Abstract
Conventional monitoring of metal ions in edible vegetable oils is crucial for assessing the quality and safety of consumers. In the current study, we developed a magnetic effervescence–enhanced emulsification microextraction (MEEM-DM) based on the employment of effervescent tablets composed of dicationic ionic liquids (DILs), MFe2O4 nanoparticles, and acidic and alkaline sources. The MEEM-DM pre-treatment was combined with inductively coupled plasma mass spectrometry (ICP-MS) analysis for trace-level detection of Cr(VI) and Cu(II) in ten types of edible oil. It realized efficient preconcentration/extraction by DILs, vigorous dispersion by effervescent reaction, and rapid separation/collection by MFe2O4 in one synchronous step. As the DIL ([Cn(MIM)2]Br2) possesses two active centers, it provided superior adsorption/extraction performance for metal ions when compared with its corresponding monocationic form ([Cn(MIM)]Br). Four types of MFe2O4 were synthesized and characterized, in which NiFe2O4 nanoparticles presented a larger specific surface area and smaller particle diameter than others. The optimized parameters for ICP-MS were as follows: flow rate of carrier gas, 1.15 L/min, and ICP ratio frequency power, 1550 W. The optimized MEEM-DM conditions were as follows: 0.46 g Na2CO3, 60 mg [C4(MIM)2]Br2, 45 mg Na[N(CN)2], 10 mg NiFe2O4, 0.58 g for each tablet, and 0.50 M HCl solution. The newly developed method gave satisfactory detection limits (0.076–0.086 μg/kg) and recoveries (96.9–105.8%) for Cr(VI) and Cu(II) that were comparable with conventional ultrasound-assisted extraction and microwave-assisted acid-digestion methods. These superior performance metrics show an additive extraction action between DILs and MFe2O4 in an effervescent reaction–enhanced microextraction and great potential in the conventional monitoring of heavy metals in edible oil samples.
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Acknowledgements
The authors also thank the support by the Key Discipline of Zhejiang Province in Medical Technology (First Class, Category A).
Funding
This work was jointly supported by the Wenzhou Municipal Science and Technology Bureau (Y20210086), the National Innovation and Entrepreneurship Training Program for College Students (202210343004), Science and Technology Innovation Program of Zhejiang Province College Students and the Sprout Talents Plan (2022R413A004), and Jiangsu Provincial Key Research & Development Program (BE2022733).
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Jia Wu: overall design; writing—original draft; writing—review and editing; Shuning Lan: preparation and characterization of the METs; Jiaju Sun and Hui She: optimization of the MEEM-DM procedures. Gang Wang and Xingfu Wen: validation of method performance; Shanle Zhou and Bingxia Ying: sample collection and detection; Xuedong Wang: management and supervision of experiment process; Huili Wang: methodology, writing—review and editing.
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Jia Wu declares no conflict of interest. Shuning Lan declares no conflict of interest. Jiaju Sun declares no conflict of interest. Hui She declares no conflict of interest. Gang Wang declares no conflict of interest. Xingfu Wen declares no conflict of interest. Shanle Zhou declares no conflict of interest. Bingxia Ying declares no conflict of interest. Xuedong Wang declares no conflict of interest. Huili Wang declares no conflict of interest.
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Wu, J., Lan, S., Sun, J. et al. Trace-Level Detection of Cr(VI) and Cu(II) in Edible Vegetable Oils Using Dicationic Ionic Liquids and MFe2O4-Based Effervescence-Enhanced Emulsification Microextraction Followed by ICP-MS Analysis. Food Anal. Methods 16, 1655–1672 (2023). https://doi.org/10.1007/s12161-023-02528-y
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DOI: https://doi.org/10.1007/s12161-023-02528-y