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Determination of benzoylecgonine in synthetic urine samples via square-wave voltammetry with boron-doped diamond electrode

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Abstract

This study describes the development of an electroanalytical methodology using square-wave voltammetry (SWV) to quantify benzoylecgonine (BE) in synthetic urine samples using a boron-doped diamond electrode. Due to the oxidation of the tertiary amine present in the tropane group, it was possible to observe an irreversible oxidation process, with a maximum oxidation peak around + 2.10 V, in an acidic medium. Initially, the design of experiments (DoE) was applied to optimize the SWV parameters using a central composite design. All DoE analyses occur in a solution of H2SO4 0.5 mol L−1 as a supporting electrolyte and a fixed concentration of 0.20 mmol L−1 of BE; the optimal parameters found were 6.023 mV for step potential, 87.045 mV for modulation amplitude, and 30.795 Hz for frequency. Performance characteristics were obtained after constructing the analytical curve, including a limit of detection of 1.20 μmol L−1, and a limit of quantification of 4.0 μmol L−1 within a linear working range from 4.93 to 154.20 μmol L−1, and a R2 of 99.76%. BE analysis was performed on a solution containing different proportions of synthetic urine and H2SO4, specifically 9:1, 6:4, and 3:7 (v/v) of acid and synthetic urine, respectively. Nevertheless, it was not possible to conduct a standard recovery test in ratios higher than 9:1 (v/v) of urine to acid due to a lack of response. In conclusion, this methodology offers a reliable approach for determining BE, an important analyte in forensic chemistry, and the DoE allows a comprehensive analysis of the performance parameters of the technique used.

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Acknowledgements

The authors thank the Nucleus of Petroleum Chemistry Competencies (NCQP), Coordination for the Improvement of Higher Education Personnel (Capes), National Council for Scientific and Technological Development (CNPq), and Federal University of Espírito Santo (Ufes) for their technical and financial support, Petroleomics and Forensic laboratory for supplying the BE standard, and Civil Police of Espírito Santo (PC-ES, Brazil), cooperation agreement process No. 23068.022157/2020-69, for providing the forensic samples.

Funding

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior, 001, Conselho Nacional de Desenvolvimento Científico e Tecnológico.

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Authors and Affiliations

  1. Department of Chemistry, Federal University of Espírito Santo, 29075-910, Vitória, ES, Brazil

    Sidnei B. Gomes Junior, Nathália S. Conceição, Gabriel F. S. dos Santos, José Guilherme A. Rodrigues, Wanderson Romão & Rafael Q. Ferreira

  2. Federal Institute of Espírito Santo, Vila Velha, 29106-010, Vitória, ES, Brazil

    Wanderson Romão

  3. National Institute of Forensic Science and Technology, 29106-010, Vila Velha, ES, Brazil

    Nathália S. Conceição & Wanderson Romão

Authors
  1. Sidnei B. Gomes Junior
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  2. Nathália S. Conceição
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  3. Gabriel F. S. dos Santos
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  4. José Guilherme A. Rodrigues
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  5. Wanderson Romão
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  6. Rafael Q. Ferreira
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Contributions

Sidnei B. Gomes, Junior: conceptualization, formal analysis, visualization, investigation, data curation, writing—original draft, and methodology; Gabriel F. S. dos Santos: methodology, formal analysis, and writing—review and editing; José G. A. Rodrigues: formal analysis; Nathalia S. Conceição: investigation and visualization; Wanderson Romão: resources; Rafael Q. Ferreira: supervision, and writing—review and editing.

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Correspondence to Rafael Q. Ferreira.

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Gomes Junior, S.B., Conceição, N.S., dos Santos, G.F.S. et al. Determination of benzoylecgonine in synthetic urine samples via square-wave voltammetry with boron-doped diamond electrode. J Solid State Electrochem (2024). https://doi.org/10.1007/s10008-024-05922-6

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  • DOI: https://doi.org/10.1007/s10008-024-05922-6

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