动源性食品中常见氟喹诺酮类残留检测前处理的优化

Determination of six Fluoroquinolones Pretreatment Optimization by Liquid Chromatography Flurorescence Detector

关键词:  氟喹诺酮  高效液相色谱法  荧光检测器  动源性食品

Key words:  HPLC-FLD , Fluoroquinolones(FQS), fish , egg , pork

摘要:

建立了一个检测动源性食品中6种氟喹诺酮类药物残留的高效液相色谱方法。对不同基质的样品前处理条件经行了优化：鱼、肉及肝脏样品经过乙腈-0.1mol/L磷酸二氢钾缓冲液提取，正己烷洗涤去除油脂；蛋及乳制品样品经过乙腈提取，正己烷洗涤去除油脂。目标化合物采用高效液相色谱-荧光检测器检测，外标法定量。添加10、20、50、100μg/kg浓度水平时，回收率在82%～105%之间，相对标准偏差在4%～12%之间，方法的检出限为诺氟沙星、环丙沙星、沙拉沙星及单诺沙星为5.0μg/Kg、，恩诺沙星、达氟沙星为3.0μg/Kg。方法操作简单、实用，基质干扰小，灵敏度高，可以满足动源性食品中氟喹诺酮类药物残留检测的需要。

Abstract:

A High performance Liquid Chromatography method was proposed for analyzing 6 Fluoroquinolones(FQS) in products of animal tissues. The sample pretreatment of different substrates were optimized, fish, meat and liver samples were extracted by CH3CN-0.1mol / L KH2PO4 buffer solution, eggs and dairy products extracted by CH3CN, then hexane was added in to remove grease; Target compounds were detected by HPLC-Flurorescence detector, and quantitative with external standard method. The recoveries of 6 FQS were 82%～105% at four spiked level: 10, 20, 50, 100 μg/kg, and the RSD were blew 12.0%. The LOD of Norfloxacin, Ciprofloxacin, Sarafloxacin and Difloxacin were 5.0μg/Kg, The LOD of Danofloxacin and Enrofloxacin were 3.0μg/Kg. Method was simple, practical, and sensitive. It can meet the needs of determination of FQS in products of animal tissues.