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Green Electroanalytical Method for Fast Measurement of Xanthine Oxidase Inhibitor Febuxostat

At a Glance

Section titled “At a Glance”
MetadataDetails
Publication Date2017-11-01
JournalAnalytical Sciences
AuthorsBiljana Nigović, Ivona Milanović
InstitutionsUniversity of Zagreb
Citations12
AnalysisFull AI Review Included

Technical Documentation & Analysis: Green Electroanalytical Method for Febuxostat using BDDE

Section titled “Technical Documentation & Analysis: Green Electroanalytical Method for Febuxostat using BDDE”

Executive Summary

Section titled “Executive Summary”

This document analyzes the research demonstrating a highly efficient, fast, and environmentally “green” electroanalytical method for quantifying Febuxostat (FBX) using an unmodified Boron-Doped Diamond Electrode (BDDE). The findings validate BDDE as the premier platform for high-sensitivity pharmaceutical quality control and clinical analysis.

  • Core Achievement: Development of a simple, rapid square-wave voltammetric (SWV) method for FBX detection, avoiding toxic solvents and complex electrode modifications.
  • Speed and Efficiency: The analytical SWV scan requires only 0.66 s, enabling extremely high-throughput analysis ideal for pharmaceutical quality control (QC).
  • High Sensitivity: Achieved a low detection limit (LOD) of $9.5 \times 10^{-8}$ M, comparable to advanced chromatographic methods.
  • Material Validation: Confirms the exceptional electrochemical stability, low fouling resistance, and wide potential window of the BDDE.
  • Pharmaceutical Relevance: Demonstrated quantitative determination of FBX in film-coated tablets with excellent recovery (99.6%).
  • Future Potential: The distinct oxidation potentials of FBX (+1.38 V) and uric acid (+0.64 V) open possibilities for simultaneous clinical analysis using 6CCVD’s custom BDD materials.

Technical Specifications

Section titled “Technical Specifications”

The following key data points were extracted from the study detailing the performance and parameters of the BDDE in FBX analysis:

ParameterValueUnitContext
Detection Limit (LOD)9.5 x 10-8MCalculated based on $3s/a$ criterion.
Quantitation Limit (LOQ)2.9 x 10-7MCalculated based on $10s/a$ criterion.
Linear Concentration Range7.5 x 10-7 - 2.0 x 10-5MRange achieved in BR buffer pH 5.
Oxidation Peak Potential (FBX)+1.38Vvs. Ag/AgCl reference electrode.
Oxidation Peak Potential (Uric Acid)+0.64VAllows for potential simultaneous detection.
Tablet Recovery (FBX)99.6%Excellent recovery obtained by standard addition method.
Relative Standard Deviation (RSD)±1.4%For replicate measurements of peak current.
Electrode TypeBoron-Doped Diamond (BDDE)N/AUnmodified, O-terminated surface.
Electrode Diameter3mmWorking electrode size used in the three-electrode cell.
SWV Scan Time0.66sExtremely fast analysis time due to high pulse frequency.
SWV Frequency300HzOptimized for highest sensitivity.
SWV Pulse Amplitude50mVOptimal setting for square-wave voltammetry.

Key Methodologies

Section titled “Key Methodologies”

The experiment utilized highly controlled MPCVD diamond material combined with specific electrochemical preparation steps to achieve optimal results.

  1. Electrode Preparation:
    • The 3-mm BDDE disc was cleaned by rinsing with deionized water and gently rubbing on filter paper until a mirror-like surface was observed.
  2. Anodic Activation (Surface Termination):
    • The BDDE was intentionally converted to a predominantly O-terminated surface by applying +2 V for 90 s in 0.5 M H2SO4.
  3. Electrolyte Optimization:
    • Britton-Robinson (BR) buffer at pH 5 was selected, yielding the best defined peak shape and the highest current sensitivity, avoiding the use of toxic organic solvents (e.g., methanol) required by previous methods.
  4. Voltammetric Technique:
    • Square-wave voltammetry (SWV) was chosen over Cyclic Voltammetry (CV) for its higher sensitivity and speed.
    • Optimized parameters included 300 Hz frequency, 50 mV pulse amplitude, and 4 mV scan increment, ensuring rapid, high-resolution data acquisition.
  5. Reaction Mechanism Confirmation:
    • Cyclic voltammetry confirmed that the oxidation of FBX is an irreversible, diffusion-controlled process (indicated by the linear relationship between peak current and the square root of the scan rate).

6CCVD Solutions & Capabilities

Section titled “6CCVD Solutions & Capabilities”

This study confirms the necessity of high-quality, customized Boron-Doped Diamond for advanced electroanalytical applications. 6CCVD is uniquely positioned to supply the materials required to replicate, scale, and extend this critical research.

Applicable Materials

Section titled “Applicable Materials”

To replicate and industrialize the high-performance green electrochemistry demonstrated, researchers and engineers require the following:

Material SpecificationApplication Requirement6CCVD Advantage
Heavy Boron Doped Diamond (BDD)The core working electrode material, requiring high conductivity and stable background current.6CCVD offers BDD thin films and substrates with optimized boron doping uniformity for superior electrochemical performance and low resistivity.
Polycrystalline Diamond (PCD) WafersNeeded to process large areas or numerous small electrodes efficiently.We provide PCD wafers up to 125 mm in diameter, offering scalable manufacturing solutions for BDDE arrays.
Polishing RequirementsThe BDDE requires a mirror-like, stable surface for reproducibility and low fouling.6CCVD guarantees ultra-smooth surfaces with polishing capabilities down to Ra < 5 nm for inch-size PCD/BDD wafers.

Customization Potential

Section titled “Customization Potential”

The experimental setup relied on a specific 3-mm diameter BDDE disc. 6CCVD specializes in delivering application-ready customized dimensions and configurations:

  • Custom Dimensions: While the paper used a 3 mm disc, 6CCVD can supply wafers up to 125 mm, or custom laser-cut/machined pieces down to millimeter scale, precisely matching specific cell designs.
  • Controlled Doping and Termination: We provide BDD materials with controlled doping profiles. We can also assist researchers targeting specific surface chemistries (e.g., achieving the O-terminated surface via post-deposition processing).
  • Metalization Services: Although this study used a simple three-electrode system, for complex microsensors or integrated devices, 6CCVD offers in-house metalization (Au, Pt, Ti, W, Cu) for contact pads and interconnection layers.

Engineering Support

Section titled “Engineering Support”

The BDDE’s ability to simultaneously analyze FBX and uric acid—compounds with vastly different oxidation potentials—is a significant finding for clinical diagnostics.

6CCVD’s in-house PhD engineering team is available to assist with material selection and design optimization for similar clinical electroanalytical sensing projects. We ensure the delivered material properties (doping density, thickness, surface finish) are perfectly matched to the required detection limits and operational environment (e.g., pH stability in buffers).

For custom specifications or material consultation, visit 6ccvd.com or contact our engineering team directly.

Tech Support

Section titled “Tech Support”

Original Source

Section titled “Original Source”

References

Section titled “References”
  1. 2011 - Electroanalytical Methods in Pharmaceutical Analysis and Their Validation

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