Kristína Cinková

Simple and Rapid Quantification of Folic Acid in Pharmaceutical Tablets using a Cathodically Pretreated Highly Boron-doped Polycrystalline Diamond Electrode

ABSTRACT A simple, rapid, and sensitive electroanalytical method for the direct quantification of folic acid was developed using square-wave voltammetry with a cathodically pretreated highly boron-doped polycrystalline diamond electrode. The morphology and structure of this electrode were investigated by scanning electron microscopy and Raman spectroscopy. The electrochemical behavior of folic acid was studied by cyclic voltammetry and an irreversible oxidation peak was observed at +0.78 volt vs. Ag/AgCl in Britton-Robinson buffer at pH 5. Using optimized square-wave voltammetric parameter values, the response of folic acid was linear from 0.1 to 167 micromolar with a limit of detection of 30 nanomolar with good repeatability. The influence of some interfering compounds was also evaluated. The method was successfully applied to the quantification of folic acid in pharmaceutical tablets. Considering the importance of the analyte upon human health, the boron-doped diamond electrode may be employed as an effective alternative electroanalytical approach.

Electroanalytical application of a boron-doped diamond electrode for sensitive voltammetric determination of theophylline in pharmaceutical dosages and human urine

In this paper, a novel voltammetric method for the determination of 1,3-dimethylxanthine alkaloid theophylline is elaborated using differential pulse (DPV) and square-wave voltammetric (SWV) modes on a boron-doped diamond electrode. Direct oxidation of the analyte at very positive potentials was observed by cyclic voltammetry, as evidenced by the presence of a well-shaped irreversible peak at +1.63 V (vs. Ag/AgCl electrode) in 1 mol L−1 sulphuric acid. After optimization of experimental conditions, the current response of theophylline was proportionally linear from 2 to 380 μmol L−1 using both pulse techniques. The developed electroanalytical method yielded low detection limits of 0.91 and 1.45 μmol L−1 associated with good intra-day repeatability (relative standard deviation of 3.2 and 2.5%) using DPV and SWV, respectively. The influence of some possible interferents was also evaluated. The practical feasibility of the proposed methodology was tested in the analysis of pharmaceutical dosages and human urine samples and good recovery values were accomplished (93.2–102.5%). The results of analysis of pharmaceuticals were also in close agreement at a 95% confidence level with those obtained using the titration (reference) method. Taking these attributes into consideration, the proposed sensor may be employed as a simple and effective analytical tool in drug control analysis and analysis of biological samples as well as a useful alternative to previously utilized modified electrodes in this field.

The doping level of boron-doped diamond electrodes affects the voltammetric sensing of uric acid

In this work, the electrochemical oxidation and subsequent determination of uric acid was investigated using boron-doped diamond electrodes with various B/C ratios (0–2000 ppm). The cyclic voltammetric study showed one irreversible oxidation peak at +(1.1–1.25) V (vs. Ag/AgCl/3 M KCl) in the presence of Britton–Robinson buffer (pH 2.25) depending on the boron content. Employing differential pulse voltammetry using the 2000 ppm boron-doped diamond electrode the acquired analytical parameters were as follows: a limit of detection of 7.7 μM, a limit of quantification of 26 μM and intra-day repeatability (relative standard deviation of 2.9% for n = 15). After performing an interference study, the method was applied to the determination of uric acid in biological samples (human urine). The uric acid concentrations determined in the urine samples were compared with the reference values stated in the literature. The proposed methodology using boron-doped diamond electrodes could find applications in uric acid sensing within clinical, pharmaceutical and environmental analysis.

Rapid electrochemical platform for nicotine sensing in cigarettes and chewing gums

Abstract A novel protocol for the simple and rapid determination of nicotine using square-wave voltammetry at boron-doped diamond electrode was developed. The effect of pH of supporting electrolyte, scan rate and square-wave voltammetric parameters was examined. Behavior study revealed that nicotine provided two irreversible oxidation peaks, the first one well-shaped at +1.14 V and the second one poorly-defined at +1.61 V vs. Ag/AgCl electrode in the presence of phosphate buffer (pH 9.0). Under optimal experimental conditions (modulation amplitude of 40 mV, frequency of 50 Hz and scan rate of 0.225 V · s-1), the current response of nicotine was proportionally linear in the concentration range from 9.9 × 10-6 to 1.7 × 10-4 mol · L-1 (R2 = 0.996) with the detection limit of 6.1 × 10-6 mol · L-1 (0.989 mg · L-1) and the relative standard deviation of 8.8 % (number of measurements n = 10, 5.7 × 10-5 mol · L-1 nicotine). The proposed procedure was applied to the quantification of nicotine in cigarettes and chewing gums with the determined values in good agreement with those declared by producer. In this respect, the developed protocol could represent an effective and rapid alternative to chemically modified electrodes in analysis of alkaloids.

Electrochemical and analytical performance of boron-doped diamond electrode for determination of ascorbic acid

Abstract The electrochemical behavior and determination of ascorbic acid (AA) was investigated at a bare boron-doped diamond (BDD) electrode using cyclic and differential pulse voltammetry. The influence of pH of supporting electrolyte and scan rate on the current response of analyte was examined to select the suitable experimental conditions. It was found that AA provided one well-shaped irreversible and diffusioncontrolled oxidation peak at +0.87 V vs. Ag/AgCl in Britton-Robinson buffer pH 4.0. Applying differential pulse voltammetry, the peak current of AA was linearly proportional to its concentration from 5 × 10-6 to 2 × 10-4 mol L-1 (R2 = 0.999), with the limit of detection of 1.1 × 10-6 mol L-1 and the good repeatability (relative standard deviation of 2.3 %). The developed electroanalytical protocol was successfully applied to determine the content of AA in commercial pharmaceutical preparations, based on the standard additions method, with the obtained recovery of 122 %. The accomplished analytical performance indicates that BDD electrodes are promising electrochemical sensors for pharmaceutical analysis.

Utilization of electrochemical methods in determination of trace elements in beverages

Utilization of electrochemical methods in determination of trace elements in beverages Electrochemical methods have many inherent advantages such as simplicity, low cost and amenability to miniaturization. A new, sensitive and selective electrochemical method for the caffeine determination using boron doped diamond electrode was developed. It was found by cyclic voltammetry that caffeine provided highly reproducible and well-defined irreversible oxidation peak, at very positive potential of +1.55 V vs. Ag/AgCl electrode. The effect of pH and scan rate on the voltammetric response of caffeine oxidation were studied to select the optimum experimental conditions. Linear response of peak current on the concentration in the range from 4 × 10-7 to 2.5 × 10-5 mol L-1, good repeatability (RSD of 2.1 %) and the detection limit of 1.5 × 10-7 mol L-1 without any chemical modifications and electrochemical surface pretreatment were observed by differential pulse voltammetry in 0.4 mol L-1 perchloric acid. The effect of possible interfering compounds appeared to be negligible which evidently proved very good selectivity. The proposed method was successfully applied for the caffeine determination in commercially available beverage samples, with results in a close statistical agreement to these declared by manufacturer.

Electrochemical method for point-of-care determination of ciprofloxacin using boron-doped diamond electrode

Abstract This paper presents an electrochemical behavior study and quantification of fluoroquinolone antibiotic ciprofloxacin using boron-doped diamond electrode. Ciprofloxacin provides a diffusion-driven electrode reaction with an irreversible and poorly defined peak at +1.6 V vs. Ag/AgCl electrode in the presence of Britton-Robinson buffer solution pH 4. Applying differential pulse voltammetry (modulation amplitude of 60 mV, modulation time of 50 ms), the calibration curve with high linearity (R2 = 0.997) was obtained within the concentration range of (0.74 – 20.0) × 10−6 mol L−1 with the detection limit of 6.0 × 10−7 mol L−1 and repeatability expressed by relative standard deviation of 2.7 % (for 20 measurements). Interference study was performed to explore the selectivity of the elaborated procedure. By analysis of pharmaceutical dosages and model human urine samples, the ciprofloxacin content with the recovery values ranging from 88.4 to 121.2 % were determined. The developed approach using point-of-care electrochemical sensor based on boron-doped diamond material could represent inexpensive analytical alternative to separation methods and could be beneficial in analysis of biological samples and in the quality control in pharmaceutical industry.