfonamides in food samples previously extracted with an adequate solvent.

Highlights

Sulfonamides (SAs) are the most widely used antimicrobial veterinary drugs due to their low cost and high efficacy for targeting bacterial infections [1]
SAs cannot be completely metabolized by animals, resulting in SAs residues from veterinary drugs entering the human body through the food chain, potentially posing many risks to consumers [2]
Fourier-transform infrared (FT-IR) spectroscopy is a common method for characterization of chemical bonds and functional groups, providing insight into chemical groups that have been transformed or are present for a given compound

Summary

Introduction

Sulfonamides (SAs) are the most widely used antimicrobial veterinary drugs due to their low cost and high efficacy for targeting bacterial infections [1]. SAs cannot be completely metabolized by animals, resulting in SAs residues from veterinary drugs entering the human body through the food chain, potentially posing many risks to consumers [2]. In order to protect consumer safety, many countries and regions have established standardized acceptable levels for SAs in food products of animal origin. The European Union (EU) has adopted a maximum residue limit of 100 μg/kg for SAs in foods of animal origin [6,7,8]. It is, important to establish an effective, rapid, simple, and sensitive method for SAs determination for pre-enrichment before analysis

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