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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

Sigma-Aldrich
Sodium hydroxide, AR, pellets, ≥98.5%
Marbofloxacin, European Pharmacopoeia (EP) Reference Standard
Supelco
tert-Butyl Methyl Ether, Pharmaceutical Secondary Standard; Certified Reference Material
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Hydrochloric acid, meets analytical specification of Ph. Eur., BP, NF, fuming, 36.5-38%
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Hydrochloric acid, puriss., 24.5-26.0%
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Sodium hydroxide, puriss., meets analytical specification of Ph. Eur., BP, NF, E524, 98-100.5%, pellets
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tert-Butyl methyl ether, puriss. p.a., ≥99.5% (GC)
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Acetone, ACS reagent, ≥99.5%
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Diethyl ether, ACS reagent, ≥98.0%, contains ≤2% ethanol and ≤10ppm BHT as inhibitor
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Ammonia solution, 2.0 M in methanol
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Ammonia solution, 0.4 M in dioxane
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Diethyl ether, reagent grade, ≥98%, contains ≤2% ethanol and ≤10ppm BHT as inhibitor
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Hydrogen chloride solution, 4.0 M in dioxane
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Hydrogen chloride solution, 2.0 M in diethyl ether
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Ammonia solution, 2.0 M in ethanol
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tert-Butyl methyl ether, HPLC Plus, for HPLC, GC, and residue analysis, 99.9%
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Ammonium acetate, ≥99.99% trace metals basis
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Diethyl ether, ACS reagent, anhydrous, ≥99.0%, contains BHT as inhibitor
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Diethyl ether, puriss., contains ~5 mg/L 2,6-di-tert.-butyl-4-methylphenol as stabilizer, meets analytical specification of Ph. Eur., BP, ≥99.5% (GC)
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tert-Butyl methyl ether, ACS reagent, ≥99.0%
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