Document Detail

Multiresidue method for simultaneous determination of ten quinolone antibacterial residues in multimatrix/multispecies animal tissues by liquid chromatography with fluorescence detection: single laboratory validation study.
MedLine Citation:
PMID:  16156083     Owner:  NLM     Status:  MEDLINE    
Quinolone antibacterials are veterinary drugs authorized for use in food animal production. The analysis of residual amounts of drugs in food from animal origin is important for quality control of products for consumers. For this purpose, Maximum Residue Limits (MRLs) have been set up by a European Union Council Regulation on Veterinary Drug Residues (No. 90/2377/EEC and subsequent), and 8 quinolones received MRLs at concentration levels depending on both the matrix and the animal species of interest. A method was developed for screening and confirming 10 quinolone residues (ciprofloxacin, danofloxacin, difloxacin, enrofloxacin, flumequine, marbofloxacin, nalidixic acid, norfloxacin, oxolinic acid, sarafloxacin) in a wide variety of matrixes of different animal species. It involves extraction of the residues from the biological tissues/fluids by acidic aqueous solution, centrifugation and filtration prior to injection on a C18 narrow-bore column, and detection through a 3-step-mode fluorescence detector. The method was validated during a 2-week study for a set of 8 species-matrixes (i.e., bovine raw milk, bovine muscle, porcine muscle, porcine kidney, porcine liver, fish flesh and skin, poultry muscle, whole egg). Residues were quantified down to 15 microg/kg with limits of detection and quantitation ranging from 4 to 11 and 13 to 36 microg/kg, respectively, which are sufficient compared to the wide range of MRLs set for these substances (from 30 microg/kg for danofloxacin in milk to 1900 microg/kg for difloxacin in poultry liver). The limit of performance of the method in terms of CCalpha and CCbeta, the critical concentrations stated in the Decision No. 2002/657/EC and the ISO Standard No. 11843, has been calculated for the authorized (MRL) substances but only estimated in the case of the nonauthorized (non-MRL) substances.
Eric Verdon; Pierrick Couedor; Brigitte Roudaut; Pascal Sandérs
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Publication Detail:
Type:  Journal Article; Research Support, Non-U.S. Gov't    
Journal Detail:
Title:  Journal of AOAC International     Volume:  88     ISSN:  1060-3271     ISO Abbreviation:  J AOAC Int     Publication Date:    2005 Jul-Aug
Date Detail:
Created Date:  2005-09-12     Completed Date:  2005-10-31     Revised Date:  2013-04-24    
Medline Journal Info:
Nlm Unique ID:  9215446     Medline TA:  J AOAC Int     Country:  United States    
Other Details:
Languages:  eng     Pagination:  1179-92     Citation Subset:  IM    
Unité des Résidus de Médicaments Vétérinaires, BP 90203, 35302 Fougères, France.
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MeSH Terms
Anti-Infective Agents / analysis*
Chromatography / methods
Chromatography, Liquid
Ciprofloxacin / analogs & derivatives,  analysis
Drug Residues*
Fluoroquinolones / analysis
Food Analysis
Kidney / metabolism
Nalidixic Acid / analysis
Norfloxacin / analysis
Oxolinic Acid / analysis
Quinolones / analysis*
Reference Standards
Reproducibility of Results
Time Factors
Reg. No./Substance:
0/Anti-Infective Agents; 0/Fluoroquinolones; 0/Quinolones; 112398-08-0/danofloxacin; 115550-35-1/marbofloxacin; 14698-29-4/Oxolinic Acid; 389-08-2/Nalidixic Acid; 5Z7OO9FNFD/difloxacin; 70458-96-7/Norfloxacin; 85721-33-1/Ciprofloxacin; 93106-60-6/enrofloxacin; RC3WJ907XY/sarafloxacin; UVG8VSP2SJ/flumequine

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