title: Simultaneous determination of thiamethoxam, clothianidin, and metazachlor residues in soil by ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry.
abstract: A rapid pioneering method has been developed to simultaneously determine residues of three pesticides (thiamethoxam, clothianidin, and metazachlor) in soil by ultrahigh performance liquid chromatography coupled to a mass spectrometry detector (quadrupole time-of-flight). An efficient extraction procedure (90-105% average analyte recoveries) has also been proposed, involving solid-liquid extraction by a mixture of water and methanol (60:40, v/v), centrifugation, and concentration. A chromatographic analysis of the compounds was achieved in 5.5 min by means of a core-shell technology based column (Kinetex®EVO C18, 50 × 2.1 mm, 1.7 μm, 100 Å). The mobile phase (0.3 mL/min, gradient elution mode) consisted of 0.1% v/v formic acid in water and 0.1% v/v formic acid in acetonitrile. The method was fully validated in terms of selectivity, detection and quantification limits, matrix effect, linearity, trueness, and precision. Low limits of detection and quantification were obtained, ranging from 0.2 to 3.0 μg/kg, which are similar to those published in previous studies, while the absence of a significant matrix effect allowed quantification of the pesticides with standard calibration curves. The proposed method was applied for an analysis of pesticides in several soil samples from experimental fields dedicated to oilseed rape cultivars.
authors.affiliation: IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011, Valladolid, Spain.
authors.forename: Silvia
authors.initials: S
authors.lastname: Valverde
authors.affiliation: IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011, Valladolid, Spain.
authors.forename: Ana M
authors.initials: AM
authors.lastname: Ares
authors.affiliation: IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011, Valladolid, Spain.
authors.forename: José Luis
authors.initials: JL
authors.lastname: Bernal
authors.affiliation: IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011, Valladolid, Spain.
authors.forename: María Jesús
authors.initials: MJ
authors.lastname: Nozal
authors.affiliation: IU CINQUIMA, Analytical Chemistry Group, University of Valladolid, 47011, Valladolid, Spain.
authors.forename: José
authors.initials: J
authors.lastname: Bernal
keywords: core-shell columns; liquid chromatography; mass spectrometry; pesticides; soil