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<p>Benzo[a]pyrene (BaP) is the sole polycyclic aromatic hydrocarbon (PAH) classified as carcinogenic to humans and is widely used as a PAH contamination marker in food and beverages, including distilled spirits such as cachaça. Despite the recognized contamination risk, electroanalytical methods for BaP determination in cachaça or other distilled spirits have not been previously reported. This work proposes a surfactant-assisted adsorptive stripping square-wave voltammetric method for BaP determination at a carbon paste electrode modified with an electrodeposited gold film. The method was optimized using a Taguchi robust experimental design, which maximized the BaP oxidation peak current while minimizing its sensitivity to experimental variability. The optimized procedure requires no sample pretreatment, a complete standard-addition determination taking approximately 40&#xa0;min. Under the selected conditions—a 1:1 BR buffer (pH 4.0)/acetonitrile medium, 0.05% sodium dodecyl sulfate (SDS), and a 600&#xa0;s open-circuit preconcentration step—the method exhibited a linear range of 14–175&#xa0;µg L<sup>−1</sup>, with limits of detection and quantification of 4.3&#xa0;µg L<sup>−1</sup> and 14&#xa0;µg L<sup>−1</sup>, respectively. BaP was not detected in the unfortified commercial cachaça samples. Trueness was assessed by standard addition, with apparent recoveries of 100–110%. The voltammetric results agreed with those of an independent spectrofluorimetric reference method based on second-order multivariate calibration (PARAFAC), with no significant difference (paired <i>t</i>-test, <i>p</i> ≈ 0.09; mean difference 5.5&#xa0;µg L<sup>−1</sup>), supporting method accuracy. The proposed approach provides a practical and accessible screening tool for BaP in distilled spirits.</p>

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Surfactant-assisted Adsorptive Stripping Square-wave Voltammetric Determination of Benzo[a]pyrene in Cachaça Using a Gold-modified Carbon Paste Electrode Optimized by Taguchi Robust Design

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年7月8日

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  • Flávia Rhuana Pereira Sales,
  • Ingrid Gabriela Bezerra de Lima Cruz,
  • Wallace Duarte Fragoso,
  • Sherlan Guimarães Lemos

摘要

Benzo[a]pyrene (BaP) is the sole polycyclic aromatic hydrocarbon (PAH) classified as carcinogenic to humans and is widely used as a PAH contamination marker in food and beverages, including distilled spirits such as cachaça. Despite the recognized contamination risk, electroanalytical methods for BaP determination in cachaça or other distilled spirits have not been previously reported. This work proposes a surfactant-assisted adsorptive stripping square-wave voltammetric method for BaP determination at a carbon paste electrode modified with an electrodeposited gold film. The method was optimized using a Taguchi robust experimental design, which maximized the BaP oxidation peak current while minimizing its sensitivity to experimental variability. The optimized procedure requires no sample pretreatment, a complete standard-addition determination taking approximately 40 min. Under the selected conditions—a 1:1 BR buffer (pH 4.0)/acetonitrile medium, 0.05% sodium dodecyl sulfate (SDS), and a 600 s open-circuit preconcentration step—the method exhibited a linear range of 14–175 µg L−1, with limits of detection and quantification of 4.3 µg L−1 and 14 µg L−1, respectively. BaP was not detected in the unfortified commercial cachaça samples. Trueness was assessed by standard addition, with apparent recoveries of 100–110%. The voltammetric results agreed with those of an independent spectrofluorimetric reference method based on second-order multivariate calibration (PARAFAC), with no significant difference (paired t-test, p ≈ 0.09; mean difference 5.5 µg L−1), supporting method accuracy. The proposed approach provides a practical and accessible screening tool for BaP in distilled spirits.