Abstract

This paper shows the simultaneous electrochemical determination of dypirone (DIP) and paracetamol (PAR) by differential pulse voltammetry technique (DPV) using an unmodified carbon paste electrode. Because of the overlapping of the voltammetric peaks of DIP and PAR, the multivariate calibration methodology based on Partial Least Square Regression (PLSR) was proposed. The data pre-treatment used in this process was mean centering and to choose the principal component number a cross validation procedure was used (leave-one-out). Four principal components were necessary to obtain the lowest PRESS (Prediction Residual Error Sum of Squares). The statistics showed that this model explains approximately 95.5% of the variance from the data set. Using this model, high correlation between real and predicted concentrations was observed. However, for low concentrations of PAR the relative error increased to 25%. Comparing RMSEP (Root Mean Square of Error Prediction) between PAR and DIP, it was observed that it was lower for DIP probably due to higher analytical information in the voltammograms for this analyte when compared to the electrochemical process of PAR, which presented only one potential peak due to its irreversible oxidation.

Highlights

  • The development of analytical techniques for the rapid analysis of pharmaceuticals is important for quality and medical control

  • This paper reports the simultaneous electrochemical determination of dypirone (DIP) and paracetamol (PAR) by differential pulse voltammetry technique (DPV) using an unmodified carbon paste electrode

  • A multivariate calibration methodology based on Partial Least Square Regression (PLSR) using the Differential Pulse Voltammetry (DPV) was proposed

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Summary

Introduction

The development of analytical techniques for the rapid analysis of pharmaceuticals is important for quality and medical control. Vol 19, No 4, 2008 methods for simultaneous determination of pharmaceuticals without the necessity of a previous separation of the sample components, besides being rapid and with low cost To overcome these limitations, electrochemical methods, such as voltammetric ones were extensively used for their accuracies, precisions, simplicities and possibilities of analysis without tedious sample pre-treatment.[11,12]. While the Brazilian Pharmacopoeia uses a spectrophotometric technique.[24,25] there are many studies described in the literature using different analytical techniques for determination of this drug.[26,27,28,29,30] Some electrochemical methods have been used for analysis of paracetamol,[31,32,33] specially the voltammetric ones using chemically modified electrodes in order to improve the sensitivity.[34,35]. The data pre-treatment used in this process was mean centering and to choose the number of principal components a cross validation procedure was used (leave-one-out)

Preparation of the carbon paste electrodes
Simultaneous Voltammetric Determination of Dypirone and Paracetamol
Electrochemical measurements
Multivariate calibration methodology
Results and Discussion
Linear Regression Equation
Multivariate method
Conclusions
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