<p>A simple and centrifugation-free method was developed by implementing a magnetic deep eutectic solvent (MDES) in the vortex-assisted liquid–liquid microextraction (VA-LLME) technique for the separation and determination of inorganic and organic Hg species in beverage samples. The Hg(II) ion was complexed with ammonium diethyldithiophosphate (DDTP) and extracted in 100 µL of MDES composed of lauric acid:decanoic acid:dysprosium(III) chloride (LA:DA:DyCl<sub>3</sub>; 2:1:0.1 molar ratio). The extraction phase was dispersed using vortex stirring for 2&#xa0;min and then separated without centrifugation and by the assistance of an external magnet, followed by back-extraction with concentrated HNO<sub>3</sub> and determination of Hg by cold vapor atomic fluorescence spectrometry (CV-AFS). Total Hg was determined by CV-AFS after photo-oxidation of organic species, and total organic Hg species concentration was obtained by subtracting total inorganic Hg from total Hg. Different experimental variables were optimized using response surface methodology, yielding a maximum extraction efficiency of 97.5% for Hg(II). The method exhibited adequate analytical performance, with a relative standard deviation of 2.6%, limits of detection and quantification of 0.12 and 0.36&#xa0;µg L<sup>−1</sup> Hg, respectively, and a linear range between 0.36 and 4&#xa0;µg L<sup>−1</sup> Hg. The developed methodology was applied to the determination of inorganic and organic Hg species in tap water, mineral water, apple juice, and white wine.</p>

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Centrifugation-Free Magnetic Deep Eutectic Solvent Liquid–Liquid Microextraction Combined with Cold Vapor Atomic Fluorescence Spectrometry for Hg Speciation in Beverages

  • Aldana A. Lemos,
  • Rodolfo G. Wuilloud

摘要

A simple and centrifugation-free method was developed by implementing a magnetic deep eutectic solvent (MDES) in the vortex-assisted liquid–liquid microextraction (VA-LLME) technique for the separation and determination of inorganic and organic Hg species in beverage samples. The Hg(II) ion was complexed with ammonium diethyldithiophosphate (DDTP) and extracted in 100 µL of MDES composed of lauric acid:decanoic acid:dysprosium(III) chloride (LA:DA:DyCl3; 2:1:0.1 molar ratio). The extraction phase was dispersed using vortex stirring for 2 min and then separated without centrifugation and by the assistance of an external magnet, followed by back-extraction with concentrated HNO3 and determination of Hg by cold vapor atomic fluorescence spectrometry (CV-AFS). Total Hg was determined by CV-AFS after photo-oxidation of organic species, and total organic Hg species concentration was obtained by subtracting total inorganic Hg from total Hg. Different experimental variables were optimized using response surface methodology, yielding a maximum extraction efficiency of 97.5% for Hg(II). The method exhibited adequate analytical performance, with a relative standard deviation of 2.6%, limits of detection and quantification of 0.12 and 0.36 µg L−1 Hg, respectively, and a linear range between 0.36 and 4 µg L−1 Hg. The developed methodology was applied to the determination of inorganic and organic Hg species in tap water, mineral water, apple juice, and white wine.