SPE-HPLC检测动物源性食品中3种氟喹诺酮类药物残留  

Determination of Three Fluoroquinolones in Animal-derived Food by Combining SPE with HPLC

作　　者：池永红[1] 云雅光[1] 

机构地区：[1]包头轻工职业技术学院,内蒙古包头014035

出　　处：《食品研究与开发》2015年第20期152-155,共4页Food Research and Development

摘　　要：以3种氟喹诺酮类抗菌药物-诺氟沙星、环丙沙星,恩诺沙星为研究对象,结合固相萃取串联高效液相色谱,建立动物源性食品中3种分析物残留的准确、灵敏的分析方法。研究采用Cleanert S C18固相萃取小柱为基质净化柱,以Hypersil-ODS C18柱(4.6 mm×250 mm)为液相分离柱,0.05 mol/L H3PO4-三乙胺溶液(p H 2.4)∶乙腈为82∶18(体积比)为流动相,流速0.8 m L/min,能够达到基质净化和分析物富集、分离目的。根据实验结果,所建立的方法对3种氟喹诺酮类药物的最低检出限分别达到1.5、1.3、1.5μg/L;对3个添加浓度下的鸡肉、鸡蛋、牛奶和牛肉等复杂食品样品中3种分析物残留的检测也具有较高的准确度(回收率>90.0%)和重现性(RSD<5.0%,n=3)。An accurate and sensitive method for the detection of three fluoroquinolones-norfloxacin （NOR）, ciprofloxacin （CIPRO）, enrofloxacin （ENRO） residues in animal-derived food products was developed by combining solid-phase extraction with high performance liquid chromatography. The Cleanert S C18 solid-phase extraction column was used for complex matrix purification and one Hypersil-ODS C18 column （4.6 mm × 250 mm） was employed for separation in liquid chromatography. The mobile phase consisted of 0.05 mol/L H3PO4 was controlled pH at 2.4 by triethylamine and mixed with ACN at the ratio of 82∶18 （volume ratio）, and the flow rate controlled at 0.8 mL/min for the purpose of obtaining good substrate clean-up and analytes enrichment. Based on the obtained resluts, the detection limit of three chosen analytes achieved to 1.5 μg/L （NOR）,1.3μg/L （CIPRO）,1.5μg/L （ENRO） in the developed method, good recoveries in chosen chicken muscle, egg, milk and beef samples at three spiked levels of NOR, CIPRO and ENRO were obtained higher than 90.0 %with RSD less than 5.0%（n=3）, meaning that the developed method in this research was high accuracy and reproducibility.

关 键 词：氟喹诺酮类药物 固相萃取 高效液相色谱 检测 

分 类 号：O657.72[理学—分析化学] TS207.53[理学—化学]