Screening of pesticides in blood with liquid chromatography–linear ion trap mass spectrometry |
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Authors: | Sylvain Dulaurent Christian Moesch Pierre Marquet Jean-Michel Gaulier Gérard Lachâtre |
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Institution: | (1) Department of Pharmacology and Toxicology, CHU de Limoges, 87042 Limoges, France;(2) University of Limoges, 87032 Limoges, France;(3) INSERM U850, 87025 Limoges, France |
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Abstract: | In clinical or forensic toxicology, general unknown screening procedures are used to identify as many xenobiotics as possible,
belonging to numerous chemical classes. We present here a general unknown screening procedure based on liquid chromatography
coupled with use of a single linear ion trap mass spectrometer, and focus on the identification of pesticides and/or metabolites
in whole blood. After solid-phase extraction (SPE), the compounds of interest were separated using a reversed-phase column
and identified by the mass spectrometer operated first in the full-scan mass spectrometry (MS) mode, in the positive and negative
polarities, followed by MS2 and MS3 scanning of ions selected in data-dependent acquisition. The total scan time was 2.45 s. Two mass spectral libraries (MS2 and MS3), each of 450 spectra, were created for the 320 pesticides and metabolites detected after injection of pure solutions. Robustness
of the spectra and matrix effects were studied and were satisfactory for the present application. Detection limits for the
320 compounds were studied by extracting 1 mL spiked blood at concentrations between 10 μg/L and 10 mg/L. If necessary, it
was possible to decrease the detection limits of some compounds by 10–100-fold by scanning MS2 in only one polarity, owing to a shorter total scan time. However, at the same time, the detection specificity decreased
as no confirmation could be recorded in the following MS3 scan and no information could be registered in the other polarity. So, in these rare cases, confirmation by another method
was required. |
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