Analytical and Bioanalytical Chemistry

, Volume 399, Issue 8, pp 2863–2875 | Cite as

Comparison of the efficiency of different extraction methods for the simultaneous determination of mycotoxins and pesticides in milk samples by ultra high-performance liquid chromatography-tandem mass spectrometry

  • M. M. Aguilera-Luiz
  • P. Plaza-Bolaños
  • R. Romero-González
  • J. L. Martínez Vidal
  • A. Garrido Frenich
Original Paper


A rapid multi-analyte method has been developed for the simultaneous determination of pesticides and mycotoxins in milk by ultra high-performance liquid chromatography coupled to triple quadrupole mass spectrometry (UHPLC–QqQ–MS/MS). A variety of methodologies has been evaluated, including solid-phase extraction (SPE), “dilute-and-shoot” (liquid–liquid extraction-based procedures), and QuEChERS (quick, easy, cheap, effective, rugged, and safe)-based methods. The optimization and development process was carried out considering that the maximum residue level for aflatoxin M1 (AFM1) in milk in the European Union (EU) is set at 0.05 μg kg−1, which is the lowest tolerance in the target compounds. The selected method consisted of an extraction by SPE using C18 as sorbent and methanol as elution solvent. The final determination was performed by UHPLC–QqQ–MS/MS. Matrix-matched standard calibration was used for quantification, obtaining recoveries in the range 60–120% with relative standard deviations <25%, at three spiking levels: 0.5, 10, and 50 μg kg−1 (ten times lower for AFM1). Limits of quantification ranged from 0.20 to 0.67 μg kg−1, which were always below or equal to the established tolerance levels by the EU. Finally, the selected method was applied to different types of milk.


Mycotoxins Pesticides Milk Analysis SPE UHPLC–QqQ–MS/MS 



The authors gratefully acknowledge the Spanish Ministry of Science and Innovation (MICINN-FEDER) for financial support (Project Ref. AGL2006-12127-C02-01 and CTQ2009-07686). MMAL acknowledges her grant (F.P.U.) from the Spanish Ministry of Science and Innovation (Ref. AP2008-02811). PPB is grateful for personal funding through Juan de la Cierva Program (Spanish Ministry of Science and Innovation-European Social Fund, SMSI-ESF). RRG is also grateful for personal funding through the Ramón y Cajal Program (SMSI-ESF).


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Copyright information

© Springer-Verlag 2011

Authors and Affiliations

  • M. M. Aguilera-Luiz
    • 1
  • P. Plaza-Bolaños
    • 1
    • 2
  • R. Romero-González
    • 1
  • J. L. Martínez Vidal
    • 1
  • A. Garrido Frenich
    • 1
  1. 1.Group “Analytical Chemistry of Contaminants”, Department of Hydrogeology and Analytical ChemistryUniversity of AlmeriaAlmeriaSpain
  2. 2.Department of Analytical ChemistryUniversity of Granada, Campus de FuentenuevaGranadaSpain

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