title: 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.
authors: Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece.
authors: Eftichia G
authors: EG
authors: Karageorgou
authors: Victoria F
authors: VF
authors: Samanidou
mesh_terms: D000818:Animals; D002701:Chloramphenicol / Q000032:analysis* / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000592:standards; D004350:Drug Residues / Q000032:analysis* / Q000737:chemistry; D005062:European Union; D008892:Milk / Q000737:chemistry*; D010406:Penicillins / Q000032:analysis* / Q000737:chemistry; D052616:Solid Phase Extraction; D013839:Thiamphenicol / Q000031:analogs & derivatives* / Q000032:analysis / Q000737:chemistry; D014465:Ultrasonics
chemical_list: D010406:Penicillins; D002701:Chloramphenicol; C035534:florfenicol; D013839:Thiamphenicol