环境友好的HPLC方法检测鸡蛋中6种氟喹诺酮类药物残留  

Development of environment-friendly HPLC method for simultaneous determination of six fluoroquinolones in eggs

作　　者：程勇翔[1] 夏曦[1] 张鹏春[1] 赵坤霞[1] 李晓薇[1] 丁双阳[1] OHENG Yongxiang XIA Xi ZHANG Pengchun ZHAO Kunxia LI Xiaowei DING Shuangyang(College of Veterinary Medicine, China Agricultural University, Beiling 100093, China)

机构地区：[1]中国农业大学动物医学院,北京100193

出　　处：《中国农业大学学报》2017年第4期109-119,共11页Journal of China Agricultural University

基　　金：农业部公益性行业(农业)科研专项经费项目(201203069-2)

摘　　要：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 regents, decrease the pollution of environment and increase the efficiency of detection, an analytical method for simultaneous determination of six fluoroquinolones （FQs, including ofloxacin, peflocacin, ciproflocacin, danofloxacin, enrofloxacin and sarafloxacin） residues in eggs based on high performance liquid chromatography with fluorescence detection （HPLC/FLD） was established. Samples were extracted by water and added NaCI to salt out. The extracts were heated and frozen, degreased by n-hexane. Six FQs were separated by C18 column with 0.5% methanoic acid/acetonitrile as the mobile phase and detected with fluorescence detection. The fluorometric excitation wavelength was 280 nm, and emission wavelength was 450 nm. The tested ranges of quinolone calibrations were 0- 1 000μg/kg for ofloxacin,0- 50μg/kg for danofloxacin,0- 250 μg/kg for the other four FQs with the correlation coefficients greater than 0.99. The limits of detection （LODs） were ofloxacin 4 μg/kg, danofloxacin 0.2μg/kg,and the other four FQs 1 μg/kg. And the limits of quantification （LOQs） were ofloxacin 20 μg/kg, danofloxacin 1 μg/kg,and the other four FQs 5μg/kg. The average percentage recoveries were ranged from 80.52% to 101.10% for six FQs in eggs samples,coefficients of variability （CV） were ranged from 2.99% - 10.40%.

关 键 词：氟喹诺酮类药物 高效液相 鸡蛋 药物残留 环境友好 

分 类 号：S859.84[农业科学—临床兽医学]