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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 quantitative method for the determination of four fluoroquinolones residues in white fish of Taiping Lake using rapid solvent extraction (ASE) and reversed-phase high performance liquid chromatography-ultraviolet tandem fluorescence detection. Methods Fluoroquinolones in samples were extracted with 8% aqueous ammonia and acetonitrile as solvent. The extracts were extracted with fast solvent extraction. The extracts were degreased with n-hexane and ether, and determined by high performance liquid chromatography-ultraviolet tandem fluorescence detector. Standard method of quantitative. Results The calibration curve showed a good linearity in the range of 10 ~ 200μg / L, and the correlation coefficients of the four substances were all above 0.999. The spiked recoveries of four fluoroquinolones in fish were between 82.7% and 95.6% with relative standard deviations between 2.1% and 4.1% (n = 5) at the spiked levels of 255 and 0 μg / kg, respectively. The detection limits were 1.3 ~ 3.0μg / kg. Conclusion The method is rapid, simple, accurate and reliable, and can be used for routine testing of fluoroquinolones in whitefish.