摘要
目的:通过实验条件优化,建立了水产品中环丙沙星的高效液相色谱紫外、荧光检测法。方法:样品经磷酸盐缓冲液提取后,用Waters Oasis MAX小柱进行净化,XBridgeTMShield RP18柱(250 mm×3.0 mm×5μm)分离;流速:0.6 ml/min;柱温:25℃;流动相:乙腈+BR缓冲溶液(20+80);紫外检测波长:280 nm,荧光检测波长:λex为275 nm,λem为445 nm;外标法定量。结果:在0.05～5.0 mg/kg范围内呈良好线性关系,方法回收率在77.8%～95.1%之间,平均回收率为86.4%,相对标准偏差为7.5%,定量检测下限为10.0μg/kg。结论:本方法简便、灵敏、重现性好、干扰少、特异性好,能满足水产品中环丙沙星的检测要求。
Objective：To establish a HPLC - UV - FLD method for determination of ciprofloxacin in aquatic products by optimization of parameters. Methods： After ciprofloxacin in aquatic products was extracted by phosphate buffer, the sample was cleaned with solid phase extraction using Oasis MAX cartridges and the sample was separated on XBridgeTM Shield RP18 （250 mm×3.0 mm×5μm） with UV at 280 nm and FLD at λex 275 nm, λem 445 nm by using the mobile phase consisting of CH3CN （20%） and BR buffer （80%）. The flow rate was 0. 6 ml/min and the column temperature was controlled at 25℃. Results. Calibration curve was linear within the range of 0. 05 ～ 5.0 mg/kg and the limit of quantification was found to be 10. 0μg/kg. The extraction recovery was between 77. 8% ～ 95. 1% and the average recovery was 86.4%, the RSD was 7. 5%. Conclusion： This method is found to be simple, sensitive, accurate, and of good specificity for the determination of trace ciprofloxacin in aquatic products.
出处
《中国卫生检验杂志》
CAS
2007年第6期977-978,1056,共3页
Chinese Journal of Health Laboratory Technology
