【摘要】 目的:建立牛奶中环丙沙星、双氟沙星和沙拉沙星3种氟喹诺酮残留的高效液相色谱荧光检测方法。方法:样品经磷酸盐缓冲液稀释、提取后,用Waters Oasis HLB固相萃取小柱进行浓缩、净化,Extend-C18柱(250 mm×4.6 mm×5μm)分离;流速:0.8 ml/min;柱温:35℃;流动相:甲醇+乙腈+0.2%甲酸(15+15+70);荧光检测波长:λex为275 nm;λem为445 nm。结果:在0.1~5.0 mg/L范围内三种被测化合物均呈良好线性关系,方法回收率在90.0%~102.0%之间,相对标准偏差为4.1%~10.0%,最低检出限环丙沙星、双氟沙星和沙拉沙星分别为0.02、0.015和0.02 mg/L。结论:所建方法简便、灵敏、重现性好、干扰少、特异性好,能满足牛奶中三种目标化合物的检测要求。更多还原

【Abstract】 Objective:To establish a HPLC-FLD method for simultaneous determination of 3 fluoroquinolones in milk.Methods:After fluoroquinolones in milk were diluted and extracted by phosphate buffer,the sample was concentrated and cleaned by solid phase extraction using Oasis HLB cartridges and the sample was separated on a Extend-C18 column(250 mm×4.6 mm×5 μm)with FLD at λex 275 nm,λem 445 nm by using the mobile phase consisting of CH3OH+CH3CN+0.2% HCOOH(15+15+70).The flow rate was 0.8 ml/min and the column temperature was controlled at 35℃.Results:Calibration curves were linear within the range of 0.1～5.0 mg/L and the limits of quantification were 0.02,0.015 and 0.02 mg/L for ciprofloxacin,difloxacin and sarafcoxacin.The extraction recoveries were between 90.0%～102.0%,the RSD 4.1%~10.0%.Conclusion:This method is simple,sensitive,accurate and of good specificity for the determination of 3 trace fluoroquinolones in milk.更多还原