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 |
| |
Authors: | Aguilera-Luiz M M Plaza-Bolaños P Romero-González R Vidal J L Martínez Frenich A Garrido |
| |
Institution: | (1) Group “Analytical Chemistry of Contaminants”, Department of Hydrogeology and Analytical Chemistry, University of Almeria, 04071 Almeria, Spain;(2) Department of Analytical Chemistry, University of Granada, Campus de Fuentenueva, 18071 Granada, Spain; |
| |
Abstract: | 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. |
| |
Keywords: | |
本文献已被 PubMed SpringerLink 等数据库收录! |
|