磁性微球表面光引发聚合制备金属配位印迹层及选择性富集奶样中氟喹诺酮类药物残留

Metal complex imprinted layer synthesized by photo-polymerization on surface of magnetic microspheres for selective enrichment of fluoroquinolones residues from milk

中文关键词:  分子印迹磁性微球  金属配位  磁分散萃取  奶样  氟喹诺酮类药物

英文关键词:molecularly imprinted magnetic microspheres  metal complex  magnetic dispersion extraction  milk  fluoroquinolones

中文摘要:

      目的 发展一种金属配位印迹磁性微球的制备方法, 并用于奶样中氟喹诺酮类药物残留的选择性富集。方法 采用简便的溶剂热法合成磁性纳米粒子, 再采用溶胶-凝胶法制备磁性硅胶微球, 然后在磁性硅胶微球表面接枝光引发剂, 在125 W紫外灯辐射下合成恩诺沙星-Co(Ⅱ)配位印迹层, 并用于磁分散萃取奶样中恩诺沙星、环丙沙星和洛美沙星。结果 该方法的加标回收率为89.6%~100.8%, 相对标准偏差为1.4%~5.5%, 其中环丙沙星的检出限和定量限分别为1.72 μg/kg和5.74 μg/kg, 洛美沙星的检出限和定量限分别为2.05 μg/kg和6.82 μg/kg, 恩诺沙星的检出限和定量限分别为1.18 μg/kg和3.94 μg/kg。结论 该样品处理方法是一种选择性好、简单快速的分离检测奶样中氟喹诺酮类药物残留的方法。

英文摘要:

      Objective To develop a preparation method of metal coordination imprinted magnetic microspheres for selective enrichment of fluoroquinolones drug residues from milk. Methods The magnetic microspheres were synthesized by the solvothermal method, and was coated with silica gel, the iniferter was synthesized on surface of the magnetic silica microspheres, and then enrofloxacin–Co(Ⅱ) coordination imprinted layer was synthesized under an ultraviolet spotlight of 125 W. The obtained sorbents were used for magnetic dispersion extraction of enrofloxacin (ENR), ciprofloxacin (CIP) and lomefloxacin (LOM) from milk samples. Results The present methods showed that the average recoveries were obtained in the range of 89.6%~100.8% with precision 1.4%~5.5%. The limits of detection and quantitation of the proposed method were 1.72 μg/kg and 5.74 μg/kg for CIP, 2.05 μg/kg and 6.82 μg/kg for LOM, 1.18 μg/kg and 3.94 μg/kg for ENR, respectively. Conclusion The sample preparation method has good selectivity, and is simple and rapid for the separation and determination of fluoroquinolones residues in milk samples.