Improvement of chemical analysis of antibiotics. XVI. Simple and rapid determination of residual pyridonecarboxylic acid antibacterials in fish using a prepacked amino cartridge

J Chromatogr. 1989 Aug 30;477(2):397-406. doi: 10.1016/s0021-9673(01)89648-5.

Abstract

A simple and rapid method for the determination of residual pyridonecarboxylic acid antibacterials (PCAs) (oxolinic acid, nalidixic acid and piromidic acid) in fish was developed using a combination of high-performance liquid chromatography (HPLC) and clean-up with an amino-type prepacked cartridge. PCAs were extracted with n-hexane-ethyl acetate (1:3) and the extract was applied to a Baker 10 amino cartridge. PCAs were eluted from the cartridge with acetonitrile-methanol-0.01 M aqueous oxalic acid solution (pH 3.0) (3:1:6) and were determined by HPLC. The separations were performed on Nucleosil 3C18 (3 microns, 75 x 4.6 mm I.D.) using a mobile phase containing oxalic acid. The recoveries of PCAs from various fishes fortified at the level of 1.0 ppm were 77.1-95.5%, and the detection limits were 0.05 ppm. The analytical time per sample was less than 30 min.

MeSH terms

  • Animals
  • Anti-Infective Agents / analysis*
  • Chromatography, High Pressure Liquid
  • Drug Residues / analysis*
  • Fishes*
  • Food Analysis*
  • Nalidixic Acid / analysis
  • Oxolinic Acid / analysis
  • Piromidic Acid / analysis

Substances

  • Anti-Infective Agents
  • Nalidixic Acid
  • Piromidic Acid
  • Oxolinic Acid