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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
Hydrogen chloride solution, 3 M in cyclopentyl methyl ether (CPME)
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Acetone, natural, ≥97%
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Sodium phosphate monobasic-16O4, 99.9 atom % 16O
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Acetone, ≥99.5%, ACS reagent
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Ammonia-14N, 99.99 atom % 14N
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Marbofloxacin, VETRANAL®, analytical standard
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Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
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Hydrochloric acid solution, 32 wt. % in H2O, FCC
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Ammonium acetate, reagent grade, ≥98%
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Diethyl ether, analytical standard
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Diethyl ether, contains 1 ppm BHT as inhibitor, anhydrous, ≥99.7%
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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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Diethyl ether
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Isopropyl alcohol, ≥99.7%, FCC, FG
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Ammonium acetate, LiChropur, eluent additive for LC-MS
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Acetone, analytical standard
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Ammonium acetate, BioXtra, ≥98%
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Acetone, suitable for HPLC, ≥99.9%
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3-Ethyl-2,4-pentanedione, mixture of tautomers, 98%
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Hydrochloric acid, puriss., 24.5-26.0%
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Diethyl ether, ACS reagent, ≥98.0%, contains ≤2% ethanol and ≤10ppm BHT as inhibitor
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tert-Butyl methyl ether, puriss. p.a., ≥99.5% (GC)
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Acetone, Laboratory Reagent, ≥99.5%
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Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
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Acetone, ACS reagent, ≥99.5%
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Sodium hydroxide, reagent grade, 97%, powder
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Sodium hydroxide, anhydrous, free-flowing, Redi-Dri, reagent grade, ≥98%, pellets
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Diethyl ether, contains BHT as inhibitor, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8% (GC)