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Simultaneous Determination and Investigation of Nine Fungicides in Fruits Using Diethylenetriamine-Functional Magnetic Core-Shell Polymer Modified Graphene Oxide as an Efficient Adsorbent Coupled to UPLC-HRMS

by Ming-Li Ye * and Yan Zhu
Department of Chemistry, Zhejiang University, Hangzhou 310028, China
*
Author to whom correspondence should be addressed.
Int. J. Mol. Sci. 2017, 18(11), 2333; https://doi.org/10.3390/ijms18112333
Received: 10 October 2017 / Revised: 28 October 2017 / Accepted: 2 November 2017 / Published: 5 November 2017
(This article belongs to the Section Biochemistry)
In this study, diethylenetriamine-functional magnetic core-shell polymer modified graphene oxide (DETA-MPs-GO) was prepared via precipitation polymerization and amidation reaction, and it was characterized by transmission electron microscopy (TEM), Fourier-transformed infrared spectroscopy (FTIR), and X-ray diffractometer (XRD). Subsequently, a magnetic solid-phase extraction (MSPE) procedure was applied to the as-synthesized DETA-MPs-GO for the detection of nine fungicides in fruit samples, prior to ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). The homogenized fruit samples, spiked with D-labelled internal standards, were firstly extracted by 5 mL of acetonitrile twice and then purified by DETA-MPs-GO adsorbents. The optimization of the adsorption and elution conditions of DETA-MPs-GO toward fungicides was carried out to attain a satisfactory adsorption performance and desorption efficiency. The adsorption mechanism was carefully investigated, and the results revealed that a synergistic adsorption mechanism, including hydrogen bond and a π–π stacking interaction, was confirmed. Moreover, the limits of quantitation (LOQs) of the proposed approach were in the range of 0.01 to 0.30 μg/kg under the optimum conditions. The average recoveries at three spiking levels were 84.9% to 105.2%, with relative standard deviations (RSDs) varying from 0.8% to 8.2% (n = 6). The developed method was successfully utilized for the screening and detection of fungicides in 81 fruit samples purchased from markets. A detailed survey was carried out about the concentration distribution, types of fungicides, and combined use of fungicides in different fruits. View Full-Text
Keywords: diethylenetriamine-functional magnetic core-shell polymer modified graphene oxide (DETA-MPs-GO); magnetic solid-phase extraction (MSPE); synergistic adsorption mechanism; ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS); fungicides diethylenetriamine-functional magnetic core-shell polymer modified graphene oxide (DETA-MPs-GO); magnetic solid-phase extraction (MSPE); synergistic adsorption mechanism; ultra-performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS); fungicides
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Ye, M.-L.; Zhu, Y. Simultaneous Determination and Investigation of Nine Fungicides in Fruits Using Diethylenetriamine-Functional Magnetic Core-Shell Polymer Modified Graphene Oxide as an Efficient Adsorbent Coupled to UPLC-HRMS. Int. J. Mol. Sci. 2017, 18, 2333.

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