Determination of Fluoroquinolones in Grass Carp by High Performance Liquid Chromatography-Ion Trap Mass Spectrometry Using Mixed-templates Imprinted Polymer Extraction

Abstract

The molecularly imprinted polymer(MIP) has been prepared using levofloxacin and ciprofloxacin as the mixed-templates,α-methacrylic acid(MAA) as functional monomers and trimethylolpropane trimethylacrylate(TRIM) as crosslinker.A method has been established for simultaneous determination of residues of ten fluoroquinolones in grass carp by high performance liquid chromatography-ion trap mass spectrometry(HPLC-ITMS) combining with molecularly imprinted polymer solid phase extraction(MISPE).The samples were extracted with 2% acetic acid in acetonitrile and defatted with n-hexane,then purified by the self-made molecularly imprinted cartridge.The preparation of samples and the separation conditions had been optimized,HPLC was performed with a gradient elution program while acetonitrile and water(containing 0.05% formic acid) were used as mobile phase.The identification and quantification were done with ion trap mass spectrometry.The recove-ries ranged from 80.6% to 104.6% with a relative standard deviations of 8.6%.The limits of detection(LOD) were 0.11-0.25 μg/kg and the limits of quantification(LOQ) were 0.35-0.84 μg/kg.This method is suitable for validation and multi-residue analysis of fluoroquolones in aquatic products.