【摘要】 本文合成了磁性金属有机骨架材料Fe₃O₄@[Cu₃（btc）₂],并作为分散微固相萃取的吸附剂用于四环素类抗生素的富集.对萃取的条件,包括萃取时间、溶液pH和洗脱溶剂对四环素类抗生素萃取效率的影响进行了研究.结果显示Fe₃O₄@[Cu₃（btc）₂]可以有效富集四环素类抗生素,而四环素类抗生素与Fe₃O₄@[Cu₃（btc）₂]之间的静电相互作用主导了这一过程.利用分散微固相萃取结合液相色谱-串联质谱法对天然水中的四种四环素类抗生素（土霉素,四环素,金霉素和多西环素）残留进行了测定.四种抗生素的检出限（S/N=3）为0.01～0.02μg/L,定量限（S/N=10）为0.04～0.07μg/L.河水和养殖水中四环素三个水平的加标回收率为70.3%～96.5%,相对标准偏差为3.8%～12.8%.结果表明,基于磁性金属有机骨架材料的分散微固相萃取可以从水中简单、快速、高效地富集四环素类抗生素.更多还原

【Abstract】 Residues of tetracycline antibiotics（TCs） in environments may be harmful to human.Due to their high polarities,it is extremely challenging to efficiently enrich TCs with low concentrations in natural waters for analysis.In this work,a magnetic metal-organic framework Fe₃O₄@[Cu₃（btc）₂]was synthesized and applied as a dispersive micro-solid phase extraction adsorbent for TCs enrichment.Effects of dispersive micro-solid phase extraction conditions including extraction time,solution p H,and elution solvent on the extraction efficiencies of TCs were investigated.Results show that TCs could be enriched efficiently by Fe₃O₄@[Cu₃（btc）₂],and electrostatic interaction between TCs and Fe₃O₄@[Cu₃（btc）₂]dominated this process.Combined with liquid chromatography-tandem mass spectrometry,four TCs residues （oxytetracycline,tetracycline,chlortetracycline,and doxycycline） in natural waters were determined.The detection limits （LOD,S/N=3） of the four antibiotics were 0.01-0.02μg/L,and the limits of quantitation （LOQ,S/N=10）were 0.04-0.07μg/L.The recoveries obtained from river water and aquaculture water spiked with three TCs concentration levels ranged from 70.3%to 96.5%with relative standard deviations of 3.8%-12.8%.Results indicate that the magnetic metal-organic framework based dispersive micro-solid phase extraction is simple,rapid and high-loading for antibiotics enrichment from water,which further expand the practical application of metal-organic frameworks in sample pretreatment for environmental pollutant analysis.更多还原