4.6 Article

Comprehensive qualitative and quantitative determination of pesticides and veterinary drugs in honey using liquid chromatography-Orbitrap high resolution mass spectrometry

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1248, Issue -, Pages 130-138

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2012.05.088

Keywords

Exact mass database; High resolution Orbitrap mass spectrometry; Pesticide; Veterinary drug; Generic extraction; Honey

Funding

  1. Spanish Ministry of Economy and Competitiveness (MINECO)
  2. FEDER [AGL2010-21370]
  3. MINECO [AGL2010-21370]
  4. Juan de la Cierva Program (MINECO-European Social Fund, ESF)
  5. Ramon y Cajal Program (MINECO-ESF)

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A database has been created for the simultaneous analysis of more than 350 pesticides and veterinary drugs (including antibiotics) using ultra-high performance liquid chromatography coupled to high resolution Orbitrap mass spectrometry (UHPLC-Orbitrap-MS). This is a comprehensive exact mass database built using the Exactive-Orbitrap analyzer. The developed database includes exact masses of the target ions and retention time data, and allows the automatic search of the included compounds. Generic chromatographic and MS conditions have been applied. The presented database is suitable for qualitative analysis, and it was also evaluated for quantitative purposes in routine analysis, after the optimization and validation of a generic extraction method in honey samples. Adequate recovery and precision values for most of the studied analytes were obtained and the limits of detection (LOD) ranged from 1 to 50 mu g kg(-1). For pesticides, LODs were always lower than the MRLs established by European Union in honey, except for a few compounds. This method was applied to the analysis of 26 real honey samples and some pesticides (azoxystrobin, coumaphos, dimethoate and thiacloprid) were detected in 4 samples. Azoxystrobin and coumaphos were determined in two different samples (organic honey) at 1.5 mu g kg(-1) and 5.1 mu g kg(-1). Veterinary drugs were not detected in the analyzed samples. (c) 2012 Elsevier B.V. All rights reserved.

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