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Single‐step extraction followed by LC for determination of (fluoro)quinolone drug residues in muscle,eggs, and milk
Authors:Hee‐Jung Cho  Hee Yi  Soo Min Cho  Dong Goo Lee  Kyul Cho  A M Abd El‐Aty  Jae‐Han Shim  Soon‐Ho Lee  Ji‐Yoon Jeong  Ho‐Chul Shin
Institution:1. Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea;2. Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, Giza, Egypt;3. Natural Products Chemistry Lab., Department of Biological Chemistry, College of Agriculture and Life Science, Chonnam National University, Gwangju, Republic of Korea;4. Residue & Chemicals Team, Korea Food and Drug Administration, Seoul, Republic of Korea
Abstract:In this study, a simplified method for the extraction and determination of seven fluoroquinolone residues (danofloxacin, difloxacin, enrofloxacin, marbofloxacin, orbifloxacin, ofloxacin, and sarafloxacin) and three quinolones (oxolinic acid, flumequine, and nalidixic acid), in porcine muscle, table eggs, and commercial whole milk, which required no cleanup step, was devised. This procedure involves the extraction of analytes from the samples via liquid‐phase extraction, and the subsequent quantitative determination was accomplished via LC‐fluorescence detection. Analyte separation was successfully conducted on an XBridge‐C18 column, with a linear gradient mobile phase composed of acetonitrile and 0.01 M oxalic acid buffer at pH=3.5. The one‐step liquid‐liquid extraction method evidenced good selectivity, precision (RSDs=0.26–15.07%), and recovery of the extractable analytes, ranging from 61.12 to 115.93% in matrices. The LOQs ranged from 0.3 to 25 μg/kg. A survey of ten samples purchased from local markets was conducted, and none of the samples harbored fluoroquinolone residues. This method is an improvement over existing methodologies, since no additional cleanup was necessary.
Keywords:Egg  Fluoroquinolones  Milk  Porcine muscle  Residue analysis
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