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<p>Alpelisib, a selective PI3Kα inhibitor, benefits from reliable quantitative measurements to support exposure assessment and dose individualization. Here, we report a portable surface-enhanced Raman spectroscopy (SERS) workflow for rapid urinary screening and quantification of alpelisib using shaped-controlled silver nanoparticles, with silver nanorods selected as the substrate providing the highest SERS response among spherical, cubic, and rod-like morphologies. Key substrate-preparation and instrumental parameters were systematically optimized using a portable 785-nm Raman device, and the analytical figures of merit were thoroughly assessed in urine following a sample clean-up by protein precipitation and liquid–liquid extraction. Under optimized conditions, the diagnostic band at 993 cm⁻<sup>1</sup> was adopted for quantification, and the method provided a linear response from 7.93 to 113.26 µM (<i>R</i><sup>2</sup> = 0.9993), with limits of detection and quantification of 2.28 µM and 7.61 µM, respectively. Precision was suitable for a rapid SERS workflow (repeatability and reproducibility RSD ≤ 8.71% and ≤ 8.25%, respectively), with accuracy close to 100% across quality-control levels. A selectivity assessment was performed in urine using an equimolar alpelisib mixture with representative pharmaceutical interferents, and the method reliability was further supported by LC–MS benchmarking, with no statistically significant differences between SERS and LC–MS results for calibration and QC samples at the 95% confidence level (two-tailed <i>t</i>-test). An apparent enhancement factor up to 10<sup>3</sup> was estimated for the 993 cm⁻<sup>1</sup> band under the selected conditions, consistent with a predominantly electromagnetic enhancement mechanism with a plausible interfacial chemical contribution. Finally, method sustainability was discussed using the AGREE metric (overall score 0.74/1.00) as a diagnostic tool to identify improvement hotspots. Overall, this portable SERS approach provides a practical, low-instrumentation option for rapid urinary screening and quantification of alpelisib, complementary to LC–MS-based methods for comprehensive bioanalysis.</p> Graphical abstract <p></p>

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Screening-confirmation approach for urinary alpelisib by silver-nanorod enabled portable SERS platform and LC–MS validation

  • 期刊论文

  • 发表日期：

    2026年5月2日

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  • Claudia López-Sánchez,
  • Mohammed Zougagh,
  • Ángel Ríos,
  • Fernando de Andrés

摘要

Alpelisib, a selective PI3Kα inhibitor, benefits from reliable quantitative measurements to support exposure assessment and dose individualization. Here, we report a portable surface-enhanced Raman spectroscopy (SERS) workflow for rapid urinary screening and quantification of alpelisib using shaped-controlled silver nanoparticles, with silver nanorods selected as the substrate providing the highest SERS response among spherical, cubic, and rod-like morphologies. Key substrate-preparation and instrumental parameters were systematically optimized using a portable 785-nm Raman device, and the analytical figures of merit were thoroughly assessed in urine following a sample clean-up by protein precipitation and liquid–liquid extraction. Under optimized conditions, the diagnostic band at 993 cm⁻1 was adopted for quantification, and the method provided a linear response from 7.93 to 113.26 µM (R2 = 0.9993), with limits of detection and quantification of 2.28 µM and 7.61 µM, respectively. Precision was suitable for a rapid SERS workflow (repeatability and reproducibility RSD ≤ 8.71% and ≤ 8.25%, respectively), with accuracy close to 100% across quality-control levels. A selectivity assessment was performed in urine using an equimolar alpelisib mixture with representative pharmaceutical interferents, and the method reliability was further supported by LC–MS benchmarking, with no statistically significant differences between SERS and LC–MS results for calibration and QC samples at the 95% confidence level (two-tailed t-test). An apparent enhancement factor up to 103 was estimated for the 993 cm⁻1 band under the selected conditions, consistent with a predominantly electromagnetic enhancement mechanism with a plausible interfacial chemical contribution. Finally, method sustainability was discussed using the AGREE metric (overall score 0.74/1.00) as a diagnostic tool to identify improvement hotspots. Overall, this portable SERS approach provides a practical, low-instrumentation option for rapid urinary screening and quantification of alpelisib, complementary to LC–MS-based methods for comprehensive bioanalysis.

Graphical abstract