Response surface optimization for determination of pesticides residues in grapes using MSPD and GC/MS: assessment of global uncentainty.

  1. Lagunas-Allué, L. 1
  2. Sanz-Asensio, J. 1
  3. Martínez-Soria, M.T. 1
  1. 1 Universidad de La Rioja
    info

    Universidad de La Rioja

    Logroño, España

    ROR https://ror.org/0553yr311

Revista:
Analytical and Bioanalytical Chemistry

ISSN: 1618-2642

Año de publicación: 2010

Volumen: 398

Número: 3

Páginas: 1509-1523

Tipo: Artículo

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DOI: 10.1007/S00216-010-4046-4 PMID: 20694812 SCOPUS: 2-s2.0-77957846293 WoS: WOS:000281670400038 GOOGLE SCHOLAR

Otras publicaciones en: Analytical and Bioanalytical Chemistry

Resumen

In this work, a simple and low-cost method based on matrix solid-phase dispersion (MSPD) and gas chromatography to determine eight multi-class pesticides such as vinclozolin, dichlofluanid, penconazol, captan, quinoxyfen, fluquinconazol, boscalid, and pyraclostrobin in grapes is described. Fungicide residues were identified and quantified using gas chromatography-mass spectrometry in selected ion monitoring mode (GC-MS, SIM). The experimental variables that affect the MSPD method, such as the amount of solid phase, solvent nature and elution volume were optimized using an experimental design. The best results were obtained using 0.5 g of grapes, 1.0 g of silica as clean-up sorbent, 1.50 g of C18 as bonded phase and 10 mL of dichloromethane/ethyl acetate (1:1, v/v) as eluting solvent. Significant matrix effects observed for most of the pesticides tested were eliminated using matrix-matched standards. The pesticide recoveries in grapes samples were better than 80% except for captan. Intra-laboratory precision in terms of Horwitz ratio of the pesticides evaluated was below 0.5, suggesting ruggedness of the method. The quantification limits of the pesticides were in the range of 3.4-8.7 μg kg-1, which were lower than the maximum residue limits (MRLs) of the pesticides in grapes samples established by the European legislation. Decision limits (CCα) and detection capability (CCβ) have been calculated. The expanded uncertainties at two levels of concentration were <20% for all analytes. © 2010 Springer-Verlag.