固相萃取——超高效液相色谱法测定水产品中6种氟喹诺酮类药物残留

Determination of 6 fluoroquinolones residues in aquatic products by solid phase extraction and ultra performance lquid chromatography

基于固相萃取(SPE)和超高效液相色谱(UPLC)技术,建立可同时测定水产品中诺氟沙星、氧氟沙星、环丙沙星、培氟沙星、洛美沙星、恩诺沙星6种氟喹诺酮类药物残留量的检测方法。经优化后的检测过程及参数为:样品匀浆后以磷酸盐缓冲液为提取剂,提取液经SPE净化、氮吹浓缩后,残渣用0.2%的甲酸水溶液溶解供UPLC分析;选用BEH C18(1.7μm,2.1mm×50 mm)色谱柱,以体积比为937的0.05mol/L柠檬酸+0.1 mol/L乙酸铵缓冲液-乙腈为流动相,流速为0.42mL/min,进样体积为0.2μL,柱温为50℃,荧光检测器检测波长λex=278nm、λem=465nm。该方法简单有效,添加回收率为63.69%～90.83%,最低检出限为0.5～1.8μg/kg,相对标准偏差均低于10%。

Based on solid phase extraction（SPE）and ultra high performance liquid chromatography（UPLC）technique,a method has been developed for the simultaneous detection and analysis of 6 fluoroquinolones residues in aquatic products.The optimized process and parameters of this method were as followed：treated aquatic products were extracted with phosphate buffer,the extracting solution were purified by SPE and concentrated by blowing nitrogen,and the residues were then dissolved in 0.2% formic acid solution for UPLC analysis;Chromatographic column BEH C18（1.7μm,2.1 mm ×50 mm）were applied,and citric acid（0.05 mol/L）-ammonium acetate（0.1 mol/L）buffer were used as the mobile phase with0.42 mL/min.the sample volume was 0.2μL,column temperature was 50 degree centigrade,and the excitation and emission wave length of fluorescence detector were 278 nm and 465 nm,respectively.The proposed method is simple and effective,with recovery rate range between 63.69% and 90.83%,limit of detection range between 0.5 and 1.8μg/kg,and relative standard deviation less than 10%.