title: Multiresidue LC-MS/MS analysis of cephalosporins and quinolones in milk following ultrasound-assisted matrix solid-phase dispersive extraction combined with the quick, easy, cheap, effective, rugged, and safe methodology.
abstract: 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 × 4 mm, 5 μm) 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 μg/kg, substantially lower than the maximum residue limits established by the European Union (30-100 μg/kg).
authors.affiliation: Department of Chemistry, Laboratory of Analytical Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
authors.forename: Eftichia
authors.initials: E
authors.lastname: Karageorgou
authors.forename: Antonis
authors.initials: A
authors.lastname: Myridakis
authors.forename: Euripides G
authors.initials: EG
authors.lastname: Stephanou
authors.forename: Victoria
authors.initials: V
authors.lastname: Samanidou
mesh_terms: D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis* / Q000302:isolation & purification; D002511:Cephalosporins / Q000032:analysis* / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000191:economics / Q000379:methods*; D004350:Drug Residues / Q000032:analysis* / Q000302:isolation & purification; D005506:Food Contamination / Q000032:analysis; D008892:Milk / Q000737:chemistry*; D015363:Quinolones / Q000032:analysis* / Q000302:isolation & purification; D052616:Solid Phase Extraction / Q000191:economics / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000191:economics / Q000379:methods*; D014465:Ultrasonics
chemical_list: D000900:Anti-Bacterial Agents; D002511:Cephalosporins; D015363:Quinolones