Hayes John M
Schering-Plough Research Institute, Analytical Development, 2000 Galloping Hill Rd, Kenilworth, NJ 07033, USA.
J AOAC Int. 2005 Nov-Dec;88(6):1777-83.
A simple, accurate, and reproducible assay was developed for the determination of Florfenicol in medicated fish feed. Florfenicol was extracted from ground feed into an acetonitrile-water mixture by shaking and sonication. A portion of the centrifuged extract was passed through an Envi-Carb solid-phase extraction cartridge, through which Florfenicol eluted unretained. The collected eluant was diluted to adjust for analyte concentration, and injected into a reversed-phase liquid chromatography system. Samples were quantitated by external standard analysis versus multilevel calibration solutions. The procedure is suitable for the quantitation of samples medicated with 0.2-4 g/kg Florfenicol. Accuracy was evaluated by 2 analysts, who determined recovery of Florfenicol from feeds fortified over a range of 0.1-6.0 g/kg. The average recovery was 100.5% (relative standard deviation, 1.2%). The linearity, accuracy, precision, reproducibility (interday and analyst), and selectivity of the method are presented. The detection and quantitation limits were determined to be 0.2 and 1.0 mg/kg, respectively.
开发了一种简单、准确且可重复的方法用于测定药饵鱼饲料中的氟苯尼考。通过振荡和超声处理，将氟苯尼考从粉碎的饲料中萃取到乙腈 - 水混合液中。取一部分离心后的萃取液通过Envi - Carb固相萃取柱，氟苯尼考未被保留地从该柱中洗脱出来。收集的洗脱液经稀释以调整分析物浓度，然后注入反相液相色谱系统。通过与多级校准溶液进行外标分析对样品进行定量。该方法适用于定量含0.2 - 4 g/kg氟苯尼考的药饵样品。由2名分析人员评估准确性，他们测定了在0.1 - 6.0 g/kg范围内添加氟苯尼考的饲料中氟苯尼考的回收率。平均回收率为100.5%（相对标准偏差为1.2%）。给出了该方法的线性、准确性、精密度、重现性（日间和分析人员间）以及选择性。检测限和定量限分别确定为0.2和1.0 mg/kg。
