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为减少有机试剂使用,减轻环境污染,提高检测效率,建立了可同时检测鸡蛋中氧氟沙星(Ofloxacin,OFL)、培氟沙星(Pefloxacin,PEF)、环丙沙星(Ciprofloxacin,CIP)、达氟沙星(Danofloxacin,DAN)、恩诺沙星(Enrofloxacin,ENR)和沙拉沙星(Sarafloxacin,SAR)6种氟喹诺酮类药物残留的环境友好型高效液相色谱荧光检测方法。鸡蛋样品用纯水提取,氯化钠盐析,加热冷冻净化,正己烷脱脂,采用0.5%甲酸水-乙腈体系作为流动相,荧光激发波长280nm,发射波长450nm检测。结果显示:OFL的线性范围为8~1 000μg/kg,DAN为0.4~50.0μg/kg,其余4种均为2~250μg/kg,相关系数大于0.99。OFL检测限为4μg/kg,DAN为0.2μg/kg,其余4种均为1μg/kg;OFL定量限为20μg/kg,DAN为1μg/kg,其余4种均为5μg/kg。6种药物添加平均回收率为80.52%~101.10%;相对标准偏差为2.99%~10.40%。
In order to reduce the use of organic reagents, reduce the environmental pollution and improve the detection efficiency, a method was developed for the simultaneous detection of Ofloxacin (OFL), Pefloxacin (PEF), Ciprofloxacin (CIP) , Danofloxacin (DAN), Enrofloxacin (ENR) and Sarafloxacin (SAR) were detected by fluorescence spectrometry. Egg samples were extracted with pure water, sodium chloride salting, heating and freezing purification, degreasing n-hexane, using 0.5% formic acid water - acetonitrile as mobile phase, fluorescence excitation wavelength 280nm, emission wavelength 450nm detection. The results showed that the linear range of OFL was 8-1 000μg / kg, DAN was 0.4-50.0μg / kg, and the remaining 4 were 2 ~ 250μg / kg, the correlation coefficient was greater than 0.99. The detection limit of OFL was 4μg / kg, DAN was 0.2μg / kg, the remaining 4 were 1μg / kg; OFL limit of quantification was 20μg / kg, DAN was 1μg / kg, the remaining 4 were 5μg / kg. The average recoveries of six drugs were 80.52% ~ 101.10% with relative standard deviations of 2.99% -10.40%.