Determination of methylprednisolone acetate in biological fluids at gold nanoparticles modified ITO electrode.

The electrochemical behavior of a corticosteroid methylprednisolone (MP), used for doping, has been studied at gold nanoparticles modified indium tin oxide (nanoAu/ITO) electrode. The nanoAu/ITO electrode exhibited an effective catalytic response towards its oxidation and lowered its oxidation potential by approximately 127 mV when compared with bare ITO electrode. Oxidation of MP has been carried out in phosphate containing electrolyte in the pH range 2.13-10.00 and a well-defined oxidation peak was noticed. Linear concentration curves are obtained over the concentration range 0.01-1.0 microM with a detection limit of 2.68 x 10(-7)M at nanoAu/ITO electrode. A diffusion coefficient of 2.36 x 10(-6)cm(2)/s is calculated for MP using chronoamperometry. The proposed method is effectively applied to detect the concentration of MP in pharmaceutical formulations and human blood plasma and urine samples. A comparison of MP concentration determined in blood plasma and urine by the proposed method and GC/MS indicated that the results are essentially similar. It is believed that the method will be useful in determining this drug in case of doping.

Fullerene C60 modified gold electrode and nanogold modified indium tin oxide electrode for prednisolone determination.

The electrochemical determination of prednisolone has been investigated at fullerene-C(60)-modified gold (C(60)/Au) electrode and gold nanoparticles modified indium tin oxide (nano Au/ITO) electrode in phosphate buffer solution (PBS) of pH 7.2. During oxidation of prednisolone, an anodic peak with peak potential (E(p)) at 570 mV and 400 mV appeared at nano Au/ITO and C(60)/Au electrode, respectively. The experimental results revealed that gold nanoparticles as well as fullerene (C(60)) promote the rate of prednisolone oxidation by increasing the peak current (i(p)) and oxidizing at lower peak potentials as compared to the respective bare electrodes due to their electrocatalytic effect. The linear concentration range at both the electrodes was in the range of 1 microM to 0.10 mM. The detection limit obtained at C(60)/Au electrode was 26 nM, while at nano Au/ITO electrode the detection limit was 90 nM. The applicability of the method to direct assays of human urine and whole blood sample is described to use the method for testing cases of doping by athletes.

Differential pulse voltammetric determination of methylprednisolone in pharmaceuticals and human biological fluids.

Electrochemical behaviour of methylprednisolone (MP) at the fullerene-C60-modified glassy carbon electrode has been investigated using differential pulse voltammetry. The experimental results suggest that the modified electrode exhibits electrocatalytic effect on the oxidation of MP resulting in a marked enhancement of the peak current response. Under the selected conditions, the oxidation peak current was linearly dependent on the concentration of MP in the range 5.0 nM-1.0 microM with a sensitivity of 0.0107 microA microM(-1). The detection limit was estimated to be 5.6 nM. The electrode showed good sensitivity, selectivity, stability and reproducibility. In addition, the developed method was satisfactorily applied to the determination of MP in pharmaceutical formulations and human serum and urine samples without any necessity for sample treatment or time-consuming extraction steps prior to the analysis. GC-MS method was used to cross-validate the results obtained for the quantitative estimation of MP in biological fluids and the results showed approximately 2% deviation to those obtained using the proposed method.

Voltammetric determination of adenosine and guanosine using fullerene-C(60)-modified glassy carbon electrode.

A fullerene-C(60)-modified glassy carbon electrode (GCE) is used for the simultaneous determination of adenosine and guanosine by differential pulse voltammetry. Compared to a bare glassy carbon electrode, the modified electrode exhibits an apparent shift of the oxidation potentials in the cathodic direction and a marked enhancement in the voltammetric peak current response for both the biomolecules. Linear calibration curves are obtained over the concentration range 0.5muM-1.0mM in 0.1M phosphate buffer solution at pH 7.2 with a detection limit of 3.02x10(-7)M and 1.45x10(-7)M for individual determination of adenosine and guanosine, respectively. The interference studies showed that the fullerene-C(60)-modified glassy carbon electrode exhibited excellent selectivity in the presence of hypoxanthine, xanthine, uric acid and ascorbic acid. The proposed procedure was successfully applied to detect adenosine and guanosine in human blood plasma and urine, without any preliminary pre-treatment.

Gold nanoparticles modified indium tin oxide electrode for the simultaneous determination of dopamine and serotonin: Application in pharmaceutical formulations and biological fluids.

A new rapid, convenient and sensitive electrochemical method based on a gold nanoparticles modified ITO (Au/ITO) electrode is described for the detection of dopamine and serotonin in the presence of a high concentration of ascorbic acid. The electrocatalytic response was evaluated by differential pulse voltammetry (DPV) and the modified electrode exhibited good electrocatalytic properties towards dopamine and serotonin oxidation with a peak potential of 70mV and 240mV lower than that at the bare ITO electrode, respectively. The selective sensing of dopamine is further improved by applying square wave voltammetry (SWV) which leads to the lowering of its detection limit. A similar effect on the detection limit of serotonin was observed on using SWV. Linear calibration curves are obtained in the range 1.0x10(-9)-5.0x10(-4)M and 1.0x10(-8)-2.5x10(-4)M with a detection limit of 0.5nM and 3.0nM for dopamine and serotonin, respectively. The Au/ITO electrode efficiently determines both the biomolecules simultaneously, even in the presence of a large excess of ascorbic acid. The adequacy of the developed method was evaluated by applying it to the determination of the content of dopamine in dopamine hydrochloride injections. The proposed procedure was also successfully applied to simultaneously detect dopamine and serotonin in human serum and urine.

Fullerene-C60-modified electrode as a sensitive voltammetric sensor for detection of nandrolone--an anabolic steroid used in doping.

The electrochemical behaviour of nandrolone is investigated by cyclic, differential pulse and square-wave voltammetry in phosphate buffer system at fullerene-C60-modified electrode. The modified electrode shows an excellent electrocatalytic activity towards the oxidation of nandrolone resulting in a marked lowering in the peak potential and considerable improvement of the peak current as compared to the electrochemical activity at the bare glassy carbon electrode. The oxidation process is shown to be irreversible and diffusion-controlled. A linear range of 50 microM to 0.1 nM is obtained along with a detection limit and sensitivity of 0.42 nM and 0.358 nA nM(-1), respectively, in square-wave voltammetric technique. A diffusion coefficient of 4.13x10(-8) cm2 s(-1) was found for nandrolone using chronoamperometry. The effect of interferents, stability and reproducibility of the proposed method were also studied. The described method was successfully employed for the determination of nandrolone in human serum and urine samples. A cross-validation of observed results by GC-MS indicates that the results are in good agreement with each other.

Nickel(II)-selective sensor based on dibenzo-18-crown-6 in PVC matrix.

Nickel(II)-selective sensors have been fabricated from poly(vinyl chloride) (PVC) matrix membranes containing neutral carrier dibenzo-18-crown-6 as electroactive material, sodium tetraphenylborate (NaTPB) as an anion excluder and tris-(2-ethylhexyl) phosphate (TEHP) as plasticizing solvent mediator. The membrane having the composition of crown ether:NaTPB:TEHP:PVC in the ratio 10:1:200:200 (w/w) exhibits best results with linear potential response in the concentration range of 1.0x10(-5) to 1.0x10(-1)M and a Nernstian slope of 29.5mV/decade of activity between 2.6 and 6.8. The sensor exhibits a fast response time of <25s, is inert towards non-aqueous medium up to 15% (v/v) and was used over a period of 4 months with good reproducibility. It is selective over a number of mono-, bi- and trivalent cations. The practical utility of the sensor has been demonstrated by using it as an indicator electrode in the potentiometric titration of Ni(2+) against EDTA and also for the estimation of Ni(2+) in some Indian brand chocolates.