快速溶剂萃取-高效液相色谱-紫外串联荧光检测法测定太平湖白鱼中4种氟喹诺酮类药物残留

Detection of residual fluoroquinolones in Taiping lake whitefish by ASE/HPLC/UV-FLD

目的利用快速溶剂萃取(ASE),反相高效液相色谱-紫外串联荧光检测技术,建立了检测太平湖白鱼中4种氟喹诺酮类药物残留的定量分析方法。方法以8%氨水乙腈作为提取溶剂,对样品中的氟喹诺酮类药物采用快速溶剂萃取仪提取,萃取液经正己烷和乙醚去脂净化,用高效液相色谱-紫外串联荧光检测器测定,外标法定量。结果试样在10～200μg/L范围内校正曲线呈良好的线性关系,4种物质的相关系数都在0.999以上。当添加水平为255、0μg/kg时,鱼肉中4种氟喹诺酮类药物的加标回收率在82.7%～95.6%,相对标准偏差在2.1%～4.1%(n=5),检出限为1.3～3.0μg/kg。结论方法快速,操作简便,准确可靠,可以用于白鱼实际样品中氟喹诺酮类药物的日常检测。

Objective To establish a ASE/HPLC/UV-FLD analytical method for the detection of four fluoroquinolones residues in Taiping lake whitefish.Methods Samples were extracted with 8%（V/V） ammonia in acetonitrile by accelerated solvent extractor（ASE）,and then were defatted with hexane and ethylether.The collected sample solutions were analyzed by high performance liquid chromatography（HPLC） with ultraviolet（UV） detector tandem programmable fluorescence detector（FLD） and quantified by external standard.Results The linearity of standard curve was in the range of 10-200 μg/L,and the correlation coefficient was higher than 0.999.The recoveries in spiked samples with fluoroquinolones were 82.7%-95.6%.The relative standard deviations were all below 5%（n=5）.The limits of detection were 1.3-3.0 μg/kg.Conclusion The method was rapid,simple,accurate and reliable and could be applied to detect fluoroquinolones in whitefish.