Determination of the antibiotic chloramphenicol in meat and seafood products by liquid chromatography–electrospray ionization tandem mass spectrometry

Abstract

A confirmatory method based on isotope dilution liquid chromatography–electrospray ionization tandem mass spectrometry is described for the determination of the antibiotic chloramphenicol (CAP) in foods. The method is quantitative and entails liquid–liquid extraction followed by a clean-up step on a silica gel solid-phase extraction cartridge. Mass spectral acquisition is done in the negative ion mode applying multiple reaction monitoring of two diagnostic transition reactions for CAP ( m/z 321→257 and m/z 321→152). In addition, the presence of two chlorine atoms in the CAP molecule provides further analyte certainty by assessing the 37Cl/ 35Cl ratio using the transition reactions m/z 323→257 and m/z 323→152. Validation of the method in chicken meat is conducted according to the latest European Union criteria for the analysis of veterinary drug residues at levels of 0.05, 0.10, and 0.20 μg/kg, employing [ 2H 5]-chloramphenicol as internal standard. The decision limit and the detection capability were calculated at 0.01 μg/kg and 0.02 μg/kg, respectively. At the lowest fortification level (i.e. 0.05 μg/kg), precision values below 14 and 17% were achieved under repeatability and within-laboratory reproducibility conditions, respectively. The accuracy of the method was within 20, 15, and 5% of the target values at the 0.05, 0.10, and 0.20 μg/kg fortification levels, respectively. The applicability of this procedure was demonstrated by the analysis of other meat (turkey, pork, beef) and seafood (fish, shrimps) products. The method is robust and suitable for routine quality control operations, and more than 200 sample injections were performed without excessive pollution of the mass spectrometer or loss of LC column performance.