Development of a dispersive liquid-liquid microextraction method for the determination of fluoroquinolones in chicken liver by high performance liquid chromatography.
A simple and cost effective sample pre-treatment method, dispersive liquid-liquid microextraction (DLLME), has been developed for the extraction of six fluoroquinolones (FQs) from chicken liver samples. Clean DLLME extracts were analyzed for fluoroquinolones using liquid chromatography with diode array detection (LC-DAD). Parameters such as type and volume of disperser solvent, type and volume of extraction solvent, concentration and composition of phosphoric acid in the disperser solvent and pH were optimized. Linearity in the concentration range of 30-500 μg kg(-1) was obtained with regression coefficients ranging from 0.9945 to 0.9974. Intra-day repeatability expressed as % RSD was between 4 and 7%. The recoveries determined in spiked blank chicken livers at three concentration levels (i.e. 50, 100 and 300 μg kg(-1)) ranged from 83 to 102%. LODs were between 5 and 19 μg kg(-1) while LOQs ranged between 23 and 62 μg kg(-1). All of the eight chicken liver samples obtained from the local supermarkets were found to contain at least one type of fluoroquinolone with enrofloxacin being the most commonly detected. Only one sample had four fluoroquinolone antibiotics (ciprofloxacin, difloxacin, enrofloxacin, norfloxacin). Norfloxacin which is unlicensed for use in South Africa was also detected in three of the eight chicken liver samples analyzed. The concentration levels of all FQs antibiotics in eight samples ranged from 8.8 to 35.3 μg kg(-1), values which are lower than the South African stipulated maximum residue limits (MRL).
Department of Chemistry, College of Science, Engineering and Technology, University of South Africa, Pretoria, South Africa.
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D000818:Animals; D000900:Anti-Bacterial Agents / Q000032:analysis*; D002645:Chickens; D002851:Chromatography, High Pressure Liquid / Q000379:methods; D002939:Ciprofloxacin / Q000031:analogs & derivatives / Q000032:analysis; D000077422:Enrofloxacin; D024841:Fluoroquinolones / Q000032:analysis*; D006863:Hydrogen-Ion Concentration; D057230:Limit of Detection; D059627:Liquid Phase Microextraction / Q000379:methods*; D008099:Liver / Q000737:chemistry*; D009643:Norfloxacin / Q000032:analysis; D012044:Regression Analysis; D013019:South Africa
D000900:Anti-Bacterial Agents; D024841:Fluoroquinolones; D000077422:Enrofloxacin; D002939:Ciprofloxacin; C047225:difloxacin; D009643:Norfloxacin