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A Microfluidic Device to Realize Electrochemically Controlled SERS Detection in HPLC.

Maximilian E Blaha¹, Julius Schwieger¹, Rico Warias¹

¹Institute for Analytical Chemistry, Leipzig University, Linnéstraße 3, Leipzig 04103, Germany.

Analytical Chemistry

|June 23, 2025

Summary

This study introduces a novel, pressure-stable Surface-Enhanced Raman Spectroscopy (SERS) flow cell for High-Performance Liquid Chromatography (HPLC). This innovation enables real-time analysis of complex mixtures, overcoming previous limitations in sensitivity and signal carry-over.

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Area of Science:

Analytical Chemistry
Spectroscopy
Materials Science

Background:

Surface-enhanced Raman spectroscopy (SERS) offers high sensitivity for vibrational analysis but struggles with spectral overlap in complex mixtures.
Online coupling of SERS with separation techniques like High-Performance Liquid Chromatography (HPLC) is hindered by compatibility issues, leading to poor analyte interaction and signal artifacts.
Existing methods face challenges with irreversible analyte adsorption, signal carry-over, and low sensitivity in flow systems.

Purpose of the Study:

To develop the first HPLC-compatible, pressure-stable SERS flow cell for real-time, continuous flow analysis.
To enable online electrochemical SERS (EC-SERS) for enhanced analyte detection and substrate management.
To overcome limitations of traditional SERS in analyzing mixtures and improve sensitivity and substrate longevity.

Main Methods:

Fabrication of a monolithic, glass-based SERS flow cell using selective laser etching.
Integration of a silver-based SERS substrate and a counter electrode for electrochemical control.
Online coupling of the SERS flow cell with HPLC for real-time vibrational spectroscopy.

Main Results:

Demonstrated a pressure-stable, HPLC-compatible SERS flow cell for continuous flow analysis.
Utilized electrochemical control for on-demand substrate activation, enhancing signal intensity and eliminating memory effects.
Successfully analyzed model dyes and pharmaceutical compounds, showcasing broad applicability and improved detection capabilities.

Conclusions:

The developed glass-based SERS flow cell provides a robust platform for online HPLC-SERS analysis.
Electrochemical control significantly improves SERS performance, extending substrate lifetime and broadening detectable analytes.
This innovation facilitates the integration of SERS into high-throughput analytical workflows, offering a novel detection method.