SPE-HPLC检测动物源性食品中3种氟喹诺酮类药物残留

摘要

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.%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（pH 2.4）∶乙腈为82∶18（体积比）为流动相，流速0.8 mL/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）。