Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

COF-SiO2@Fe3O4 Core-Shell Composite for Magnetic Solid-Phase Extraction of Pyrethroid Pesticides in Vegetables

Version 1 : Received: 17 February 2024 / Approved: 18 February 2024 / Online: 19 February 2024 (11:28:09 CET)

How to cite: Yu, L.; Xia, A.; Hao, Y.; Li, W.; Xing, C.; Shang, Z.; Zhang, Y. COF-SiO2@Fe3O4 Core-Shell Composite for Magnetic Solid-Phase Extraction of Pyrethroid Pesticides in Vegetables. Preprints 2024, 2024020937. https://doi.org/10.20944/preprints202402.0937.v1 Yu, L.; Xia, A.; Hao, Y.; Li, W.; Xing, C.; Shang, Z.; Zhang, Y. COF-SiO2@Fe3O4 Core-Shell Composite for Magnetic Solid-Phase Extraction of Pyrethroid Pesticides in Vegetables. Preprints 2024, 2024020937. https://doi.org/10.20944/preprints202402.0937.v1

Abstract

Pyrethroid pesticides (PYRs) as the third most widely used pesticides, following organophosphorus and carbamate pesticides, which are of significant importance in the analysis and detection of vegetables. However, the current pretreatment technology for PYRs confronts challenges of difficult separation and low enrichment efficiency, resulting in a cumbersome and time-consuming pretreatment process with poor selectivity. Here, a simple and efficient magnetic solid-phase extraction (MSPE) strategy was developed to simultaneously purify and enrich five PYRs in vegetables, with the magnetic covalent organic framework nanomaterial COF-SiO2@Fe3O4 as an adsorbent. The COF-SiO2@Fe3O4 was prepared by a simple solvothermal conditions method, using Fe3O4 as magnetic core, benzidine and 3,3,5,5-tetraaldehyde biphenyl as two building units. COF-SiO2@Fe3O4 could effectively capture the targeted PYRs by virtue of its abundant π-electron system and hydroxyl groups. The impact of various experimental parameters on extraction efficiency was investigated to optimize the MSPE conditions, including adsorbent amount, extraction time, elution solvent type and elution time. Subsequently, method validation was conducted under the optimal conditions in conjunction with gas chromatography-mass spectrometry (GC-MS). Within the range of 5.00–100 μg·kg-1 (1.00–100 μg·kg-1 for bifenthrin and 2.5–100 μg·kg-1 for fenpropathrin), the five PYRs exhibited a strong linear relationship, with determination coefficients ranging from 0.9990 to 0.9997. The limits of detection (LODs) were 0.3–1.5 μg·kg-1, and the limits of quantification (LOQs) were 0.9–4.5 μg·kg-1. The recoveries were 80.2–116.7% with relative standard deviations (RSDs) below 7.0%. Finally, COF-SiO2@Fe3O4, NH2-SiO2@Fe3O4 and Fe3O4 were compared as MSPE adsorbents for PYRs. The results indicated that COF-SiO2@Fe3O4 was an efficient and rapid selective adsorbent for PYRs. This method holds promising prospects for the determination of PYRs in real samples.

Keywords

covalent organic framework; magnetic solid-phase extraction; gas chromatography-mass spectrometry; pyrethroids pesticides

Subject

Chemistry and Materials Science, Analytical Chemistry

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