Development and validation according to European Union Decision 2002/657/EC of an HPLC‐DAD method for milk multi‐residue analysis of penicillins and amphenicols based on dispersive extraction by QuEChERS in MSPD format

Abstract

A precise and reliable method for milk residue analysis regarding five penicillins and three amphenicols by HPLC-diode array detection has been developed herein. The chromatographic separation was performed using a mobile phase of CH3 COONH4 (0.05 M) and ACN delivered by gradient program on a Kinetex(™) -C18 core-shell, 2.6 μm column, starting at a volume ratio of 95:5 and ending at 60:40 after 17 min, remaining stable for 3 more min. A modified matrix solid phase dispersion procedure was applied for the extraction and clean-up procedure of antibiotics using a mixture of Strata by Phenomenex and QuEChERS as a sorbent. The method was validated at the respective 0.5× MRL, MRL and 1.5 ×MRL level for each compound. Results were quantitated against the internal standard paracetamol (2 ng/μL) according to the matrix-matched approach. The method was validated in line with the EC guidelines as cited in the Decision 2002/657/EC. The within-laboratory reproducibility, expressed as a RSD, never exceeded 16%. All decision limit (CCα) values lay in the range between 35.2 and 56.3 μg/kg and the corresponding results for detection capability (CCβ) were 39.9 and 61.9 μg/kg. Ruggedness was estimated according to the Youden approach.

Multiplug filtration cleanup method with multi-walled carbon nanotubes for the analysis of malachite green, diethylstilbestrol residues, and their metabolites in aquatic products by liquid chromatography–tandem mass spectrometry

“…Therefore, lower detection limits were reached. Since no MRL was established for MG, DES, and their metabolites, according to 2002/657/EC guidelines, the CC α and CC β values were calculated at LOQ levels [26]. The minimum required performance levels (MRPL) was introduced by the 2002/657/EC decision.…”

Current Trends in Sample Treatment Techniques for Environmental and Food Analysis

“…The extraction of veterinary drugs residues from animal tissues [98] and from milk [95,99,100] has also been described. For instance in [95] the use of QuEChERS was proposed as a fast sample treatment for a rapid screening method in the identification of 21 veterinary drug residues in milk.…”

Depletion of florfenicol and florfenicol amine residues in chicken eggs

“…Drug residues in eggs result from the misuse of medicated feed, contaminated feed and administration of extra-label drug (Goetting et al, 2011;Sireli et al, 2006). Even though FF has not been approved for use in laying hens, it has been administered as an extra-label drug.…”