Electroanalytical method for determination of the pesticide dichlorvos using gold-disk microelectrodes

This paper reports the use of laboratory-prepared gold microelectrodes and square-wave voltammetry for analytical determination of low concentrations of the pesticide dichlorvos in pure and natural water samples. After optimization of the experimental and voltammetric conditions, the best voltammetric responses-current intensity and voltammetric profile-were obtained in 0.1 mol L(-1) NaClO4 with f=100 s(-1), a=50 mV, and DeltaE(s)=2 mV. The observed detection and quantification limits in pure water were 7.8 and 26.0 microg L(-1), respectively. The reproducibility and repeatability of the method were also determined; the results were 1.4% (n=5) and 1.2% (n=10), respectively. Possible interfering effects were evaluated in natural water samples collected at different points with different levels of contamination from agricultural, domestic, or industrial waste from an urban stream. Results showed that the detection and quantification limits increased as a function of the quantity of organic matter present in the samples. Nonetheless, the values observed for these method characteristics were below the maximum value allowed by the Brazilian code for organophosphorus pesticides in water samples. Recovery curves constructed using the standard addition method were shown to be satisfactory compared with those obtained from high-performance liquid chromatography, confirming the suitability of the method for analysis of natural water samples. Finally, when the method was used to determine dichlorvos in spiked cows' milk samples, satisfactory recovery and relative standard deviations were obtained.