Department of Veterinary Pharmacology and Toxicology, College of Veterinary Medicine, Konkuk University, Seoul, Republic of Korea.
J Sep Sci. 2010 Apr;33(8):1034-43. doi: 10.1002/jssc.200900772.
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-C(18) 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 microg/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.
本研究建立了一种无需净化步骤即可同时提取和测定猪肌肉、鸡蛋和商品全牛奶中 7 种氟喹诺酮类（丹诺沙星、二氟沙星、恩诺沙星、马波沙星、奥比沙星、氧氟沙星和沙拉沙星）和 3 种喹诺酮类（恶喹酸、氟甲喹和萘啶酸）残留的简化方法。该方法通过液液萃取从样品中提取分析物，然后通过 LC-荧光检测进行定量测定。分析物的分离在 XBridge-C(18)柱上成功进行，采用由乙腈和 0.01 M 草酸缓冲液（pH=3.5）组成的线性梯度流动相。一步液液萃取法具有良好的选择性、精密度（RSDs=0.26-15.07%）和提取分析物的回收率，在基质中的回收率为 61.12-115.93%。LOQs 范围为 0.3-25μg/kg。对当地市场购买的 10 个样品进行了调查，均未检出氟喹诺酮类残留。与现有的方法相比，该方法有所改进，因为无需额外的净化步骤。
