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Microwave-Assisted Preparation of Zirconium Intercalated Expanded Graphite for Chlorpyrifos Determination in Honey

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Abstract

Herein, we proposed a simple and efficient microwave-assisted preparation method for the fabrication of zirconium (IV) intercalated expanded graphite (Zr-EG). The synthetic approach could be completed in one step within 20 s, where KMnO4 was used as the oxidizing agent, H2SO4 and ZrOCl2 as the intercalating agents. The as-prepared Zr-EG exhibited thin multi-layered structure, plenty of small Zr-relevant particles and oxygenated groups in both layers and surface, which gave Zr-EG high absorption capability. Subsequently, the Zr-EG, as a new kind of solid-phase extraction absorbent, was applied to the separation, purification and enrichment of chlorpyrifos in honey samples, followed by high-performance liquid chromatography analysis. Under optimal extraction and analysis conditions, the detection limit was 100 ng g−1. The relative standard deviations ranged from 2.6 to 6.8%. At three spiked levels (1, 10, 100 μg g−1), the recoveries of chlorpyrifos were in the range of 86.1–92.2%. Comparison with other conventional solid-phase extraction adsorbents, modified EG showed rapid synthesis, layered modification flexibility, stable structure, large adsorption capacity and good selectivity, demonstrating great potential in pollutants separation and detection.

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Acknowledgements

This work is supported by National Natural Science Foundation of China, China (NSFC, No. 21804017), the China Postdoctoral Science Foundation, China (No. 2019M651242), the Heilongjiang Postdoctoral Science Foundation funded project, China (No. LBH-Z18009).

Funding

This study was funded by National Natural Science Foundation of China (NSFC, No. 21804017), the China Postdoctoral Science Foundation (No. 2019M651242), the Heilongjiang Postdoctoral Science Foundation funded project (No. LBH-Z18009).

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Authors and Affiliations

  1. Department of Chemistry, Chemical Engineering and Resource Utilization, Northeast Forestry University, 26 Hexing Road, Harbin, 150040, People’s Republic of China

    Juan Hou, Xu Gao, Zhaoyu Yang, Jing Qin, Yongqi Li & Bin Li

  2. Post-Doctoral Mobile Research Station of Forestry Engineering, Northeast Forestry University, Harbin, 150040, People’s Republic of China

    Juan Hou & Bin Li

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  1. Juan Hou
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  2. Xu Gao
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  3. Zhaoyu Yang
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  4. Jing Qin
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  5. Yongqi Li
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  6. Bin Li
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Correspondence to Bin Li.

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Hou, J., Gao, X., Yang, Z. et al. Microwave-Assisted Preparation of Zirconium Intercalated Expanded Graphite for Chlorpyrifos Determination in Honey. Chromatographia 84, 117–125 (2021). https://doi.org/10.1007/s10337-020-03992-y

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