Simultaneous determination of thiamethoxam, clothianidin, and metazachlor residues in soil by ultrahigh performance liquid chromatography coupled to quadrupole time-of-flight mass spectrometry

作者：Valverde Silvia; Ares Ana M; Bernal Josc Luis; Nozal Mara Jesus; Bernal Jose

来源：Journal of Separation Science, 2017, 40(5): 1083-1090.

DOI：10.1002/jssc.201601143

• core-shell columns
• liquid chromatography
• mass spectrometry
• pesticides
• soil

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 amass spectrometry detector (quadrupole time-of-flight). An efficient extraction procedure (90105% 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 r EVO C18, 50 x 2.1 mm, 1.7 mu m, 100 angstrom). 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. Lowlimits of detection and quantificationwere obtained, ranging from 0.2 to 3.0 mu g/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.

• 出版日期2017-3