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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
Sigma-Aldrich
Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
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Hydrochloric acid solution, 0.2 M
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Hydrochloric acid solution, 0.02 M
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Hydrochloric acid solution, 1 M
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Acetone, SAJ first grade, ≥99.0%
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Hydrochloric acid solution, 6 M
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Acetone, ≥99.5%, for residue analysis
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Hydrogen chloride – ethanol solution, 0.1 M in ethanol
Sigma-Aldrich
Hydrochloric acid solution, 12 M
Sigma-Aldrich
Diethyl ether, JIS 300, ≥99.5%, for residue analysis
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Hydrochloric acid solution, 0.5 M
Sigma-Aldrich
Sodium hydroxide solution, 7 M
Sigma-Aldrich
Hydrochloric acid solution, 0.05 M
Sigma-Aldrich
Diethyl ether, JIS special grade, ≥99.5%
Sigma-Aldrich
Ammonium acetate solution, 50 % (w/v), for copper determination
Sigma-Aldrich
Hydrochloric acid solution, 2 M
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Acetone, JIS special grade, ≥99.5%
Sigma-Aldrich
Sodium hydroxide solution, 0.01 M
Sigma-Aldrich
Hydrochloric acid solution, 0.01 M
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Sodium hydroxide solution, 4 M
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Sodium hydroxide solution, 6 M
Sigma-Aldrich
Sodium hydroxide, JIS special grade, ≥96.0%
Sigma-Aldrich
Diethyl ether, SAJ first grade, ≥99.0%
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Acetone, for residue analysis, ≥99.5%
Sigma-Aldrich
tert-Butyl methyl ether, SAJ special grade, ≥99.0%
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Diethyl ether, ≥99.5%
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Hydrochloric acid, SAJ first grade, 35.0-37.0%
Sigma-Aldrich
Diethyl ether, JIS 1000, ≥99.5%, for residue analysis
Sigma-Aldrich
Sodium hydroxide solution, 1 M