Voltammetric Method Development for Itopride Assay in a Pharmaceutical Formulation

2020 ◽  
Vol 16 (3) ◽  
pp. 312-318
Author(s):  
Abdulaziz N. Amro

Background: Itopride used for the gastrointestinal symptoms caused by reduced gastrointestinal mobility. For the first time rapid, low cost and green voltammetric method has been applied to analyze itopride in pharmaceutical formulation. Method: Cyclic Voltammetry (CV), Linear Sweep Voltammetry (LSV), Square Wave Voltammetry (SWV) and Differential Pulse Voltammetry (DPV) methods have been applied in this study. Results: Na2SO4 (1M) supporting electrolyte exhibited sharper anodic peak current than other used supporting electrolytes; glassy carbon electrode (GC) working electrode shows better results than platinum electrode (Pt). SWV results show the lowest limit of detection and quantitation values of 2.3 and 18.1 μg.mL-1, respectively. SWV recovery is 100.56% and 100.46% for 50 μg.mL-1 and 100 μg.mL-1 of commercially available itopride tablets, respectively. Furthermore, SWV inter and intraday results precessions are better than other used methods with 0.96 and 0.56% RSD, respectively. Conclusion: The optimum method of applied methods in this study is SWV method. Voltammetry showed low LOD and LOQ values with high accuracy and precession in addition to comparable repeatability and reproducibility values.

2020 ◽  
Vol 67 (4) ◽  
pp. 1053-1060
Author(s):  
Sayed I. M. Zayed ◽  
Yousry M. Issa

The electrochemical behavior of chlorzoxazone at the carbon paste electrode was investigated in 0.04 mol/L Britton-Robinson buffer pH 6.50 using cyclic and differential pulse voltammetric techniques. Cyclic voltammetric studies indicated that the oxidation of the drug was irreversible and controlled mainly by diffusion. Experimental and instrumental parameters were optimized (50 mV/s scan rate, 50 mV pulse amplitude, and 0.04 mol/L Britton-Robinson (BR) buffer pH 6.50 as a supporting electrolyte) and a sensitive differential pulse anodic voltammetric method has been developed for the determination of the drug over the concentration range 0.17–1.68 μg/mL chlorzoxazone, with detection and quantitation limits of 0.05 and 0.16 μg/mL, respectively. The proposed voltammetric method was successfully applied to the determinationof the drug in its pharmaceutical formulation (Myoflex tablets), and in spiked human urine samples.


2020 ◽  
Vol 10 (23) ◽  
pp. 8419
Author(s):  
Adriana Remes ◽  
Florica Manea ◽  
Sorina Motoc (m. Ilies) ◽  
Anamaria Baciu ◽  
Elisabeta I. Szerb ◽  
...  

A novel electrochemical glucose sensor was developed, based on a multiwall carbon nanotubes (MWCNTs)-copper-1,3,5-benzenetricarboxylic acid (CuBTC)-epoxy composite electrode, named MWCNT-CuBTC. The electrode nanocomposite was prepared by a two-roll mill procedure and characterized morphostructurally by scanning electron microscopy (SEM). The CuBTC formed defined crystals with a wide size distribution, which were well dispersed and embedded in the MWCNTs. Its electrical conductivity was determined by four-point probe contact (DC) conductivity measurements. The electroactive surface area, determined using cyclic voltammetry (CV), was found to be 6.9 times higher than the geometrical one. The results of the electrochemical measurements using CV, linear sweep voltammetry (LSV), differential pulse voltammetry (DPV), chronoamperometry (CA) and multiple pulse amperometry (MPA) showed that the MWCNT-CuBTC composite electrode displayed high electrocatalytic activity toward the oxidation of glucose and, as a consequence, very high sensitivity. The best sensitivity of 14,949 µAmM−1cm−1 was reached using MPA at the potential value of 0.6 V/SCE, which was much higher in comparison with other copper-based electrodes reported in the literature. The good analytical performance, low cost and simple preparation method make this novel electrode material promising for the development of an effective glucose sensor.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Chennupalle Nageswara Reddy ◽  
Puthalapattu ReddyPrasad ◽  
NeelamYughandhar Sreedhar

The electrochemical reduction of zanosar was investigated systematically by direct current polarography, cyclic voltammetry, and differential pulse polarography (DPP). A simple DPP technique was proposed for the direct quantitative determination of anticancer drug zanosar in pharmaceutical formulation and spiked human urine samples for the first time. The reduction potential was −0.28 V versus Ag/AgCl with a hanging mercury drop electrode in Britton-Robinson buffer as supporting electrolyte. The dependence of the intensities of currents and potentials on pH, concentration, scan rate, deposition time, and nature of the supporting electrolyte was investigated. The calibration curve was found to be linear with the following equation:y=0.4041x+0.012, with a correlation coefficient of 0.992 (R2) over a concentration range from1.0×10-7 M to1.0×10-3 M. In the present investigation, the achieved limit of detection (LOD) and limit of quantization (LQD) were7.42×10-8 M and2.47×10-8 M; respectively. Excipients did not interfere with the determination of zanosar in pharmaceutical formulation and spiked urine samples. Precision and accuracy of the developed method were checked by recovery studies in pharmaceutical formulation and spiked human urine samples.


2020 ◽  
Vol 16 (4) ◽  
pp. 337-349
Author(s):  
Leyla Karadurmus ◽  
Kaan Eşme ◽  
Nurgul K. Bakirhan ◽  
Sibel A. Ozkan

: Antibiotics are an important class among drugs because they are a significant agent to deal with infections. Cephalosporins are a very important group of antibiotics in the β-lactam class. The cephalosporins are semisynthetic antibiotics derived from products of the fungus Cephalosporium. Cephalosporins are classified as first, second, third, fourth, and advanced generation, based largely on their antibacterial spectrum and stability to β-lactamases. Electrochemical methods have been used for the determination of cephalosporin just as used in the determination of many antibiotic drugs. Electroanalytical methods present generally high sensitivity, low cost, low requirements, ease of preparation of the samples in a very short time, and a short analysis time. The most commonly used types are cyclic voltammetry, differential pulse voltammetry, square wave voltammetry and linear sweep voltammetry. The aim of this review is to evaluate the advantages and uses of electroanalytical methods used in the determination of cephalosporins. In addition, current applications of the methods to the pharmaceutical analysis of cephalosporins will also be summarized in a table.


Author(s):  
J. Satish ◽  
P. Radhakrishnanand ◽  
K. Surendra Babu

Objective: To develop and validate a sensitive and stability indicating gradient reverse phase ultra-high performance(UHPLC-PDA) liquid chromatography with photodiode array(PDA) and mass spectroscopy (MS) of Norethindrone Acetate (NA) assay and organic impurities (OI) in active pharmaceutical Ingredient(API) and Pharmaceutical Formulation (PF).Methods: The chromatographic conditions were optimized using Zorbax SB-C18 analytical UHPLC column with the dimensions (100 x 2.1) mm and 1.8 μm particle sizes. The mobile phase consisted of water (solution A) and acetonitrile (solution B) with gradient elution as mentioned time (min)/% Solution B: Initial/40,0.2/40, 9.2/55,12.0/55,12.2/90,15.5/90, 15.8/40 and 18.0/40. The flow rate was at the rate of 0.4 ml/min and the detection wavelengths were 254 nm and 210 nm. The column was kept at 40 °C and the injection volume was 5 μL. Stability of NA sample in different conditions was investigated by exposing the drug to stress study utilizing acid, base, oxidation, thermal, Humidity and photolytic.Results: There was no interference from excipients, impurities or degradation products at the retention time of NA about 9.1 min indicating the specificity of the method.The drug showed good stability under oxidation, thermal, humidity and photolytic conditions, but significant degradation was observed under acid and base conditions. The procedure was validated for specificity, linearity, accuracy, precision and robustness. The degradation products were well resolved from NA and its impurities. The obtained LOD (Limit of detection) values are 0.001% to 0.015% and LOQ (Limit of quantification) values are 0.003% to 0.05% of impurities.Conclusion: A sensitive, rapid, specific and stability indicating gradient Reverse Phase UHPLC-PDA-PDA with MS (Orthogonal detectors) method for the determination of NA for the assay and organic impurities was successfully developed. The developed method was validated to be specific, linear, accurate, precise and robust. The peak purity and LC-MS test results confirmed that the NA peak was homogenous in all stress samples and the mass balance was found to be more than 99%, thus proving the stability indicating power of the method


2009 ◽  
Vol 74 (10) ◽  
pp. 1503-1515 ◽  
Author(s):  
Zuzana Jemelková ◽  
Jiří Zima ◽  
Jiří Barek

Direct current voltammetric (DCV) and differential pulse voltammetric (DPV) determination of antineoplastic agent doxorubicin (DOX) at a carbon paste electrode (CPE) was developed. Britton–Robinson buffer (pH 7.0) was used as a supporting electrolyte. The limits of detection are 8 × 10–7 mol l–1 (DCV) and 6 × 10–8 mol l–1 (DPV). The accumulation of DOX at the electrode surface was used to decrease the limits of detection down to 2.2 × 10–7 mol l–1 for adsorptive stripping DC voltammetry (DCAdSV) and 2.8 × 10–9 mol l–1 for adsorptive stripping differential pulse voltammetry (DPAdSV) at CPE. The results of the voltammetric methods were utilized for the development of a new determination of doxorubicin using HPLC with amperometric detection on CPE based on spherical microparticles of glassy carbon in a wall-jet configuration. A column with chemically bonded C18 stationary phase and a mobile phase containing 0.01 M phosphate buffer (pH 5.0)–methanol 25:75 (v/v) were used. The limit of detection is 4 × 10–7 mol l–1 (HPLC with electrochemical detection (ED)).


2021 ◽  
Author(s):  
Irum Naz Qureshi ◽  
Aneela Tahira ◽  
Khoulwod Aljadoa ◽  
Ali M. Alsalme ◽  
Asma A. Al-Othman ◽  
...  

Abstract The successful monitoring of the anticancer drugs using nanostructured materials is very important but very challenging task. Beside this, uniform and ultra-small size of metal oxide nanoparticles is highly needed in order to enhance the catalytic activity which could result into the development of sensitive and selective electrochemical sensors for methotrexate (MTX). For this purpose, we have used a simple approach involving the polyaniline (PANI) as a sacrificing template for the growth of uniform and ultra-small Co3O4 nanoparticles by hydrothermal method. The structure, shape, composition and phase purity were studied by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Fourier transform Infrared (FTIR) techniques. The average size of Co3O4 nanoparticles was below 50 nm. The cubic crystallography is confirmed for the Co3O4 nanoparticles. The electrochemical properties of PANI assisted Co3O4 nanoparticles for MTX drug was evaluated by cyclic voltammetry (CV) and linear sweep voltammetry (LSV) in Britton–Robinson buffer (BRB) of pH 3.5. The PANI assisted Co3O4 nanoparticles were found highly sensitive for the MTX drug and exhibited a linear range from 5-75µM of MTX and limit of detection for the modified electrode was estimated 1.98µM. The proposed electrochemical sensor is low cost, simple, highly sensitive and selective towards MTX detection. The synthetic methodology using the conducting polymer as a sacrificing template for the growth of controlled and ultra-small Co3O4 nanoparticles can be utilized for the wide range of electrochemical applications.


1994 ◽  
Vol 59 (5) ◽  
pp. 1018-1029 ◽  
Author(s):  
Jiří Barek ◽  
Roman Hrnčíř

The polarographic and voltammetric behaviour was examined for the title compound, which is the basic component in many commercial optical whitening agents. Dimethylformamide containing 5 vol.% water was chosen as the solvent and tetraethylammonium bromide as the supporting electrolyte. The optimum conditions were found for determining the substance by tast polarography, differential pulse polarography, linear sweep voltammetry on a hanging mercury drop electrode, and differential pulse voltammetry on a hanging mercury drop electrode. The analyte concentration regions for the four techniques were 0.1 - 0.5, 0.01 - 0.5, 0.01 - 0.5 and 0.01 - 0.1 mmol l-1, respectively. Practical applicability of the methods to the determination of the title compound in technical products was verified.


2018 ◽  
Vol 11 (4) ◽  
pp. 99
Author(s):  
Luane Ferreira Garcia ◽  
Carlos Eduardo Peixoto da Cunha ◽  
Emily Kussmaul Gonçalves Moreno ◽  
Douglas Vieira Thomaz ◽  
Germán Sanz Lobón ◽  
...  

Methyldopa is a catecholamine widely used in the treatment of mild to moderate hypertension whose determination in pharmaceutical formulae is of upmost importance for dose precision. Henceforth, a low-cost carbon paste electrode (CPE) consisting of graphite powder obtained from a crushed pencil stick was herein modified with nanostructured TiO2 (TiO2@CPE) aiming for the detection of methyldopa in pharmaceutical samples. The TiO2-modified graphite powder was characterized by scanning electron microscopy and X-ray diffraction, which demonstrated the oxide nanostructured morphology. Results evidenced that sensitivity was nonetheless increased due to electro-catalytic effects promoted by metal modification, and linear response obtained by differential pulse voltammetry for the determination of methyldopa (pH = 5.0) was between 10–180 μmol/L (Limit of Detection = 1 μmol/L) with the TiO2@CPE sensor. Furthermore, the constructed sensor was successfully applied in the detection of methyldopa in pharmaceutical formulations and excipients promoted no interference, that indicates that the sensor herein developed is a cheap, reliable, and useful strategy to detect methyldopa in pharmaceutical samples, and may also be applicable in determinations of similar compounds.


2015 ◽  
Vol 19 (05) ◽  
pp. 679-687 ◽  
Author(s):  
Ramona Georgescu ◽  
Jacobus Frederick van Staden ◽  
Raluca-Ioana Stefan-van Staden ◽  
Cristian Boscornea

Nineteen amperometric dot microsensors based on graphite and graphene modified with a selection of porphyrins and phthalocyanines were evaluated and tested for their ability of the analysis of folic acid in pharmaceutical tablets (e.g. Acifol) and biological samples (e.g. urine), using differential pulse voltammetry. Cyclic voltammetry was used to optimize the working conditions, e.g. pH and electrolyte for the proposed amperometric dot microsensors. The optimum working pH was 7.0 (phosphate buffer), with a 0.1 M potassium chloride supporting electrolyte. The linear concentration ranges for folic acid were between 10-6 and 10-3) M for all dot microsensors except dot microsensors based on graphite modified with tetraamino cobalt(II) phthalocyanine and tetranitro manganese(II) phthalocyanine which had linear concentration ranges between 10-6 and 10-4 M . The highest sensitivity (0.770 nA. mmolL-1) was recorded for the graphite modified with tetraamino cobalt(II) phthalocyanine based dot sensor and the lowest limit of detection (1.14 10-7 M ) for the graphite modified with tetranitro zinc(II) phthalocyanine based dot sensor. The dot sensors were used for the reliable analysis of folic acid in Acifol tablets and urine samples, with recoveries higher than 94.00% and 99.00%, respectively.


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