Journal
JOURNAL OF SEPARATION SCIENCE
Volume 36, Issue 12, Pages 2020-2027Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/jssc.201300194
Keywords
Cephalosporins; Milk; MSPD; QuEChERS; Quinolones
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Funding
- European Union (European Social Fund - ESF)
- Greek national funds through the Operational Program Education and Lifelong Learning of the National Strategic Reference Framework (NSRF)-Research Funding Program: Heraclitus II
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A sensitive and selective confirmatory method for milk-residue analysis of ten quinolones and eight cephalosporins by LC-MS/MS has been developed herein. For the chromatographic separation of target analytes, a Perfectsil ODS-2 (250 x 4 mm, 5 m) analytical column was used and gradient elution was applied, using a mobile phase of 0.1% w/w TFA in water and 0.1% w/w TFA in ACN. Ultrasound-assisted matrix solid-phase dispersion procedure was applied for the extraction and clean-up procedure of antimicrobials agents from milk matrix using a mixture of Bond Elut Plexa sorbent and QuEChERS. The method was validated meeting the European Legislation determining selectivity, linearity response, trueness, precision (repeatability and between-day reproducibility), decision limit, detection capability, and ruggedness following the Youden approach. Recoveries of all antibiotics ranged from 81.7 to 117.9%, while RSD values were lower than 13.7%. Limits of quantification for all examined compounds ranged from 2.4 to 15.0 g/kg, substantially lower than the maximum residue limits established by the European Union (30-100 g/kg).
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