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<p> A&#xa0;solid-phase microextraction-SERS (SPME-SERS) analysis system&#xa0;was enhanced by the synergistic integration of azo reaction and electroextraction (Azo/EEx/SPME-SERS) to directly determine aromatic amines in serum and urine. Azo reactions selectively converted aromatic amines (e.g., aniline) into positively charged derivatives, which were selectively absorbed onto a rough silver SERS substrate via charge-selective electroextraction (- 0.2&#xa0;V), excluding anionic interferents. Electroextraction-accelerated mass transfer and real-time SERS detection enabled rapid preconcentration and spectral acquisition under 3&#xa0;min. The azo reaction increased the Raman scattering cross-section of aniline, and electroextraction reduced the distance of azo aniline to the SERS hot spots. This enabled low detection limits (aniline, 0.005&#xa0;µg·mL<sup>−1</sup>). The Azo/EEx/SPME-SERS method achieved dual-dimensional interference exclusion through chemical derivatization (azo reaction) and physical charge-selective electroextraction, granting aromatic amines competitive adsorption advantage over serum metabolites at SERS hotspots. This synergy allows for the direct detemination of aniline in urine/serum with only 5–10&#xa0;fold dilutions. It avoids the need for tedious pretreatments, while maintaining recoveries of 92–107%, accuracy of 97.33%&#xa0;(urine) and 94.89% (serum), and method detection limits of 0.05&#xa0;µg·mL<sup>−1</sup> (urine) and 0.5&#xa0;µg·mL<sup>−1</sup> (serum).</p> Graphical Abstract <p></p>

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Synergistic azo reaction and electroextraction in SPME-SERS for direct determination of aromatic amines in biofluids with minimal matrix interference

  • 期刊论文

  • 发表日期：

    2025年7月8日

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  • Yadi Liu,
  • Shu Li,
  • Xinyuan Guo,
  • Tong Wang,
  • Dawei Yang,
  • Jinhua Zhan,
  • Jing Chen

摘要

A solid-phase microextraction-SERS (SPME-SERS) analysis system was enhanced by the synergistic integration of azo reaction and electroextraction (Azo/EEx/SPME-SERS) to directly determine aromatic amines in serum and urine. Azo reactions selectively converted aromatic amines (e.g., aniline) into positively charged derivatives, which were selectively absorbed onto a rough silver SERS substrate via charge-selective electroextraction (- 0.2 V), excluding anionic interferents. Electroextraction-accelerated mass transfer and real-time SERS detection enabled rapid preconcentration and spectral acquisition under 3 min. The azo reaction increased the Raman scattering cross-section of aniline, and electroextraction reduced the distance of azo aniline to the SERS hot spots. This enabled low detection limits (aniline, 0.005 µg·mL−1). The Azo/EEx/SPME-SERS method achieved dual-dimensional interference exclusion through chemical derivatization (azo reaction) and physical charge-selective electroextraction, granting aromatic amines competitive adsorption advantage over serum metabolites at SERS hotspots. This synergy allows for the direct detemination of aniline in urine/serum with only 5–10 fold dilutions. It avoids the need for tedious pretreatments, while maintaining recoveries of 92–107%, accuracy of 97.33% (urine) and 94.89% (serum), and method detection limits of 0.05 µg·mL−1 (urine) and 0.5 µg·mL−1 (serum).

Graphical Abstract