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  • Determination of fluoroquinolones in chicken feces - a new liquid-liquid extraction method combined with LC-MS/MS.

Determination of fluoroquinolones in chicken feces - a new liquid-liquid extraction method combined with LC-MS/MS.

Environmental toxicology and pharmacology (2014-10-13)
Franziska Janusch, Gesine Scherz, Siegrun A I Mohring, Gerd Hamscher
ABSTRACT

The application of antibiotics including fluoroquinolones to farming animals is widespread and may lead to the development of antibiotic resistance and other environmental effects. To calculate environmental loads and for a proper risk assessment it is necessary to determine the antibiotic concentration in feces. Therefore, a new liquid-liquid extraction method combined with HPLC-MS/MS for the detection of marbofloxacin, ciprofloxacin, enrofloxacin and difloxacin in chicken feces was developed. Recoveries ranged from 51.0% to 83.5%. LOQs were between 0.10 and 1.09μg/kg. Feces of chickens treated with an enrofloxacin dosage of 10mg/kg bodyweight revealed maximum enrofloxacin and ciprofloxacin concentrations of 61.3 and 18.8mg/kg. Both antibiotics could be detected in feces up to two days after the last application in notable amounts (∼1mg/kg). Thus, feces of recently medicated chickens should not be used as a fertilizer without any further processing.

MATERIALS
Product Number
Brand
Product Description

USP
Enrofloxacin, United States Pharmacopeia (USP) Reference Standard
Difloxacin hydrochloride, European Pharmacopoeia (EP) Reference Standard
Supelco
Enrofloxacin, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Ethyl acetate
Sigma-Aldrich
Ethyl acetate
Ciprofloxacin, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Phosphoric acid, ≥85 wt. % in H2O, ≥99.999% trace metals basis
Sigma-Aldrich
Ethylenediaminetetraacetic acid solution, 0.02% in DPBS (0.5 mM), sterile-filtered, BioReagent, suitable for cell culture
Sigma-Aldrich
2-Propanol, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%, poly coated bottles
Sigma-Aldrich
Ethyl acetate, anhydrous, 99.8%
Sigma-Aldrich
Phosphoric acid, 85 wt. % in H2O, 99.99% trace metals basis
Sigma-Aldrich
2-Propanol, anhydrous, 99.5%
Sigma-Aldrich
Phosphoric acid-16O4 solution, 70 wt. % in D2O, 99.9 atom % 16O
Sigma-Aldrich
Sodium hydroxide-16O solution, 20 wt. % in H216O, 99.9 atom % 16O
Supelco
Ciprofloxacin-d8 hydrochloride hydrate, VETRANAL®, analytical standard
Sigma-Aldrich
Dichloromethane, JIS 300, for residue analysis
Sigma-Aldrich
Sodium phosphate monobasic, SAJ special grade, 99.0-101.0%
Sigma-Aldrich
Dichloromethane, JIS special grade, ≥99.0%
Sigma-Aldrich
2-Propanol, SAJ first grade, ≥99.0%
Sigma-Aldrich
2-Propanol, JIS special grade, ≥99.5%
Sigma-Aldrich
Ethylenediaminetetraacetic acid, SAJ special grade, ≥99.0%
Sigma-Aldrich
Ethyl acetate, JIS 300, ≥99.5%, for residue analysis
Sigma-Aldrich
Ethyl acetate, JIS special grade, ≥99.5%
Sigma-Aldrich
Dichloromethane, SAJ first grade, ≥99.0%
Sigma-Aldrich
Phosphoric acid, JIS special grade, ≥85.0%
Sigma-Aldrich
Formic acid, SAJ first grade, 88.0-89.5%
Sigma-Aldrich
Phosphoric acid, SAJ first grade, ≥85.0%
Sigma-Aldrich
Potassium phosphate dibasic, SAJ first grade, ≥98.0%
Sigma-Aldrich
Ethyl acetate, SAJ first grade, ≥99.0%
Sigma-Aldrich
Formic acid, JIS special grade, ≥98.0%