摘要

A simple multiresidue method, HPLC with programmable fluorescence detection and gradient elution, has been developed for analysis of nine (fluoro)quinolones (FQs)-norfloxacin, ciprofloxacin, lomefloxacin, danofloxacin, enrofloxacin, sarafloxacin, difloxacin, oxolinic acid, and flumequine in chicken muscle. The samples were extracted with phosphate-buffered saline (PBS, 0.01 mol L-1, pH 7.0) and cleaned by SPE. Cleaned extracts reconstituted in different solvents were tested to determine which gave the maximum fluorescence response for each drug. PBS (0.01 mol L-1, pH 7.0) was used as reconstitution solvent, because the sensitivity for FQs dissolved in PBS was 1.8-3.2 times greater than when dissolved in the mobile phase. Under the optimum conditions excellent linearity was obtained, with satisfactory correlation coefficients (r > 0.9994) for PBS. The "matrix effect" was eliminated. Limits of quantification for each drug were in the range 0.3-1.0 ng g(-1). In fortification studies recoveries of the analytes were in the range 71.8-102.1 % for 1-100 ng g(-1) concentrations. Inter- and intra-day coefficients of variation were from 0.5 to 5.2% and from 1.7 to 9.0%, respectively. Short-term stability in PBS was also determined.