FOOD SCIENCE ›› 2010, Vol. 31 ›› Issue (2): 127-130.doi: 10.7506/spkx1002-6300-201002031

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A Rapid High-performance Liquid Chromatography-Tandem Mass Spectrometric Method for Determination of 4 Fluoroquinolones Residues in Fish Meat

HUANG You-sheng,LIU Bo-ping,ZHU Xiao-ling,LI Gui-sheng   

  1. HUANG You-sheng,LIU Bo-ping,ZHU Xiao-ling,LI Gui-sheng
  • Received:2009-03-05 Revised:2009-08-27 Online:2010-01-15 Published:2010-12-29
  • Contact: HUANG You-sheng


A high-performance liquid chromatography-tandem mass spectrometric (HPLC-MS/MS) method was developed for the simultaneous determination of 4 fluoroquinolone antibiotic residues in fish meat. In the method, analytes were extracted with acidified acetonitrile, cleaned up with n-hexane, concentrated to dryness under nitrogen, redissolved in 1 mL of mixed solution of acetonitrile and 1% formic acid (1:9, V/V), separated on a RP-HPLC column, detected by HPLC-MS/MS with positive electrospray ionization (ESI+) in multiple reaction monitoring (MRM) mode, and quantified using an external standard method. The standard curves for all analytes exhibited good linearity over the concentration range of 2 - 40 μg/kg with correlation coefficients (r2) beyond 0.997. The recoveries of 4 fluoroquinolone antibiotics in fish meat samples spiked at concentration levels of 4, 10 μg/kg and 20 μg/kg ranged from 79.9% to 98.1%, with relative standard deviations between 2.7% and 8.7%. The limits of detection (LOD) and limits of quantification (LOQ) of the developed method were in the ranges of 0.1-0.4μg/kg and 0.3- 1.0 μg/kg, respectively. This method is characterized by simplicity, rapidity, high sensitivity, good reproducibility and better selectivity, and therefore can be used for identification and determination of fluoroquinolones in fish meat.

Key words: high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), fluoroquinolones, residues, fish

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