Confirmatory Identification of Carbadox-Related Residues in Swine Liver by Gas-Liquid Chromatography/Mass Spectrometry with Selected Ion Monitoring

Abstract

Abstract A confirmatory method has been developed to identify quinoxaline-2-carboxylic acid, the carbadox tissue residue, in swine liver, a target tissue, at the regulatory level of 30 μg/kg. Quinoxaline-2-carboxylic acid (QCA) is isolated from liver hydrolysates by solvent extraction and ion-exclusion chromatography, and a methyl ester derivative (CP-25,536 or QME) is identified by gas-liquid chromatography/ mass spectrometry with selected ion monitoring. The relative intensities of 3 ions: the base peak at m/z = 130, a second significant mass at m/z = 158, and the molecular ion (M+) at m/z = 188, are monitored simultaneously with a quadrupole mass spectrometer. Validation studies consisting of the analysis of liver fortified with QCA at the regulatory level and analysis of swine specimens containing physiologically incurred carbadox residues demonstrated that peak height ratios of ions in these tissue extracts corresponded to ion intensities of standards monitored at m/z = 188,158, and 130.