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<p>The objective of the present work was to develop and optimize portable, lab-made screen-printed electrodes (SPEs) modified with manganese dioxide nanoparticles (MnO<sub>2</sub> Nps) anchored on carbon black (CB) nanostructures (SPE/CB/MnO<sub>2</sub>), to determine TBHQ in edible oils and canned food as matrices. First, an ecofriendly straightforward synthesis was developed to produce a novel nanocomposite CB/MnO<sub>2</sub> Nps. Afterwards several techniques were used to demonstrate the strong chemical synergy of the novel disposable electrochemical device, and the excellent electrochemical performance during the direct oxidation of TBHQ. Based on the present results, SEM analysis showed the characteristic carbon structure of CB powder and detailed the morphology of new CB/MnO<sub>2</sub> nanocomposites. EDS of the selected area indicated 96.2% atomic C and 18.7% atomic O in the CB sample. Also, EDS analysis of the delimitated region of the CB/MnO<sub>2</sub> material, displayed that a total content of manganese was 4.5%. FTIR spectra of the CB/MnO<sub>2</sub> nanocomposite showed peaks from 1733 to 1645&#xa0;cm<sup>−1</sup>, indicating COOH groups. Unique peaks at 765, 744, 710, and 675&#xa0;cm<sup>−1</sup> were attributed to MnO<sub>2</sub> Nps in the newly developed material. Due to its higher electrochemical response regarding the oxidation of TBHQ, differential pulse voltammetry (DPV) was the electrochemical technique chosen for the development of the newly proposed electrochemical method. Optimization experiments were carried out to improve the analytical signal for TBHQ. The results demonstrated that applying a step potential of 5&#xa0;mV yielded an elevated peak potential. Additionally, setting the pulse amplitude to 100&#xa0;mV significantly enhanced the peak current of the target analyte. Optimal peak definition and baseline delimitation were achieved with time modulation at a period of 40&#xa0;ms, resulting in superior resolution. The newly developed sensor exhibited a linear range of 0.46 to 33.0&#xa0;μmol L<sup>−1</sup> and a limit of detection of 0.1&#xa0;µmol L<sup>−1</sup> for TBHQ. Recovery rate of TBHQ in food matrices ranged from 99.6 to 104%. Studies on possible interferents regarding the analytical signal of TBHQ showed no significant signal variation among all possible interferents. Finally, the sensor exhibited excellent repeatability and reproducibility, with relative standard deviations (RSD) of 4.4% and 4.5%, respectively. These results demonstrate an effective, simple method for producing a disposable, inexpensive, and sensitive electrochemical sensor to detect low TBHQ levels in complex food samples; with the possibility to be applied in industry facilities.</p> Graphical Abstract <p></p>

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Edible Oils and Canned Food as Matrices for Rapid Sensing of Tert-butylhydroquinone using Screen-Printed Electrode Modified with Manganese Dioxide Nanoparticles Anchored on a Carbon Black

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年6月3日

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  • Claudio Sabbatini Capella Lopes,
  • Ruan Esteves da Silva Domingues Arneiro,
  • Francisco Walison Lima Silva,
  • Julia Oliveira Fernandes,
  • Cassiano Augusto Rolim Bernardino,
  • Claudio Fernando Mahler,
  • Ricardo Pinheiro dos Santos Filho,
  • Lucas Renan Benincasa Pinheiro,
  • Rodrigo José Corrêa,
  • Emerson Schwingel Ribeiro,
  • Ricardo Erthal Santelli,
  • Fernando Henrique Cincotto

摘要

The objective of the present work was to develop and optimize portable, lab-made screen-printed electrodes (SPEs) modified with manganese dioxide nanoparticles (MnO2 Nps) anchored on carbon black (CB) nanostructures (SPE/CB/MnO2), to determine TBHQ in edible oils and canned food as matrices. First, an ecofriendly straightforward synthesis was developed to produce a novel nanocomposite CB/MnO2 Nps. Afterwards several techniques were used to demonstrate the strong chemical synergy of the novel disposable electrochemical device, and the excellent electrochemical performance during the direct oxidation of TBHQ. Based on the present results, SEM analysis showed the characteristic carbon structure of CB powder and detailed the morphology of new CB/MnO2 nanocomposites. EDS of the selected area indicated 96.2% atomic C and 18.7% atomic O in the CB sample. Also, EDS analysis of the delimitated region of the CB/MnO2 material, displayed that a total content of manganese was 4.5%. FTIR spectra of the CB/MnO2 nanocomposite showed peaks from 1733 to 1645 cm−1, indicating COOH groups. Unique peaks at 765, 744, 710, and 675 cm−1 were attributed to MnO2 Nps in the newly developed material. Due to its higher electrochemical response regarding the oxidation of TBHQ, differential pulse voltammetry (DPV) was the electrochemical technique chosen for the development of the newly proposed electrochemical method. Optimization experiments were carried out to improve the analytical signal for TBHQ. The results demonstrated that applying a step potential of 5 mV yielded an elevated peak potential. Additionally, setting the pulse amplitude to 100 mV significantly enhanced the peak current of the target analyte. Optimal peak definition and baseline delimitation were achieved with time modulation at a period of 40 ms, resulting in superior resolution. The newly developed sensor exhibited a linear range of 0.46 to 33.0 μmol L−1 and a limit of detection of 0.1 µmol L−1 for TBHQ. Recovery rate of TBHQ in food matrices ranged from 99.6 to 104%. Studies on possible interferents regarding the analytical signal of TBHQ showed no significant signal variation among all possible interferents. Finally, the sensor exhibited excellent repeatability and reproducibility, with relative standard deviations (RSD) of 4.4% and 4.5%, respectively. These results demonstrate an effective, simple method for producing a disposable, inexpensive, and sensitive electrochemical sensor to detect low TBHQ levels in complex food samples; with the possibility to be applied in industry facilities.

Graphical Abstract