Veterinary Drugs Residue Methods


 



Category Antibacterial substances, including sulfonamides and quinolones
Drug Class Name Fluoroquinolone Antibiotics
Method Title Confirmation of Fluoroquinolone Antibiotics by HPLC Ion Trap Mass Spectrometry
Method Date 2006/01/13
Method Type Confirmatory, Quantitative
Scope and Application This method is suitable for confirming presence of the fluoroquinolones desethylene ciprofloxacin, difloxacin, enrofloxacin, norfloxacin, danofloxacin, desmethyl danofloxacin, ciprofloxacin and sarafloxacin in bovine liver and muscle.
Method Summary Fluoroquinolone antibiotics are extracted from homogenized bovine liver and muscle by centrifugation using a liquid/liquid technique. Acetonitrile, ammonium hydroxide, water, ethyl ether, hexane and 1M NaCl are used in this technique. Following evaporation of acetonitrile from the final extract, the sample residue is dissolved in 0.1M phosphate buffer (pH 9.0) and pressed through a 0.2 mircometer nylon syringe filter prior to analysis by HPLC ion trap mass spectrometry. A C18 Phenyl Zorbax analytical column is used. Desethylene ciprofloxacin and desmethyl danofloxacin are analyzed using HPLC/MS2, whereas difloxacin, enrofloxacin, norfloxacin, danofloxacin, ciprofloxacin and sarafloxacin are analyzed by HPLC/MS3.
Applicable Concentration Range The fluoroquinolones desethylene ciprofloxacin, difloxacin, enrofloxacin, norfloxacin, danofloxacin, desmethyl danofloxacin, ciprofloxacin and sarafloxacin may be analysed at the concentration level ≥ 25 µg kg-1 in bovine liver and muscle.
QC Requirements See attached SOP
Method Source USDA-FSIS
Method SOP PDF icon SOP 
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