Yang JinJing, Sun GuiZhi, Qian MingRong, Huang LingLi, Ke XianBing, Yang Bo
National Reference Laboratory of Veterinary Drug Residues/MOA Key Laboratory of Food Safety Evaluation, Huazhong Agricultural University, Wuhan 430070, PR China.
Hubei Engineering Research Center of Viral Vector, Wuhan Institute of Bioengineering, Wuhan 430415, PR China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Nov 15;1068-1069:9-14. doi: 10.1016/j.jchromb.2017.09.045. Epub 2017 Sep 29.
An effective thin layer chromatography (TLC) purification procedure coupled to high-performance liquid chromatography (HPLC) method was developed for the determination of florfenicol (FF) in pig, chicken and fish feedstuffs. The feedstuff samples were extracted with ethyl acetate, defatted with n-hexane saturated with acetonitrile, and further purified by TLC. The chromatographic separation was performed on a Waters Symmetry C column using an isocratic procedure with acetonitrile-water (35:65, v/v) at 0.6mL/min. The ultraviolet (UV) detector was set at a wavelength of 225nm. The FF concentrations in feedstuff samples were quantified using a standard curve. Good linear correlations (y=159075x-15054, r>0.9999) were achieved within the concentration range of 0.05-200μg/mL. The recoveries of FF spiked at levels of 1, 100 and 1000μg/g ranged from 80.6% to 105.3% with the intra-day and inter-day relative standard deviation (RSD) less than 9.3%. The limit of detection (LOD) and limit of quantitation (LOQ) were 0.02 and 0.06mg/kg for pig feedstuffs, 0.02 and 0.07mg/kg for chicken feedstuffs, and 0.02 and 0.05mg/kg for fish feedstuffs, respectively. This reliable, simple and cost-effective method could be applied to the routine monitoring of FF in animal feedstuffs.
建立了一种有效的薄层色谱（TLC）纯化方法与高效液相色谱（HPLC）方法相结合的方法，用于测定猪、鸡和鱼饲料中的氟苯尼考（FF）。饲料样品用乙酸乙酯提取，用乙腈饱和的正己烷脱脂，再通过TLC进一步纯化。色谱分离在Waters Symmetry C柱上进行，采用等度洗脱程序，以乙腈 - 水（35:65，v/v）为流动相，流速为0.6mL/min。紫外（UV）检测器设置在225nm波长处。饲料样品中的FF浓度通过标准曲线进行定量。在0.05 - 200μg/mL的浓度范围内，线性关系良好（y = 159075x - 15054，r > 0.9999）。在1、100和1000μg/g加标水平下，FF的回收率在80.6%至105.3%之间，日内和日间相对标准偏差（RSD）小于9.3%。猪饲料的检测限（LOD）和定量限（LOQ）分别为0.02和0.06mg/kg，鸡饲料为0.02和0.07mg/kg，鱼饲料为0.02和0.05mg/kg。这种可靠、简单且经济高效的方法可应用于动物饲料中FF的常规监测。
