Application of zirconium dioxide nanoparticle sorbent for the clean-up step in post-harvest pesticide residue analysis

The use of yttria-stabilized zirconium dioxide nanoparticles as d-SPE clean-up sorbent for a rapid and sensitive liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method for the determination of post-harvest fungicides (carbaryl, carbendazim, chlorpropham, diphenylamine, ethoxyquin, flutriafol, imazalil, iprodione, methomyl, myclobutanil, pirimiphos-methyl, prochloraz, pyrimethanil, thiabendazole, thiophanate-methyl and tolclofos-methyl) in orange and pear samples has been evaluated and validated. The sample preparation was a modification of the QuEChERS extraction method using yttria-stabilized zirconium dioxide and multi-walled carbon nanotubes (MWCNTs) nanoparticles as the solid phase extraction (d-SPE) clean-up sorbents prior to injecting the ten-fold diluted extracts into the LC system. By using the yttria-stabilized zirconium dioxide extraction method, more recoveries in the 70-120% range were obtained - thus this method was used for the validation. Quantification was carried out using a matrix-matched calibration curve which was linear in the 1-500 μg kg-1 range for almost all the pesticides studied. The validated limit of quantification was 10 μg kg-1 for most of the studied compounds, except chlorpropham, ethoxyquin and thiophanate-methyl. Pesticide recoveries at the 10 and 100 μg kg-1 concentration levels were satisfactory, with values between 77% and 120% and relative standard deviations (RSD) lower than 10% (n=5). The developed method was applied for the determination of selected fungicides in 20 real orange and pear samples. Four different pesticide residues were detected in 10 of these commodities; 20% of the samples contained pesticide residues at a quantifiable level (equal to or above the LOQs) for at least one pesticide residue. The most frequently-detected pesticide residues were carbendazim, thiabendazole and imazalil-all were below the MRL. The highest concentration found was imazalil at 1175 μg kg-1 in a pear sample. © 2015 Elsevier B.V. All rights reserved.

Bibliographic Details

Main Authors:	Uclés, A., Herrera López, S., Hernando Guil, María Dolores, Rosal, R., Ferrer, C., Fernández-Alba, A. R.
Format:	journal article biblioteca
Language:	English
Published:	Elsevier 2015
Subjects:	Post-harvest pesticides, Yttria-stabilized zirconium dioxide, Clean-up, LC–MS/MS, Pesticide residues, Recoveries,
Online Access:	http://hdl.handle.net/20.500.12792/5533 http://hdl.handle.net/10261/293957
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