Methodology using solid phase extraction and high performance liquid chromatography (SPE-C18/HPLC-DAD) was applied to pesticide determinations in ten water reservoirs in the semidarid region of northeastern Brazil. The validated method was suitable for determination of herbicides and insecticide in surface water. The recovery efficiency of atrazine, methyl-parathion and simazine was approximately 70%. The method also showed good linearity and selectivity with correlation coefficients (R) greater than 0.99. The limits of detection were below the maximum residue limits (MRLs) established by government agencies. Studied reservoirs showed presence of atrazine at mean levels from 7.0 to 15.0 µg/L. Simazine and methyl parathion were not detected during the period. The atrazine levels measured from this semiarid region are of the same magnitude as those found in regions with moderate to high agricultural activity. According to detected atrazine concentrations, the annual health risk to humans was insignificant. However, the control of herbicides is important to maintain the quality of water in the reservoirs of Ceará, Brazil.
The effects promoted by environmental aqueous matrices on pesticide determinations have been assessed, and for the first time, a simple, low-cost and efficient strategy for the correction of analytical results has been determined. This method can be useful as a parameter of quality control in a quality assurance programs. Evaluation of the matrix effect showed that environmental aqueous matrices, e.g., estuarine water, promote a distinctive and significant effect on the determination of pesticides. The picloram, atrazine and methyl parathion pesticides suffered the smallest effects promoted by the estuarine matrix, whereas chlorpyrifos and cypermethrin suffer a significant effect. For picloram, the matrix effect was a function of its physiochemical properties. However, for atrazine, methyl parathion, chlorpyrifos and cypermethrin, the matrix effect was promoted by environmental matrix components. As strategy for analytical quality control, it has been determined that there are relation factors (RFs) between pesticides and the selected surrogates standards. These RFs are not altered by the complexities and compositions of simple and complex aqueous matrices. Predetermined RFs was applied to the picloram, atrazine and methyl parathion assessment in a real sample from the estuary of the Jaguaribe River, and the results showed that when no quality control was applied, the concentration levels would be underestimated, leading to incorrect results and inaccurate conclusions.
Pesticides are used mostly in rural areas for agriculture, but urban pest control, public health campaigns, and household and veterinary products can also be important sources of these contaminants. This aim of this study was to estimate household pesticide contamination in sediments of two urban estuaries due to pest control: Cocó and Ceará rivers located in the metropolitan area of Fortaleza, Ceará, Brazil. Cypermethrin and malathion were found in both rivers. Cypermethrin levels had the same magnitudes as other studied urban areas and were highest in the estuary, while malathion was similar in both fluvial and estuarine zones.
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