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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
Ammonia-14N, 99.99 atom % 14N
Supelco
Marbofloxacin, VETRANAL®, analytical standard
USP
Acetone, United States Pharmacopeia (USP) Reference Standard
Enrofloxacin for system suitability, European Pharmacopoeia (EP) Reference Standard
Supelco
Acetone, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Hydrochloric acid solution, 32 wt. % in H2O, FCC
Sigma-Aldrich
Ammonium acetate solution, 7.5 M
Sigma-Aldrich
Hydrochloric acid, BioReagent, 36.5-38.0%
Sigma-Aldrich
Hydrochloric acid solution, 1.0 N, BioReagent, suitable for cell culture
Supelco
tert-Butyl methyl ether, analytical standard
Supelco
Acetone, analytical standard
Supelco
Diethyl ether, analytical standard
Sigma-Aldrich
Ammonium acetate solution, BioUltra, ~5 M in H2O
Sigma-Aldrich
tert-Butyl methyl ether, anhydrous, 99.8%
Sigma-Aldrich
Isopropyl alcohol, ≥99.7%, FCC, FG
Supelco
Hydrogen chloride – ethanol solution, ~1.25 M HCl, LiChropur
Sigma-Aldrich
Diethyl ether
Supelco
Sodium hydroxide concentrate, 0.1 M NaOH in water (0.1N), Eluent concentrate for IC
Sigma-Aldrich
Acetone, natural, ≥97%
Sigma-Aldrich
Acetone, ≥99%, meets FCC analytical specifications
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Phosphoric acid solution, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
Sodium phosphate monobasic-16O4, 99.9 atom % 16O
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Ammonia solution, 4 M in methanol
Sigma-Aldrich
Ammonia solution, 0.4 M in THF
Sigma-Aldrich
Diethyl ether, contains 1 ppm BHT as inhibitor, anhydrous, ≥99.7%
Sigma-Aldrich
Acetone, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Acetone, Laboratory Reagent, ≥99.5%
Sigma-Aldrich
Sodium hydroxide, puriss. p.a., ACS reagent, K ≤0.02%, ≥98.0% (T), pellets
Sigma-Aldrich
Sodium hydroxide, reagent grade, 97%, powder
Sigma-Aldrich
Sodium hydroxide, BioXtra, ≥98% (acidimetric), pellets (anhydrous)