ELECTROCHEMICAL INVESTIGATION OF OTILONIUM BROMIDE USING BORON-DOPED DIAMOND AND GLASSY CARBON ELECTRODES
At a Glance
Section titled âAt a Glanceâ| Metadata | Details |
|---|---|
| Publication Date | 2023-08-29 |
| Journal | Ankara Universitesi Eczacilik Fakultesi Dergisi |
| Authors | Leyla KaradurmuĆ, Esen Bellur Atıcı, SĂbel A. Ăzkan |
| Institutions | Ankara University, Adıyaman University |
| Citations | 1 |
| Analysis | Full AI Review Included |
Technical Documentation & Analysis: Boron-Doped Diamond for Electroanalytical Sensing
Section titled âTechnical Documentation & Analysis: Boron-Doped Diamond for Electroanalytical SensingâExecutive Summary
Section titled âExecutive SummaryâThis analysis focuses on the successful application of Boron-Doped Diamond Electrodes (BDDE) for the rapid and sensitive determination of Otilonium Bromide (OTB), an antispasmodic drug, via Differential Pulse Voltammetry (DPV).
- Material Validation: The study confirms the superior performance of BDDE over Glassy Carbon Electrodes (GCE) in electroanalytical sensing, specifically noting a higher peak current and better analytical figures of merit.
- High Sensitivity: BDDE achieved a low Limit of Detection (LOD) of 4.92x10-6 M, validating its use for trace analysis in pharmaceutical quality control.
- Diffusion Control: The electrochemical oxidation mechanism of OTB was confirmed to be irreversible and diffusion-controlled across both electrode types, simplifying modeling and application.
- Irreversible Oxidation: OTB exhibited two distinct, irreversible oxidation peaks on BDDE, with the main peak occurring at 1.5761 V in 0.1 M H2SO4.
- Cost-Effective Alternative: The proposed DPV method using BDDE offers a low-cost, rapid, and eco-friendly alternative to expensive, labor-intensive chromatographic techniques (e.g., HPLC, CE) for drug assay.
- 6CCVD Relevance: This research directly supports the demand for high-quality, heavily boron-doped MPCVD diamond material for advanced electrochemical sensor development.
Technical Specifications
Section titled âTechnical SpecificationsâThe following hard data points were extracted from the study, highlighting the performance of the Boron-Doped Diamond Electrode (BDDE) under optimal conditions.
| Parameter | Value | Unit | Context |
|---|---|---|---|
| Working Electrode | Boron-Doped Diamond (BDDE) | N/A | Used in a three-electrode cell setup |
| Measured Potential (Ep) | 1.5761 | V | Main oxidation peak potential on BDDE |
| Optimal Supporting Electrolyte | 0.1 M H2SO4 | N/A | Achieved highest peak current (pH 0.3) |
| Linearity Range (BDDE) | 8x10-5 - 8x10-4 | M | Concentration range for DPV analysis |
| Limit of Detection (LOD) | 4.92x10-6 | M | Superior sensitivity compared to GCE |
| Limit of Quantitation (LOQ) | 1.49x10-5 | M | Quantifiable minimum concentration |
| Repeatability (RSD%) | 0.62 | % | High precision of the BDDE method |
| Correlation Coefficient (R2) | 0.9909 | N/A | High linearity of the calibration graph |
| DPV Scan Rate (Optimal) | 0.010071 | mV s-1 | Used for analytical determination |
| CV Scan Rate (Mechanism Study) | 0.01 - 1.00 | V s-1 | Confirmed diffusion-controlled process |
Key Methodologies
Section titled âKey MethodologiesâThe electrochemical investigation relied on precise material preparation and controlled voltammetric parameters.
| Step | Description |
|---|---|
| Electrode Configuration | Standard three-electrode cell (10 ml capacity) employed: BDDE/GCE working, Platinum (Pt) wire counter, and Ag/AgCl reference electrode. |
| Electrode Pre-treatment | Manual polishing using 0.01 M aluminum oxide slurry on a smooth pad, followed by cleaning with double-distilled water. |
| Instrumentation | AUTOLAB 204 potentiostat/galvanostat controlled by NOVA 1.8 software. |
| Electrolyte Screening | Broad pH range investigation (0.3-12.0) using Phosphate, Acetate, Britton Robinson buffers, and H2SO4 solutions. |
| Optimal DPV Parameters | Step Potential: 0.005 V. Modulation Amplitude: 0.05 V. Modulation Time: 0.05 s. Interval Time: 0.5 s. Scan Rate: 0.010071 mV s-1. |
| Mechanism Study | Cyclic Voltammetry (CV) performed at various scan rates (0.01 V s-1 to 1.00 V s-1) to confirm diffusion control. |
6CCVD Solutions & Capabilities
Section titled â6CCVD Solutions & CapabilitiesâThis research underscores the critical role of high-quality Boron-Doped Diamond (BDD) in developing next-generation electroanalytical sensors. 6CCVD is uniquely positioned to supply the materials required to replicate, scale, and advance this technology.
Applicable Materials
Section titled âApplicable MaterialsâTo achieve the low LOD and high stability demonstrated in this study, researchers require heavily doped, high-purity BDD material.
- Heavy Boron-Doped Diamond (BDD): 6CCVD provides highly conductive, polycrystalline BDD wafers and plates, essential for achieving the low background currents and wide potential window (up to 3 V) necessary for sensitive DPV analysis.
- Custom Thickness: We offer BDD films ranging from 0.1 ”m up to 500 ”m, allowing engineers to optimize the material volume and conductivity profile for specific sensor designs.
- Polishing Excellence: For applications requiring minimal surface defects and maximum reproducibility (critical for low RSD% values like the 0.62% achieved), 6CCVD offers polishing services to achieve roughness Ra < 5 nm on inch-size PCD/BDD wafers.
Customization Potential
Section titled âCustomization PotentialâThe performance of the BDDE is highly dependent on its geometry and integration into the electrochemical cell. 6CCVD offers comprehensive customization services to meet specific research needs:
| Requirement from Research | 6CCVD Customization Solution |
|---|---|
| Custom Electrode Geometry | We provide custom dimensions for plates/wafers up to 125 mm, including laser cutting and shaping services to produce specific electrode geometries (e.g., discs, rings, or arrays) required for advanced potentiostat setups. |
| Reference Electrode Integration | While the paper used an external Ag/AgCl reference, 6CCVD can integrate metalization layers (e.g., Ti/Pt/Au) directly onto the diamond substrate for microelectrode arrays or integrated sensor chips. |
| Optimized Doping Levels | We offer precise control over boron concentration during the MPCVD growth process, allowing researchers to fine-tune conductivity and surface termination for optimal OTB oxidation kinetics. |
Engineering Support
Section titled âEngineering Supportâ6CCVDâs in-house team of PhD material scientists specializes in optimizing diamond properties for electrochemical applications.
- Application Expertise: Our team can assist researchers in material selection and design optimization for similar drug assay and electroanalytical sensing projects, ensuring the correct doping density and surface termination (e.g., hydrogen or oxygen termination) are specified for maximum sensitivity and stability.
- Global Supply Chain: We ensure reliable, global shipping (DDU default, DDP available) of sensitive diamond materials, supporting continuous research worldwide.
For custom specifications or material consultation, visit 6ccvd.com or contact our engineering team directly.
View Original Abstract
Objective: Using cyclic (CV) and differential pulse (DPV) voltammetric techniques, the electrochemical research of otilonium bromide (OTB) was carried out over a wide pH range (0.3-12) at glassy carbon electrodes (GCE) and boron-doped diamond electrodes (BDDE). The typical electrochemical behavior of OTB was identified as being dependent on the type of working electrode and pH. This research aims to provide a brand-new electroanalytical technique for measuring OTB in buffer solutions. Material and Method: All experiments employed the typical three-electrode cell of 10 ml capacity in conjunction with a platinum wire counter electrode, a BDDE and GCE working electrode, and an Ag/AgCl reference electrode. NOVA 1.8 software and an AUTOLAB 204 potentiostat/galvanostat were used for electrochemical measurements. Result and Discussion: The electrochemical behavior of OTB, which belongs to a class of drugs called âantispasmodicsâ (spasm and cramps reliever), primarily used to treat irritable bowel syndrome (IBS), and other gastrointestinal conditions characterized by motility problems, painful bowel spasms and distension (swelling and bloating in the belly area), was examined in 0.1 M H2SO4 at BDDE and GCE. The electrooxidation mechanism was also investigated by conducting CV investigations at various pH levels throughout a broad pH range (pH 0.3-12.0). Understanding the mechanism was aided by scan rate investigations, which revealed that diffusion was controlled for both electrodes. The proposed technique was successfully used to determine OTB under optimal conditions.