摘要
目的建立动物源性食品中8种氟喹诺酮类药物（麻保沙星,诺氟沙星、环丙沙星、达氟沙星、恩诺沙星,二氟沙星,噁喹酸,氟甲喹）残留的高效液相色谱检测法。方法样品用EDTA-Mcllvaine缓冲溶液提取,PEP-2固相萃取柱净化,ZORBAX C18（4.6 mm×250 mm,5μm）分离,荧光检测器检测,外标法定量。结果麻保沙星,噁喹酸,氟甲喹配制标准品浓度在30～360μg/L,其余5种在15～180μg/L范围内线性关系良好,相关系数均〉0.99,诺氟沙星,环丙沙星,恩诺沙星,二氟沙星的检出限为2μg/kg,达氟沙星的检出限为0.5μg/kg,麻保沙星,噁喹酸,氟甲喹的检出限为8μg/kg,各种组分回收率在77.6%～98.3%之间,相对标准偏差为2.8%～9.4%。结论该方法操作简单,准确度和精密度高,对人体危害较小,能够满足不同基质检测的需要。
Objective A high performance liquid chromatographic method was developed for determination of 8 fluoroquinolones residues in animal derived food （ including marbofloxacin, ciprofloxacin, danofloxacin, norfloxacin, enrofloxacin, difloxacin, oxolinic acid, and flumequine）. Methods The sample residues were extracted by EDTA- Mcllvaine buffer, purifid with PEP-2 solid-phase extrction column, seperated by ZORBAX C18 （5 μm, 4. 6 mm× 250 mm） and quanlified by external standard calibration curves. Results Marbofloxacin, oxolinic acid, and flumequine in 30-360 μg/L, and the remaining five drugs in 15-180μg/L linear relationship is good, the correlation coefficient is greater than 0. 99. The detection limit （ including norfloxacin, ciprofloxacin, enrofloxacin, difloxacin） is 2 μg/kg, the detection limit of danofloxacin is 0.5μg/kg, the detection limit of marbofloxacin, oxolinic acid and flumequine is 8 μg/kg, the recoveries are between 77.6%-98.3%, the relative standard deviations are between 2.77%-9.35%. Conclusion The method was simple, high accuracy and precision, less harmful to human body and could be satisfied with diffirent substrate test.
出处
《中国食品卫生杂志》
北大核心
2014年第5期460-464,共5页
Chinese Journal of Food Hygiene
基金
国家自然科学基金项目(SK201216(LC/MS/MS))
关键词
氟喹诺酮
高效液相色谱法
荧光检测器
动物源性食品
兽药残留
食品安全
Fluoroquinolones
high performance liquid chromatography
fluorescence detector
animal derived food
veterinary drug residue
food safety
