Preparation And Evaluation Of Molecularly Imprinted Sol-gel Hybrid Materials For Determination Of Fluoroquinolone Residues Inaquatic Products By SPE-HPLC

In this thesis, the preparation and application of molecular imprinted sol-gel materials(MI-SGM) was reviewed. The MI-SGM was preparated and were used as solid-phaseextraction (SPE) sorbent for slective extraction of fluoroquinolone residues in aquaticproducts. The main contents were as follows:Chapter1: The introduction of the dangers of fluoroquinolone residues and its detectionmethods. The progress and application of the MIP-SGM was reviewed.Chapter2: The material was prepared by the sol-gel process to imprint theanti-inflammatory drug norfloxacin (NOR) for selective solid-phase extraction of NOR fromfish samples. The prepared material was used as a solid phase extraction sorbent, which wascoupled to high-performance liquid chromatography had been developed for determination oftrace NOR. Under the optimization of the SPE conditions, fluoroquinolones in the fish weredetermined, which showed good purification effect. The recoveries of norfloxacin, ofloxacinand ciprofloxacin were93.10%-98.24%,89.30-96.00%and88.46-96.24%.Chapter3: A highly selective molecularly imprinted sol-gel material (MI-SGM) wasprepared for on-line SPE-HPLC determination of fluoroquinolones residues in shrimpsamples. The conditions of on-line SPE were optimized, and the breakthrough curves wereinvestigated. The recoveries of norfloxacin, ciprofloxacin and enrofloxacin were82.50-88.40%,79.60-86.00%,87.90-92.00%and the relative standard deviations were3.40-6.70%,3.70-6.10%and3.30-6.90%.Chapter4: The phenyl and amino-functionalized material has been synthesized by themolecular imprinting technique and sol-gel process. The recognition mechanism betweenofloxacin with the material was based on the formation of π-π stacking interaction andhydrogen bond interaction. Under the optimal condition, a new method of SPE coupled withHPLC was developed for determination of fluoroquinolones residues in fish, which showedbetter clean-up and enrichment. The recoveries of ofloxacin, lomefloxacin and sarafloxacinwere79.20-84.00%，79.86-87.00%，82.00-88.80%and the relative standard deviations were2.60-5.80%,3.70-5.20%and3.90-6.10%, respectively.