A simplified reflectometric method for the rapid determination of dipyrone in pharmaceutical formulations

Abstract

This paper describes a simple, portable and environmentally friendly method for the rapid determination of dipyrone in pharmaceuticals by using diffuse reflectance spectroscopy. The proposed method is based on the reflectance measurements of the orange compound produced from the spot test reaction between dipyrone and p-dimethylaminocinnamaldehyde (p-DAC), in acid medium, using a filter paper as solid support. Experimental design methodologies were used to optimize the measurement conditions. All reflectance measurements were carried out at 510 nm and the linear range was from 1.42 <FONT FACE=Symbol>´</FONT> 10-4-2.85 <FONT FACE=Symbol>´</FONT> 10-3 mol L-1, with a correlation coefficient of 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 1.20 <FONT FACE=Symbol>´</FONT> 10-5 mol L-1 and 4.00 <FONT FACE=Symbol>´</FONT> 10-5 mol L-1, respectively. The intraday precision and interday precision were studied for 10 replicate analyses of 7.90 <FONT FACE=Symbol>´</FONT> 10-4 mol L-1 dipyrone solution. The coefficients of variation were 1.1 and 0.9%, respectively. The proposed method was applied successfully to the determination of dipyrone in commercial brands of pharmaceuticals. No interferences were observed from the common excipients in formulations. The results obtained by the proposed method were favorably compared with those given by the Brazilian Pharmacopoeia procedure at 95% confidence level.