SiO_(2)/MnFe_(2)O_(4)磁性固相萃取-HPLC测定水中喹诺酮类抗生素  

Determination of quinolone antibiotics in water by SiO_(2)/MnFe_(2)O_(4)magnetic solid phase extraction-high performance liquid chromatography

作　　者：魏霄 陈雨莹 钟佳祺 朱霞萍[1] 任维 赵平 WEI Xiao;CHEN Yuying;ZHONG Jiaqi;ZHU Xiaping;REN Wei;ZHAO Ping(College of Materials and Chemistry and Chemical Engineering,Chengdu University of Technology,Chengdu 610059,China;105 Geological Brigade,Guizhou Bureau of Geology and Mineral Resources Exploration and Development,Guiyang 550018,China)

机构地区：[1]成都理工大学材料与化学化工学院,成都610059 [2]贵州省地质矿产勘查开发局一〇五地质大队,贵阳550018

出　　处：《分析试验室》2024年第5期627-632,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(42267009);贵州省地矿局科技计划项目(黔地矿科合[2019]1号)资助。

摘　　要：通过溶胶-凝胶法制备了SiO_(2)/MnFe_(2)O_(4)复合材料,使用X-射线衍射仪、全自动物理吸附仪、振动样品磁强计、场发射扫描电镜和X射线光电子能谱仪对其进行了表征。将其作为磁性固相萃取材料,建立了SiO_(2)/MnFe_(2)O_(4)磁性固相萃取-高效液相色谱法(MSPE-HPLC)测定水中氟罗沙星(FLE)、氧氟沙星(OFX)、诺氟沙星(NOR)、环丙沙星(CIP)和恩诺沙星(ENR)的新方法。磁性固相萃取的最佳条件为:SiO_(2)/MnFe_(2)O_(4)用量50 mg,萃取20 min后,用4 mL氨水/甲醇(12/88,V/V)混合液洗脱4 min。最佳条件下,SiO_(2)/MnFe_(2)O_(4)对FLE,OFX,NOR,CIP,ENR的富集倍数分别为57.3,62.5,53.2,49.8和51.5倍。MSPE-HPLC测定5种抗生素的线性范围为0.004~1 mg/L,相对标准偏差(RSDs)为2.5%~5.3%,检出限为0.0012~0.0023 mg/L。将建立的方法应用于稻田水和鱼塘水中5种抗生素的测定,加标回收率介于78.8%~102.8%之间,RSDs为2.5%~5.3%。SiO_(2)/MnFe_(2)O_(4)composites were prepared by sol-gel method and characterized by X-ray diffraction,automatic physical adsorption,vibrating sample magnetometer,field emission scanning electron microscope and X-ray photoelectron spectroscopy.A method for the determination of fleroxacin(FLE),ofloxacin(OFX),norfloxacin(NOR),ciprofloxacin(CIP)and enrofloxacin(ENR)in water samples was established by SiO_(2)/MnFe_(2)O_(4)magnetic solid phase extraction-high performance liquid chromatography(MSPE-HPLC).The optimum conditions for magnetic solid phase extraction were as follows:the SiO_(2)/MnFe_(2)O_(4)amount of 50 mg,the extraction time of 20 min,and the eluent time of 4 min with 4 mL of ammonia/methanol(12/88,V/V)mixture.Under the optimum conditions,the enrichment ratios of SiO_(2)/MnFe_(2)O_(4)to FLE,OFX,NOR,CIP and ENR were 57.3,62.5,53.2,49.8 and 51.5 times,respectively.The linear ranges of MSPE-HPLC determination for five antibiotics were 0.004-1 mg/L,the relative standard deviations(RSDs)were 2.5%-5.3%,and the detection limits were 0.0012-0.0023 mg/L.The method was applied to the determination of five antibiotics in paddy field water and fish-pond water,showing the recoveries of spiked antibiotics ranged from 78.8%to 102.8%,and the RSDs were 2.5%to 5.3%.

关 键 词：铁酸锰 磁性固相萃取 喹诺酮类抗生素 地表水 

分 类 号：O661.1[理学—分析化学]