Multi-residue determination of 130 multiclass pesticides in fruits and vegetables by gas chromatography coupled to triple quadrupole tandem mass spectrometry |
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Authors: | M I Cervera C Medina T Portolés E Pitarch J Beltrán E Serrahima L Pineda G Muñoz F Centrich F Hernández |
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Institution: | 1. Research Institute for Pesticides and Water, University Jaume I, Avda. Sos Baynat, 12071, Castellón de la Plana, Castellón, Spain 2. Chemistry laboratory, Public Health Agency of Barcelona (ASPB), 08001, Barcelona, Spain
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Abstract: | A multi-residue method has been developed and validated for the simultaneous quantification and confirmation of around 130
multiclass pesticides in orange, nectarine and spinach samples by GC-MS/MS with a triple quadrupole analyzer. Compounds have
been selected from different chemical families including insecticides, herbicides, fungicides and acaricides. Three isotopically
labeled standards have been used as surrogates in order to improve accurate quantitation. Samples were extracted by using
accelerated solvent extraction (ASE) with ethyl acetate. In the case of spinach, an additional clean-up step by gel permeation
chromatography was applied. Determination was performed by GC-MS/MS in electron ionization mode acquiring two MS/MS transitions
for each analyte. The intensity ratio between quantitation transition (Q) and identification transition (q) was used as confirmatory parameter (Q/q ratio). Accuracy and precision were evaluated by means of recovery experiments in orange, nectarine, and spinach samples
spiked at two concentration levels (0.01 and 0.05 mg/kg). Recoveries were, in most cases, between 70% and 120% and RSD were
below 20%. The limits of quantification objective for which the method was satisfactorily validated in the three samples matrices
were for most pesticides 0.01 mg/kg. Matrix effects over the GC-MS/MS determination were tested by comparison of reference
standards in pure solvent with matrix-matched standards of each matrix. Data obtained showed enhancement of signal for the
majority of analytes in the three matrices investigated. Consequently, in order to reduce the systematic error due to this
effect, quantification was performed using matrix-matched standard calibration curves. The matrix effect study was extended
to other food matrices such as raisin, paprika, cabbage, pear, rice, legume, and gherkin, showing in all cases a similar signal
enhancement effect. |
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