This article describes a differential pulse voltammetric (DPV) method for the determination of diclofenac in pharmaceutical preparations and human serum. The proposed method was based on electro-oxidation of diclofenac at platinum electrode in 0.1 M TBAClO 4 /acetonitrile solution. The well-defined two oxidation peaks were observed at 0.87 and 1.27 V, respectively. Calibration curves that obtained by using current values measured for second peak were linear over the concentration range of 1.5-17.5 μg mL -1 and 2-20 μg mL -1 in supporting electrolyte and serum, respectively. Precision and accuracy were also checked in all media. Intra-and inter-day precision values for diclofenac were less than 3.87, and accuracy (relative error) was better than 4.12%. The method developed in this study is accurate, precise and can be easily applied to Diclomec, Dicloflam and Voltaren tablets as pharmaceutical preparation. In addition, the proposed technique was successfully applied to spiked human serum samples. No electroactive interferences from the endogenous substances were found in human serum.Uniterms: Diclofenac/determination. Differential pulse voltammetry/quantitative analysis. Pharmaceutical formulations/analysis. Human serum/analysis Este artigo descreve um método de voltametria de pulso diferencial (VPD) para a determinação de diclofenaco em preparações farmacêuticas e em soro humano. O método proposto foi baseado em eletroxidação de diclofenaco no eléctrodo de platina em solução 0,1 M TBAClO 4 /acetonitrila. Dois picos de oxidação bem definidos foram observados em 0,87 e 1,27 V, respectivamente. As curvas de calibração obtidas utilizando-se valores de corrente medidos por segundo pico foram lineares no intervalo de concentração de 1,5-17,5 μg mL -1 e 2-20 μg mL -1 em eletrólito suporte e soro, respectivamente. Precisão e exatidão também foram verificadas em todos os meios. Valores de precisão intra-e inter-dia para o diclofenaco foram inferiores a 3.87 e a precisão (erro relativo) foi melhor do que 4,12%. O método desenvolvido neste estudo é exato, preciso e pode ser facilmente aplicado a Diclomec, Dicloflam e comprimidos Voltaren, como preparação farmacêutica. Além disso, a técnica proposta foi aplicada com sucesso em amostras de soro humano. Não se observaram interferências das substâncias endógenas no soro humano.Unitermos: Diclofenaco/determinação. Voltametria de pulso diferencial/análise quantitativa. Formulações farmacêuticas/análise. Soro humano/análise.
A simple and rapid electrochemical method for the determination of atorvastatin in pharmaceutical preparations was developed. The anodic peak at 1.07 V obtained in a buffer on glassy carbon electrode was used for analysis. The peak current and peak potential depends on pH, scan rate and initial potential. Decrease of the anodic peak with increasing pH, as well as deviations from linear plots of ip=f(C) and i=kv 1/2 indicate that this peak at higher concentrations is affected by adsorption-desorption phenomena. The calibration curves were linear for atorvastatin at the concentration range of 1-50 µg/ml or square wave and differential pulse voltammetry methods, respectively. Intra and interday precision values for atorvastatin were less than 3.17, and accuracy (relative error) was better than 1.93%. The mean recovery of atorvastatin was 100.4% for pharmaceutical preparations. Limits of detection were 0.3 µg/ml and 0.2 µg/ml for square wave and differential pulse voltammetry, respectively. Developed methods in this study are accurate, precise and can be easily applied to Ator, Cholvast and Lipitor tablets as pharmaceutical preparation.Key words: Atorvastatin, cyclic voltammetry, square wave voltammetry, differential pulse voltammetry, glassy carbon electrode Atorvastatin, (Fig. 1) an antihyperlipoproteinemic drug, inhibits 3-hydroxy-3-methylglutaryl coenzyme A (HMG-CoA) reductase, a key enzyme in the biosynthesis of cholesterol [1,2] . Using of atorvastatin leads to reducing the total cholesterol, low-density lipoprotein cholesterol [3] , apo-B [4] , triglycerides levels [5] , and C-reactive protein (CRP) [6] as well as increasing high density lipids (HDL) levels. This drug also stabilizes plaque and prevents risk of strokes, heart attack or other heart complications through antiinflammatory and other mechanisms.Several methods have been reported for the determination of atorvastatin in pharmaceutical formations and in biological fluids including reversedphase high performance liquid chromatography (RP-HPLC) [7,8] , liquid chromatography tandem mass spectrometry (LC-MS) [9] , high performance liquid chromatography (HPLC) [10] and spectrophotometry [11,12] . There are some problems encountered in using such methods. Spectrophotometric methods suffer from low sensitivity. Chromatographic methods are relatively slow and expensive and they require derivatization or time consuming extraction procedures. Thus, the use of simpler, faster and less expensive, but still sensitive electrochemical techniques can be considered as a useful alternative. Different methods are reported on
In this study, simple, fast and reliable cyclic voltammetry, linear sweep voltammetry, square wave voltammetry and differential pulse voltammetry methods were developed and validated for determination of etodolac in pharmaceutical preparations. The proposed methods were based on electrochemical oxidation of etodolac at platinum electrode in acetonitrile solution containing 0.1 M lithium perchlorate. The well-defined oxidation peak was observed at 1.03 V. The calibration curves were linear for etodolac at the concentration range of 2.5-50 μg/ml for linear sweep, square wave and differential pulse voltammetry methods, respectively. Intra- and inter-day precision values for etodolac were less than 4.69, and accuracy (relative error) was better than 2.00%. The mean recovery of etodolac was 100.6% for pharmaceutical preparations. No interference was found from three tablet excipients at the selected assay conditions. Developed methods in this study are accurate, precise and can be easily applied to Etol, Tadolak and Etodin tablets as pharmaceutical preparation.
Objective: In this study, new, rapid UV spectrophotometry (UV) and first-order derivative spectrophotometry ( 1 D) methods were developed for the determination of atorvastatin in pure and tablets. Methods: The solvent system and wavelength of detection were optimized in order to maximize the sensitivity of the proposed methods. Parameters such as linearity, precision, accuracy, specificity, stability, limit of detection and limit of quantification were studied according to the International Conference on Harmonization Guidelines.Results: Calibration curve was linear between the concentration range of 5-20 μg ml -1. Within-and between-day precision values for atorvastatin were less than 4.57%, and accuracy (relative error) was better than 3.17%. The mean recovery value of atorvastatin was 100.1% for pharmaceutical preparations. Conclusion: The developed methods were successfully applied to tablet formulations and the results were compared statistically with each other.
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