title: Development and validation of an HPLC method for the determination of penicillin antibiotics residues in bovine muscle according to the European Union Decision 2002/657/EC.
abstract: A high-performance liquid chromatographic method was developed for the determination of five penicillins: penicillin G (PENG), penicillin V (PENV), oxacillin (OX), cloxacillin (CLO), and dicloxacillin (DICLO), in bovine muscle. Samples were macerated with a mixture of H(2)O/CH(3)CN (1:1) and purified using RP-8 Adsorbex SPE cartridges after centrifugation, with mean recovery from spiked samples higher than 89%. The separation of the examined penicillins was achieved on an analytical column, an Inertsil C8 5 microm, 250x4 mm(2), at ambient temperature. The mobile phase consisted of 0.1% TFA/ACN 50:50 v/v delivered isocratically at a flow rate of 1.1 mL/min. Analytes were monitored at 240 nm. The procedure was validated according to the European Union Decision 2002/657/EC by means of selectivity, stability, decision limit, detection capability, accuracy, and precision. Method's LOQ values achieved were 54 microg/kg for PENG and DICLO, 46 microg/kg for PENV, 16 microg/kg for OX, and 43 microg/kg for DICLO. The detection capabilities (CC(beta)) were 73.6 microg/kg for PENG, 29.1 microg/kg for PENV, 350.6 microg/kg for OX, 379.9 microg/kg for CLO, and 355.8 microg/kg for DICLO. The method was applied to various samples from the local market. Two penicillins were identified by photodiode array (PDA) detection and quantified.
authors.affiliation: Laboratory of Analytical Chemistry, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, Greece. samanidu@chem.auth.gr
authors.forename: Victoria F
authors.initials: VF
authors.lastname: Samanidou
authors.forename: Styliani A
authors.initials: SA
authors.lastname: Nisyriou
authors.forename: Ioannis N
authors.initials: IN
authors.lastname: Papadoyannis
mesh_terms: D000818:Animals; D002417:Cattle; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D004350:Drug Residues / Q000032:analysis* / Q000737:chemistry; D005062:European Union; D015394:Molecular Structure; D009132:Muscles / Q000187:drug effects*; D010406:Penicillins / Q000032:analysis* / Q000737:chemistry / Q000494:pharmacology*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
chemical_list: D010406:Penicillins