ROXY™ Exceed Electrochemistry System for EC-MS

Importance of Topic

The majority of organic compounds undergo redox processes in biological and environmental contexts. Electrochemistry coupled to mass spectrometry (EC–MS) enables rapid, enzyme-free simulation of oxidation and reduction pathways, accelerating metabolite prediction, degradation studies and structural analysis without biological matrix complexities.

Study Objectives and Overview

This study introduces the ROXY™ Exceed electrochemistry system designed for seamless online and offline EC–MS integration. Key goals include fast generation of drug metabolites and degradants, efficient protein disulfide bond reduction, environmental pollutant transformation, and small-scale electrosynthesis of reference materials.

Methodology and Instrumentation

The ROXY Exceed potentiostat offers a ±4.9 V voltage range and 1 nA–100 mA current capability across four operating modes: DC, Scan, Pulse and Pulse2. It interfaces with any LC-MS or direct infusion setup under Dialogue or Chromeleon control. Four specialized flow cells support diverse applications:

• ReactorCell: thin-layer cell (1–20 µL/min) with Pt, Au, GC and BDD electrodes for rapid redox reactions without carry-over.
• μ-PrepCell™ 2.0: high-yield cell (20–100 µL/min) with tenfold larger electrode area for efficient metabolite and intermediate formation.
• μ-PrepCell™ SS: dual electrode configuration for reagent-free, high-pressure (up to 500 bar) reduction of protein disulfide bonds, ideal for HDX-MS and proteomics.
• SynthesisCell: batch reactor (up to 60 mL) with large surface electrodes for mg-scale electrosynthesis of metabolites and degradants.

Main Results and Discussion

Performance evaluations demonstrate:

• Instantaneous generation of oxidative drug metabolites mimicking CYP450 transformations, with clear MS voltammograms.
• Superior MS sequence coverage in proteomic workflows via online disulfide bond reduction at optimized pulse potentials.
• Accurate simulation of environmental degradation pathways and reactive intermediates not accessible from natural samples.
• Rapid, green forced-degradation of APIs and excipients under controlled redox stress conditions.
• Scalable electrosynthesis yielding milligram quantities of reference compounds within an hour.

Benefits and Practical Applications

EC–MS with ROXY Exceed offers major advantages:

• Time and cost savings by eliminating enzymes and lengthy chemical syntheses.
• Matrix-free analyses for cleaner spectra and reliable product identification.
• Flexibility to integrate with LC-MS, HDX-MS, proteomics and environmental screening.
• Scalable workflows from analytical screening to preparative electrosynthesis.

Future Trends and Opportunities

Emerging directions include integration with high-throughput screening platforms, AI-driven optimization of redox conditions, development of novel electrode materials, advanced multi-step pulse algorithms, and automated scale-up for industrial electrosynthesis.

Conclusion

The ROXY Exceed EC–MS system provides a robust, versatile tool for rapid redox reaction simulation across drug discovery, proteomics, environmental chemistry and synthesis, enabling cleaner, faster and more cost-effective workflows.

Reference

EP 2572188 B1, EP 2706066 A1