Method development for simultaneous determination of polar and nonpolar pesticides in surface water by low-temperature partitioning extraction (LTPE) followed by HPLC-ESI-MS/MS
2019
de Barros, André Luis Correa | de Abreu, Cíntia Grossi | da Cunha, Camila Cristina Rodrigues Ferreira | da Silva Rodrigues, Daniel Aparecido | Afonso, Robson José de Cássia Franco | da Silva, Gilmare Antônia
During this research, chemometric approaches were applied for optimization of the low-temperature partitioning extraction (LTPE) for the simultaneous analysis of the pesticides: acephate, difenoconazole, fenamidone, fluazifop, fluazinam, methamidophos, and thiamethoxam from surface water samples and determination by high-performance liquid chromatography-electrospray ionization-tandem mass spectrometry. It was used the 2³ full factorial and the Doehlert experimental designs. The extraction technique was optimized by evaluating the effects of the three variables: sample pH, ionic strength (addition of Na₂HPO₄), and organic solvent volume. Considering the interest to find an optimal condition for all analytes simultaneously, the best extraction parameters found were as follows: pH = 5.33, concentration of Na₂HPO₄ = 0.0088 mol L⁻¹ and organic phase volume = 4.5 mL. The optimized methodology showed LOD and LOQ levels from 0.33 to 8.13 ng L⁻¹ and from 1.09 to 26.84 ng L⁻¹, respectively. The recovery values ranged from 38.37 and 99.83% and the RSD values varied from 2.33 to 18.92%. The method was applied to surface water analysis sampled in areas with intensive agricultural practices in Ouro Branco City, Minas Gerais, Brazil. The difenoconazole was detected in concentrations between 12.53 and 94.76 ng L⁻¹.
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