title: Validation of method for determination of different classes of pesticides in aqueous samples by dispersive liquid-liquid microextraction with liquid chromatography-tandem mass spectrometric detection.
abstract: In this study, a simple, rapid and efficient method has been developed for the extraction and preconcentration of different classes of pesticides, carbofuran (insecticide), clomazone (herbicide) and tebuconazole (fungicide) in aqueous samples by dispersive liquid-liquid microextraction (DLLME) coupled with liquid chromatography-tandem mass spectrometric detection. Some experimental parameters that influence the extraction efficiency, such as the type and volume of the disperser solvents and extraction solvents, extraction time, speed of centrifugation, pH and addition of salt were examined and optimized. Under the optimum conditions, the recoveries of pesticides in water at spiking levels between 0.02 and 2.0 microg L(-1) ranged from 62.7% to 120.0%. The relative standard deviations varied between 1.9% and 9.1% (n=3). The limits of quantification of the method considering a 50-fold preconcentration step were 0.02 microg L(-1). The linearity of the method ranged from 1.0 to 1000 microg L(-1) for all compounds, with correlation coefficients varying from 0.9982 to 0.9992. Results show that the method we propose can meet the requirements for the determination of pesticides in water samples. The comparison of this method with solid-phase extraction indicates that DLLME is a simple, fast, and low-cost method for the determination of pesticides in natural waters.
authors.affiliation: Programa de Pós-Graduação em Química Tecnológica e Ambiental, Escola de Química e Alimentos, Universidade Federal do Rio Grande, Av Itália, km 8 s/n, Rio Grande, Rio Grande do Sul State, 96201-900, Brazil.
authors.forename: Sergiane Souza
authors.initials: SS
authors.lastname: Caldas
authors.forename: Fabiane Pinho
authors.initials: FP
authors.lastname: Costa
authors.forename: Ednei Gilberto
authors.initials: EG
authors.lastname: Primel
mesh_terms: D002235:Carbofuran / Q000032:analysis / Q000302:isolation & purification; D005591:Chemical Fractionation; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D007555:Isoxazoles / Q000032:analysis / Q000302:isolation & purification; D023303:Oxazolidinones / Q000032:analysis / Q000302:isolation & purification; D010575:Pesticides / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014230:Triazoles / Q000032:analysis / Q000302:isolation & purification; D014867:Water / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis* / Q000737:chemistry / Q000302:isolation & purification
chemical_list: D007555:Isoxazoles; D023303:Oxazolidinones; D010575:Pesticides; D014230:Triazoles; D014874:Water Pollutants, Chemical; D014867:Water; C087114:tebuconazole; C095255:clomazone; D002235:Carbofuran