DETERMINATION OF ANTI-CANCER DRUG PALBOCICLIB FROM HUMAN BIOLOGICAL FLUIDS BY USING DIFFERENTIAL PULSE VOLTAMMETRIC METHOD AT BORON DOPED DIAMOND ELECTRODE
At a Glance
Section titled âAt a Glanceâ| Metadata | Details |
|---|---|
| Publication Date | 2024-08-11 |
| Journal | Ankara Universitesi Eczacilik Fakultesi Dergisi |
| Authors | Melike Akan, ĂiÄdem KanbeĆ Dindar, Nazife Aslan, Bengi Uslu |
| Institutions | Ankara University, Ankara Hacı Bayram Veli University |
| Analysis | Full AI Review Included |
Technical Documentation & Analysis: Boron-Doped Diamond for Advanced Electroanalysis
Section titled âTechnical Documentation & Analysis: Boron-Doped Diamond for Advanced ElectroanalysisâExecutive Summary
Section titled âExecutive SummaryâThis research successfully demonstrates the superior performance of Boron-Doped Diamond Electrodes (BDDE) in the highly sensitive quantification of the anti-cancer drug Palbociclib in complex biological fluids (human serum and urine).
- Core Value Proposition: BDDE enables a highly efficient, simple, and environmentally friendly electroanalytical method (Differential Pulse Voltammetry, DPV) for Therapeutic Drug Monitoring (TDM).
- Sensitivity Achieved: The method reached Limits of Detection (LOD) as low as 1.31 nM in urine samples, demonstrating sensitivity competitive with or superior to many time-consuming chromatographic techniques (Table 2).
- Material Robustness: The BDDE proved chemically stable and effective in strongly acidic environments (optimal performance at pH 2.0 PBS), a key advantage over conventional carbon or metallic electrodes.
- Mechanism Confirmation: Electrochemical characterization confirmed the oxidation of Palbociclib on the BDDE surface is an irreversible, diffusion-controlled process, validating the materialâs suitability for solution-phase analysis.
- Reproducibility: Excellent precision was achieved, with Inter-day Relative Standard Deviation (RSD%) ranging from 1.14% to 1.87% across all sample types.
- 6CCVD Relevance: This study validates the critical need for high-quality, heavily doped BDD material, a core offering of 6CCVD, for next-generation biosensing and electroanalytical platforms.
Technical Specifications
Section titled âTechnical SpecificationsâThe following hard data points were extracted from the research paper, focusing on material performance and analytical results.
| Parameter | Value | Unit | Context |
|---|---|---|---|
| Working Electrode Material | Boron-Doped Diamond (BDDE) | - | 3 mm diameter |
| Optimal Supporting Electrolyte | pH 2.0 | - | Phosphate Buffer Solution (PBS) |
| Standard Linearity Range | 0.01-1 | ”M | Standard Drug Solution |
| Biological Sample Linearity Range | 0.02-0.8 | ”M | Human Serum and Urine |
| Lowest Limit of Detection (LOD) | 1.31 | nM | Urine Sample Analysis |
| Standard Solution LOD | 2.28 | nM | Standard Solution Analysis |
| Anodic Peak Potential (Standard) | 756 | mV | Measured using DPV |
| Anodic Peak Potential (Serum/Urine) | 786 | mV | Measured using DPV |
| Inter-day Precision (RSD%) | 1.14 to 1.87 | % | Across all sample types |
| Ep vs. pH Slope | -47.2 | mV/pH | Indicates equal proton and electron transfer |
| CV Scan Rate Range Tested | 0.005 to 1 | V s-1 | Used to confirm diffusion control |
| Correlation Coefficient (r, Serum) | 0.9931 | - | High linearity of calibration curve |
Key Methodologies
Section titled âKey MethodologiesâThe experimental procedure relied on precise control over the electrochemical cell setup and sample preparation, highlighting the need for reproducible BDDE surfaces.
- Electrode System: A standard three-electrode cell (10 ml capacity) was utilized, comprising the BDDE working electrode, a platinum (Pt) wire counter electrode, and an Ag/AgCl (3 M NaCl) reference electrode.
- Electrode Surface Preparation: The BDDE surface was mechanically prepared prior to every measurement using alumina powder and a polishing cloth to ensure a consistent, low-roughness surface finish.
- Voltammetric Technique: Differential Pulse Voltammetry (DPV) was the primary analytical technique, with parameters optimized for Palbociclib detection: Step potential (10 mV), Modulation amplitude (50 mV), and Modulation time (50 ms). Cyclic Voltammetry (CV) was used for mechanistic studies.
- Optimal Medium Determination: Electrochemical behavior was tested across a pH range of 2.0 to 9.0. Phosphate Buffer Solution (PBS) at pH 2.0 was selected as the optimal medium due to superior peak shape, maximum current, and reproducibility.
- Biological Sample Pre-treatment: Protein precipitation was performed on human serum samples using acetonitrile, followed by sonication (15 minutes) and centrifugation (5000 rpm) to isolate the supernatant for analysis. Urine samples were similarly fortified and treated with acetonitrile before centrifugation.
6CCVD Solutions & Capabilities
Section titled â6CCVD Solutions & CapabilitiesâThe successful implementation of this highly sensitive electroanalytical method hinges entirely on the quality and consistency of the Boron-Doped Diamond Electrode (BDDE). 6CCVD is uniquely positioned to supply the necessary materials and customization required to replicate, scale, and advance this research.
Applicable Materials
Section titled âApplicable MaterialsâTo achieve the low Limits of Detection (LOD) reported (down to 1.31 nM), the research requires highly conductive, electrochemically stable diamond material.
| Research Requirement | 6CCVD Solution & Material Recommendation | Technical Advantage |
|---|---|---|
| Boron-Doped Diamond (BDDE) | Heavy Boron-Doped Diamond (BDD) Wafers/Plates | 6CCVD offers precise control over doping concentration (e.g., >1020 atoms/cm3) to ensure metallic conductivity, minimizing background current and maximizing signal-to-noise ratio for nM-level detection. |
| High Chemical Stability | BDD Substrates (up to 10mm thickness) | Our MPCVD BDD is highly resistant to extreme chemical environments (like the optimal pH 2.0 PBS used), ensuring long electrode lifetime and stability crucial for routine TDM applications. |
| Surface Consistency | Polycrystalline Diamond (PCD) Polishing (Ra < 5nm) | We provide high-quality polishing services for PCD/BDD wafers, ensuring the low surface roughness necessary for reproducible electrochemical measurements and minimizing electrode fouling observed in the paper. |
Customization Potential
Section titled âCustomization PotentialâThe paper utilized a specific 3 mm diameter BDDE. 6CCVDâs custom fabrication capabilities allow researchers to optimize electrode geometry and integration.
- Custom Dimensions: 6CCVD provides BDD plates and wafers up to 125mm in size. We offer precision laser cutting and dicing services to replicate the exact 3 mm diameter geometry used in this study or to create custom microelectrode arrays for enhanced sensitivity and multiplexing.
- Metalization Services: The three-electrode setup requires robust electrical contact. 6CCVD offers internal metalization capabilities (Au, Pt, Ti, W, Cu) for creating reliable contact pads directly on the BDD substrate, simplifying integration into electrochemical cells and sensor packaging.
- Thickness Control: We offer BDD films with precise thickness control ranging from 0.1 ”m to 500 ”m, allowing researchers to tailor the material to specific application needs, whether for thin-film sensing or robust bulk electrodes.
Engineering Support
Section titled âEngineering SupportâThe challenges noted in the paper (e.g., peak intensity decrease due to contamination) are common in electroanalysis. 6CCVD provides expert support to overcome these hurdles.
- Application Expertise: 6CCVDâs in-house PhD team specializes in optimizing diamond material properties for advanced electroanalytical applications, including Therapeutic Drug Monitoring (TDM) and biosensing.
- Fouling Mitigation: We can assist researchers in selecting the ideal BDD surface termination (e.g., hydrogen or oxygen termination) to minimize electrode fouling and maximize reproducibility, directly addressing the peak intensity decay observed during repetitive CV scans in the reported study.
- Global Supply Chain: We offer global shipping (DDU default, DDP available) ensuring rapid and reliable delivery of custom diamond materials to research facilities worldwide.
Call to Action: For custom specifications or material consultation regarding high-performance Boron-Doped Diamond Electrodes for electroanalysis, visit 6ccvd.com or contact our engineering team directly.
View Original Abstract
Objective: A very efficient and sensitive electrochemical technique utilizing differential pulse voltammetry (DPV) at a boron-doped diamond electrode (BDDE) was devised to measure Palbociclib in this study. Material and Method: All experiments employed typical three-electrode cell of 10 ml capacity in conjunction with boron-doped diamond electrode, a platinum wire counter electrode, and an Ag/AgCl reference electrode. During electrochemical measurements, DPV and cyclic voltammetry (CV) methods was utilized at BDDE. Result and Discussion: Based on experimental findings from electrochemical characterization investigations, it was determined that oxidation behavior of Palbociclib in BDDE is irreversible and regulated by diffusion. Anodic peak current exhibited a linear relationship within concentration range of 0.01-1 ”M, 0.02-0.8 ”M, and 0.02-0.8 ”M in pH 2.0 phosphate buffer solution (PBS) for reference substance solution, human serum, and urine samples, respectively. Limits of detection were found as 2.28 nM, 2.93 nM, and 1.31 nM for standard drug solution, human serum and urine samples, respectively. In order to validate the developed method, its repeatability, reproducibility, selectivity, precision and accuracy in all environments were investigated and calculated. This method was successfully applied for the analysis of Palbociclib in human serum and urine samples .