Voltammetric determination of antipsychotic drug flupentixol HCl in human serum at a boron-doped diamond electrode
At a Glance
Section titled âAt a Glanceâ| Metadata | Details |
|---|---|
| Publication Date | 2022-05-31 |
| Journal | Journal of the Turkish Chemical Society Section A Chemistry |
| Authors | Burcin BozalâPalabiyik |
| Institutions | Ankara University |
| Analysis | Full AI Review Included |
Technical Documentation & Analysis: Voltammetric Determination of Flupentixol HCl using Boron-Doped Diamond Electrodes
Section titled âTechnical Documentation & Analysis: Voltammetric Determination of Flupentixol HCl using Boron-Doped Diamond ElectrodesâExecutive Summary
Section titled âExecutive SummaryâThis research validates the superior performance of Boron-Doped Diamond Electrodes (BDDE) for highly sensitive bioanalytical sensing, specifically for Therapeutic Drug Monitoring (TDM) of the antipsychotic drug Flupentixol (FLP) in human serum.
- Core Achievement: Successful development of a simple, fast, and accurate Differential Pulse Voltammetry (DPV) method for FLP determination in synthetic human serum.
- Material Validation: BDDE demonstrated exceptional robustness, chemical inertness, and resistance to electrode fouling, outperforming traditional carbon-based electrodes (e.g., Glassy Carbon Electrode, GCE).
- High Sensitivity: Achieved a low Limit of Detection (LOD) of 1.08 x 10-7 M in serum, comparable to or better than complex, high-cost chromatographic methods (e.g., HPLC).
- Diffusion Control: The oxidation behavior of FLP at the BDDE surface was confirmed to be irreversible and diffusion-controlled, indicating stable mass transport kinetics.
- Bioanalytical Accuracy: High average recovery (99.91%) from spiked serum samples confirms the methodâs accuracy and precision for clinical TDM applications.
- 6CCVD Value Proposition: This study reinforces the critical need for high-quality, heavily doped BDD materials, which 6CCVD supplies in custom dimensions and specifications for advanced electrochemical sensing platforms.
Technical Specifications
Section titled âTechnical SpecificationsâThe following hard data points were extracted from the voltammetric determination study using the Boron-Doped Diamond Electrode (BDDE).
| Parameter | Value | Unit | Context |
|---|---|---|---|
| Working Electrode Material | Boron-Doped Diamond (BDD) | N/A | Demonstrates metal-like conductivity (103 - 104 ppm doping) |
| Working Electrode Diameter | 3 | mm | Standard commercial size used in the study |
| Optimum Supporting Electrolyte | pH 2.0 | N/A | Britton-Robinson (BR) Buffer solution |
| Measured Potential (Ep) | 986 | mV | vs Ag/AgCl reference electrode |
| Bulk Linear Range | 6.0 x 10-7 to 8.0 x 10-6 | M | Concentration range for bulk FLP solution |
| Serum Linear Range | 8.0 x 10-7 to 1.0 x 10-5 | M | Concentration range for spiked serum samples |
| Serum Limit of Detection (LOD) | 1.08 x 10-7 | M | High sensitivity achieved in complex biological matrix |
| Serum Limit of Quantification (LOQ) | 3.61 x 10-7 | M | Required for accurate TDM |
| Average Serum Recovery | 99.91 | % | High accuracy confirmed (n=5 measurements) |
| Inter-day Precision (RSD) | 2.83 | % | Relative Standard Deviation for serum analysis |
| Mass Transport Mechanism | Diffusion-Controlled | N/A | Confirmed by linear Randles-Sevcik plot (ip vs v1/2) |
Key Methodologies
Section titled âKey MethodologiesâThe electrochemical determination of Flupentixol (FLP) utilized Differential Pulse Voltammetry (DPV) on a BDD electrode.
- Electrode Setup: A conventional three-electrode cell was employed, consisting of a 3 mm diameter BDDE working electrode, an Ag/AgCl (3 M NaCl) reference electrode, and a Platinum wire auxiliary electrode.
- Electrode Pre-treatment: The BDDE surface was mechanically cleaned before each measurement using alumina powder and a polishing cloth to ensure optimal surface activity and minimize fouling.
- Electrolyte Preparation: The measurement solution consisted of 20% methanol and pH 2.0 Britton-Robinson (BR) buffer solution (0.04 M), selected for providing the highest peak current and best peak shape.
- Voltammetric Technique Selection: Differential Pulse Voltammetry (DPV) was chosen as the primary working method due to its superior repeatability and sensitivity compared to Cyclic Voltammetry (CV) and Square Wave Voltammetry (SWV).
- Optimized DPV Parameters:
- Step Potential: 10 mV
- Modulation Amplitude: 50 mV
- Modulation Time: 50 ms
- Interval Time: 500 ms
- Sample Preparation: Serum proteins were precipitated using methanol and acetonitrile, followed by ultrasonication and centrifugation (5000 rpm for 15 minutes) to isolate the supernatant for analysis.
6CCVD Solutions & Capabilities
Section titled â6CCVD Solutions & CapabilitiesâThis research highlights the indispensable role of high-quality Boron-Doped Diamond (BDD) in developing next-generation bioanalytical sensors. 6CCVD is uniquely positioned to supply the materials required to replicate, scale, and advance this research into commercial TDM platforms.
Applicable Materials
Section titled âApplicable MaterialsâTo achieve the metal-like conductivity and robustness demonstrated in this study, researchers require heavily doped BDD material.
| 6CCVD Material Solution | Specification & Relevance to Research |
|---|---|
| Heavy Boron-Doped Diamond (BDD) | Required for metal-like conductivity (103 - 104 ppm B doping). 6CCVD provides BDD wafers optimized for low resistivity and wide potential windows, crucial for complex serum analysis. |
| Polycrystalline Diamond (PCD) Wafers | Available in large formats (up to 125 mm diameter) for high-throughput sensor array fabrication or integration into microfluidic devices. |
| Ultra-Smooth Polishing | 6CCVD offers polishing down to Ra < 5 nm for inch-size PCD/BDD. Minimizing surface roughness is critical for reducing the electrode fouling observed in the study (which caused peak intensity decrease). |
Customization Potential
Section titled âCustomization PotentialâThe study utilized a small, 3 mm diameter electrode. 6CCVD specializes in providing custom geometries and integration features necessary for advanced electrochemical systems.
- Custom Dimensions and Shapes: 6CCVD can supply BDD plates/wafers up to 125 mm in diameter and provide precision laser cutting services to create custom electrode geometries (e.g., 3 mm discs, microelectrode arrays, or integrated flow cell components).
- Thickness Control: We offer precise BDD layer thickness control from 0.1 ”m up to 500 ”m, allowing optimization for specific electrochemical sensitivity and substrate integration.
- Integrated Metalization: For seamless integration into sensor platforms, 6CCVD offers in-house metalization services, including Ti/Pt/Au contacts, which are essential for connecting the BDD working electrode to external circuitry.
Engineering Support
Section titled âEngineering SupportâThe success of this voltammetric method relies heavily on selecting the correct diamond material properties (doping level, surface termination, and roughness).
- Bioanalytical Expertise: 6CCVDâs in-house PhD engineering team specializes in material selection and optimization for electrochemical applications, including Therapeutic Drug Monitoring (TDM) and bioanalytical sensing.
- Fouling Mitigation: We provide consultation on surface treatments and polishing specifications (Ra < 5 nm) to minimize electrode passivation and fouling, directly addressing the limitations noted in the research paper.
- Global Supply Chain: 6CCVD ensures reliable, global shipping (DDU default, DDP available) of high-specification BDD materials, supporting international research and development efforts.
For custom specifications or material consultation, visit 6ccvd.com or contact our engineering team directly.
View Original Abstract
This study aims to offer a voltammetric method for determining the antipsychotic drug flupentixol from serum samples. According to pH and scan rate studies, the oxidation behavior of flupentixol at boron-doped diamond electrode was found as irreversible and diffusion-controlled. In order to determine flupentixol from bulk form and serum samples, differential pulse voltammetry was preferred as the working method because of the repeatability. Linear responses were obtained in the range of 6.0Ă10-7 - 8.0Ă10-6 M and 8.0Ă10-7 - 1.0Ă10-5 M for bulk form and serum samples in pH 2.0 Britton-Robinson buffer solution, with detection limit values of 1.09Ă10-7 M and 1.08Ă10-7 M, respectively. Required validation parameters were also studied and according to recovery from serum samples (99.91 %) and precision studies, it can be said that developed method was accurate and precise.