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Development and validation of an HPLC confirmatory method for the determination of seven tetracycline antibiotics residues in milk according to the European Union Decision 2002/657/EC

Journal of separation science, 2007-10, Vol.30 (15), p.2430-2439 [Peer Reviewed Journal]

Copyright © 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim ;2008 INIST-CNRS ;ISSN: 1615-9306 ;EISSN: 1615-9314 ;DOI: 10.1002/jssc.200700057 ;PMID: 17628871

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Title:
Development and validation of an HPLC confirmatory method for the determination of seven tetracycline antibiotics residues in milk according to the European Union Decision 2002/657/EC
Author: Samanidou, Victoria F. ; Nikolaidou, Konstantina I. ; Papadoyannis, Ioannis N.
Subjects: 2002/657/EC ; Animals ; Biological and medical sciences ; Chemistry Techniques, Analytical - methods ; Chromatography - methods ; Chromatography, High Pressure Liquid - methods ; Food Analysis - methods ; Food industries ; Fundamental and applied biological sciences. Psychology ; HPLC ; Milk ; Milk - metabolism ; Milk and cheese industries. Ice creams ; Quinolones - analysis ; Regression Analysis ; Reproducibility of Results ; Sensitivity and Specificity ; Solid Phase Extraction ; SPE ; Tetracyclines ; Validation
Is Part Of: Journal of separation science, 2007-10, Vol.30 (15), p.2430-2439
Description: An HPLC method with diode‐array detection, at 355 nm, was developed and validated for the determination of seven tetracyclines (TCs) in milk: minocycline (MNC), TC, oxytetracycline (OTC), methacycline (MTC), demeclocycline (DMC), chlortetracycline (CTC), and doxycycline (DC). Oxalate buffer (pH 4) was used with 20% TCA as a deproteinization agent for the extraction of analytes from milk followed by SPE. The separation was achieved on an Inertsil ODS‐3, 5 μm, 250×4 mm2 analytical column at ambient temperature. The mobile phase, a mixture of A: 0.01 M oxalic acid and B: CH3CN, was delivered using a gradient program. The procedure was validated according to the European Union decision 2002/657/EC determining selectivity, stability, decision limit, detection capability, accuracy, and precision. Mean recoveries of TCs from spiked milk samples (50, 100, and 200 ng/g) were 93.8–100.9% for MNC, 96.8–103.7% for OTC, 96.3–101.8% for TC, 99.4–107.2% for DMC, 99.4–102.9% for CTC, 96.3–102.7% for MTC, and 94.6–102.1% for DC. All RSD values were lower than 8.5%. The decision limits CCa calculated by spiking 20 blank milk samples at MRL (100 μg/kg) ranged from 101.25 to 105.84 μg/kg, while detection capability CCb from 103.94 to 108.88 μg/kg.
Publisher: Weinheim: WILEY-VCH Verlag
Language: English
Identifier: ISSN: 1615-9306
EISSN: 1615-9314
DOI: 10.1002/jssc.200700057
PMID: 17628871
Source: MEDLINE
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Development and validation of an HPLC confirmatory method for the determination of seven tetracycline antibiotics residues in milk according to the European Union Decision 2002/657/EC

Copyright © 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim ;2008 INIST-CNRS ;ISSN: 1615-9306 ;EISSN: 1615-9314 ;DOI: 10.1002/jssc.200700057 ;PMID: 17628871

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