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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

Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
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Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 3 mm × 8 in.
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Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 5 mm × 8 in.
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Hydrochloric acid solution, 32 wt. % in H2O, FCC
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Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
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Acetone, analytical standard
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Hydrochloric acid solution, ~6 M in H2O, for amino acid analysis
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Hydrogen chloride – 2-propanol solution, ~1.25 M HCl (T), for GC derivatization, LiChropur
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Diethyl ether, analytical standard
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Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
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Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
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Diethyl ether, puriss., dried over molecular sieve (H2O ≤0.005%), ≥99.8% (GC)
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Sodium hydroxide solution, BioUltra, for molecular biology, 10 M in H2O
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Sodium hydroxide solution, 49-51% in water, eluent for IC
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Sodium hydroxide, BioUltra, for luminescence, ≥98.0% (T), pellets
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Acetone, ≥99%, meets FCC analytical specifications
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Phosphoric acid solution, 85 wt. % in H2O, FCC, FG
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Ammonium acetate, 99.999% trace metals basis
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tert-Butyl methyl ether, anhydrous, 99.8%
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Hydrogen chloride – ethanol solution, ~1.25 M HCl, for GC derivatization, LiChropur
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Hydrogen chloride – methanol solution, ~1.25 m HCl (T), for GC derivatization, LiChropur
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Ammonium acetate, LiChropur, eluent additive for LC-MS
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Ammonia, anhydrous, ≥99.98%
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Phosphoric acid solution, NMR reference standard, 85% in D2O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube
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Acetone, suitable for HPLC, ≥99.9%