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摘要
Rayleigh scattering spectrometry was applied to study the degeneration of fish serum protein in different concentrations of weak organic acid aqueous solutions. The influence of proteins on extraction efficiencies of quinolones (QNs) residues from protein and oil matrixes of fish samples was also discussed by HPLC. In a 0. 5 mol/L citric acid aqueous solution, a slow but full protein denaturation takes place, which causes the dissociation of QNs-protein complex. Based on the above results, with citric acid aqueous solution as biological affinity extraction system, an effective sample pretreatment method was developed for the analysis of QNs in fish samples by HPLC. The sample pretreatment procedure was as follows. Previously homogenized fresh fish samples was added to teflon tubes, then 0. 5 mol/L citric acid aqueous solution was used as extraction solvent, QNs residues were extracted twice from samples. The mixed granular adsorbents of primary secondary amine (PSA) and Cleanert NH2 were added in the extractant to eliminate the impurities. This method has been applied to the determination of 6 kinds of QNs (enoxacin, norfloxacin, ciprofloxacin, lomefloxacin, enrofloxacin and gatifloxacin) residues in the fish samples. The detection limits were in the range of 0. 0055-0. 016 mg/kg, and the spiked recoveries were 82. 0%-95. 2% with RSD 1. 9%-5. 8%. The method was simple, quick, reliable and environment friendly.
- 出版日期2013-10
- 单位烟台大学
