期刊
JOURNAL OF CHROMATOGRAPHY A
卷 1610, 期 -, 页码 -出版社
ELSEVIER
DOI: 10.1016/j.chroma.2019.460543
关键词
Core-shell nanocomposite; Sorbent; Magnetic solid-phase extraction; Sulfonamide antibiotics tandem mass spectrometry
资金
- National Key Research and Development Program of China [2018YFC1603500]
- National Natural Science Foundation of China [21804080]
- Natural Science Foundation of Shandong Province [ZR2017MB011]
- Key R&D Program of Shandong Province [2019GSF111009, 2019GSF111001]
- Youth Science Funds of Shandong Academy of Sciences [2019QN008, 2019QN009]
- Qilu University of Technology (Shandong Academy of Science) Joint Research Fund for Young PHSs [2018BSHZ0029]
A molybdenum disulfide(MoS2)-based core-shell magnetic nanocomposite (Fe3O4@MoS2) was synthesized by the stepwise hydrothermal method. Two-dimension ultrathin MoS2 sheets with a thickness of approximately 20 nm were grown in situ on the surface of Fe3O4 (similar to 200 nm). They were employed as an adsorbent for the magnetic solid-phase extraction (MSPE) of sulfonamide antibiotics (SAs) from water samples. High-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was used for SA quantitation. Extraction parameters, including the pH effect, amount of Fe3O4@MoS2, extraction time, temperature, and desorption conditions, were systematically investigated, The electrostatic interaction between the positively charged SAs and negatively charged MoS2 nanoparticles in the optimal extraction conditions enhanced the adsorption of SAs on the sorbent surface. Under chosen conditions, the proposed strategy achieved wide linear range of 1.0-1000 ng.L-1 SAs, low limits of detection (LOD, 0.20-1.15 ng.L-1, S/N=3:1), good trueness (recoveries between 85.50-111.5%), satisfactory repeatability and reproducibility (relative standard deviation, <10%, n=5), and excellent recoveries between 80.20% and 108.6% for SAs determination in spiked waste water samples. The proposed strategy was validated and successfully applied for the analysis of water, milk, pork meat and fish meat. The nanocomposites, which have the combined advantages of magnetic separation and high adsorption affinity toward SAs, are a promising sorbent for antibiotics extraction from real samples. (C) 2019 Elsevier B.V. All rights reserved.
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