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.

Different parameters of carbon ceramic electrodes (CCE) preparation, such as type of precursor, carbon material, catalyst amount, among others, significantly influence the morphological properties and consequently their electrochemical responses. This paper describes a 2³ factorial design (2 factors and 3 levels with central point replicates), which the factors analyzed were catalyst amount (HCl 12 mol L-1), graphite/precursor ratio, and precursor type (TEOS - tetraethoxysilane and MTMOS - methyltrimetoxysilane). The design resulted in a significant third order interaction for peak current values (Ipa) and a second order interaction for potential difference (ΔE), between thefactors studied, which could not be observed when using an univariated study.

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