Rapid and Sensitive Detection of Psilocybin and Psilocin in Urine by Surface‐Enhanced Raman Spectroscopy

ABSTRACT Psilocybin, one of the primary active compounds in magic mushrooms, is metabolized into psilocin in the human body. In this study, we employed surface‐enhanced Raman spectroscopy (SERS), leveraging its unique molecular fingerprinting capabilities and high sensitivity, in combination with silver‐coated gold nanoparticles (Au@AgNPs) as the enhancement substrate (enhancement factor ~1.14 × 10 5 ), to detect psilocybin and psilocin in human urine samples. The method demonstrated remarkable sensitivity, with detection limits as low as 1.11 × 10 −10 mol·L −1 for psilocybin and 6.75 × 10 −12 mol·L −1 for psilocin. In real sample analysis, the total recovery rates for psilocybin and psilocin ranged from 80.79% to 109.53% and 83.98% to 106.78%, respectively, with relative standard deviations (RSDs) below 9%, indicating excellent accuracy and stability. By enabling rapid, accurate detection of psilocybin and psilocin at trace levels, this technique holds significant potential for practical use in drug enforcement, clinical toxicology, and future psychoactive substance surveillance.