摘要
Flavonoid-reduced gold electrode with SAM/Nafion improve detection performance. • Gold microneedle sensor enables real-time monitoring of HTL electro-synthesis. • Arduino-ADS realizes real-time digitization and intelligent regulation. • Closed-loop optimization for HTL electrolysis increases yield by 43.7%. Continuous monitoring of target reactants is essential for elucidating electrochemical system dynamics and enabling real-time measurement-control strategies in electrosynthesis. Herein, we report a flavonoid-reduced gold microneedle sensor with formed active Au sites for the electroreduction response toward carbonyl groups in homocysteine thiolactone (HTL), whereby current-concentration calibration curves are established to realize in-situ data acquisition and process control of HTL electrosynthesis. Plant flavonoid-mediated in-situ reduction enhances the dispersion and stability of gold nanoparticles on gold substrates. The synergistic combination of sulfhydryl-based self-assembled monolayers and a Nafion barrier effectively mitigates nonspecific adsorption, reducing background interference and improving signal-to-noise ratio and long-term stability for online monitoring in complex matrices. Integrated with an ADS1115 module, the sensor forms a closed-loop feedback system for real-time digital processing of concentration data and electrolysis parameter adjustment. The sensor exhibits a linear range of 1 μM to 5 mM, detection limit of 1.85 μM, sensitivity of 0.068 A/M, 94% long-term stability, and excellent reproducibility/repeatability, with only ±4% average deviation from HPLC measurements. In flow-through electrolysis, real-time current density optimization via this sensor increased HTL yield by 43.7% compared to conventional batch operation, providing a novel strategy for green and intelligent organic electrosynthesis. Download: Download high-res image (243KB) Download: Download full-size image
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