4.5 Article

Development of a procedure for the multiresidue analysis of pesticides in vineyard soils and its application to real samples

期刊

JOURNAL OF SEPARATION SCIENCE
卷 37, 期 16, 页码 2215-2224

出版社

WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201400298

关键词

Degradation products; Multiresidue analysis; Pesticides; Vineyard soils

资金

  1. Spanish Ministry of Science and Innovation [AGL2010-15976/AGR]
  2. European and Structural and Social Funds (FEDER-FSE)

向作者/读者索取更多资源

A procedure formultiresidue analysis was developed for the extraction and determination of 17 pesticides, including herbicides, fungicides, and insecticides, as well as certain degradation products, in vineyard soils from La Rioja region (Spain). Different solvents and mixtures were tested in spiked pesticide-free soils, and pesticides were comparatively evaluated by gas chromatography with mass spectrometry and liquid chromatography with mass spectrometry. Recoveries >70%, with relative standard deviations <9%, were obtained when a mixture of methanol/acetone or a mixture of methanol/CaCl2 0.01 M for the most polar compounds was selected as the extraction solvent. Method validation was accomplished with acceptable linearity (r(2) >= 0.987) within the concentration range of 0.005-1 mu g/mL corresponding to 1.667-333.4 mu g/kg and 0.835-167.1 mu g/kg for liquid chromatography with mass spectrometry and gas chromatography with mass spectrometry, respectively, and detection limits <0.4 mu g/kg for the compounds were studied. The extraction method was applied to 17 real vineyard soil samples, and terbuthylazine and its metabolite desethylterbuthylazine were the most ubiquitous compounds, as they were detected in the 100% of the soils analyzed. The presence of fungicides was also high, and the presence of insecticides was lower than other pesticides. The results confirm the usefulness of the optimized procedure for monitoring residues in vineyard soils.

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