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

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-pha...

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Bibliographic Details
Published in:Analytical and bioanalytical chemistry 2011-03, Vol.399 (8), p.2863-2875
Main Authors: Aguilera-Luiz, M. M, Plaza-Bolaños, P, Romero-González, R, Martínez Vidal, J. L, Frenich, A. Garrido
Format: Article
Language:English
Subjects:
Analysis
Analytical Chemistry
Animals
Biochemistry
Cattle
Characterization and Evaluation of Materials
Chemistry
Chemistry and Materials Science
Chromatographic methods and physical methods associated with chromatography
Chromatography, High Pressure Liquid - methods
Exact sciences and technology
Extraction
Food Contamination - analysis
Food Science
High performance liquid chromatography
Laboratory Medicine
Liquid chromatography
Mass spectrometry
Methods
Methyl alcohol
Milk
Milk - chemistry
Monitoring/Environmental Analysis
Mycotoxins
Mycotoxins - analysis
Original Paper
Other chromatographic methods
Pesticide Residues - analysis
Pesticides
SPE
Spectrometric and optical methods
Tandem Mass Spectrometry - methods
Tolerances
UHPLC-QqQ-MS/MS
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Summary: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
ISSN:1618-2642
1618-2650
DOI:10.1007/s00216-011-4670-7