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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
Author(s) -
Samanidou Victoria F.,
Nisyriou Styliani A.,
Papadoyannis Ioannis N.
Publication year - 2007
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200700199
Subject(s) - dicloxacillin , chromatography , cloxacillin , chemistry , penicillin , detection limit , high performance liquid chromatography , european union , analyte , antibiotics , biochemistry , business , economic policy
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 μm, 250×4 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 μg/kg for PENG and DICLO, 46 μg/kg for PENV, 16 μg/kg for OX, and 43 μg/kg for DICLO. The detection capabilities (CC β ) were 73.6 μg/kg for PENG, 29.1 μg/kg for PENV, 350.6 μg/kg for OX, 379.9 μg/kg for CLO, and 355.8 μg/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.