多壁碳纳米管分子印迹固相萃取柱的制备及牛奶中三种氟喹诺酮的残留测定  

Preparation of dummy template molecularly imprinted polymers on multi-walled carbon nanotubes as a solid-phase extraction for determination of three fluoroquinolones in milk samples

作　　者：章璐幸[1] 吴惠芳[1] 钱江[1] 王坚[1] 马铭研[1] ZHANG Lu-xing;WU Hui-fang;QIAN Jiang;Wang Jian;MA Ming-yan(Zhejiang Pharmaceutical College, Ningbo 315100)

机构地区：[1]浙江医药高等专科学校,宁波315100

出　　处：《分析试验室》2018年第5期574-578,共5页Chinese Journal of Analysis Laboratory

基　　金：宁波市社发攻关项目(2014C50076);浙江省食药监管系统科技计划项目(SP201609)资助

摘　　要：建立了以恩诺沙星为假模板的多壁碳纳米管分子印迹固相萃取柱-HPLC法同时测定牛奶中三种氟喹诺酮氧氟沙星、诺氟沙星、环丙沙星残留的方法。牛奶样品经碳酸钠、乙腈沉淀蛋白后,用乙酸钠-盐酸体系调p H为3.0,经自制的多壁碳纳米管分子印迹固相萃取柱(MWCNTs-MISPE)净化萃取后,用高效液相色谱仪测定氧氟沙星、诺氟沙星、环丙沙星的含量。3种化合物在20.00-1000 ng/m L浓度范围线性关系良好,相关系数均大于0.9998,3个添加水平的回收率在82.3%-99.4%,日内和日间精密度小于20%。本文首次将自制的多壁碳纳米管分子印迹固相萃取柱应用于牛奶中的氟喹诺酮类化合物净化与富集,3份市售牛奶中氧氟沙星,诺氟沙星和环丙沙星含量均低于欧盟标准。Simultaneous determination of three fluoroquinolones, ofloxacin, norfloxacin and ciprofloxacin residues in milk was accomplished by HPLC after multi-walled carbon nanotube molecular imprinting solid-phase extraction column with enrofloxacin as dummy template. The milk samples were precipitated with sodium carbonate and acetonitrile,and then adjusted to p H 3. 0 with sodium acetatehydrochloric acid system. After purification by self-made multi-walled carbon nanotubes molecularly imprinted polymers solid-phase extraction（ MWCNTs-MISPE）,the content of ofloxacin,norfloxacin and ciprofloxacin were determined by high performance liquid chromatography（ HPLC）. The calibration curves of three compounds were linear in the range of 20. 00-1000 ng/m L（ r 0. 9998）,with the recoveries of 82. 3%-99. 4% at three loading levels,and the intra-day and inter-day precision were less than 20%. The fluoroquinolones in milk（ n = 3） were detected to be lower than the EU standards. This work is the first application of MWCNTs-MISPE column to purify and concentrate fluoroquinolones in milk. This method is simple and effective with high sensitivity,and can be used for the detection of ofloxacin,norfloxacin and ciprofloxacin in milk.

关 键 词：牛奶 氟喹诺酮类 多壁碳纳米管 分子印迹 固相萃取 高效液相 

分 类 号：O657.7[理学—分析化学]