Establishment of analysis method for the quantification of residues of halquinol and its metabolites in livestock and fishery products using liquid chromatography–tandem mass spectrometry

Abstract

In this study, an analysis method was established for the quantification of residues of halquinol and its metabolites in livestock and fishery products using liquid chromatography–tandem mass spectrometry (LC–MS/MS). We selected beef, pork (muscle and fat), chicken, egg, milk, flat fish, eel, and shrimp as target samples for validation of the method owing to them being typical livestock and fishery products. Validation of the developed analysis method was performed using liquid chromatography–tandem mass spectrometry (LC–MS/MS) at three concentration levels (0.5, 1, and 2 × the maximum residue limits) following the Codex Alimentarius (CODEX) guidelines (CAC/GL 71–2009). For all samples, correlation coefficients (R2) exceeded 0.99, recoveries ranged between 75.59 and 119.36%, and coefficients of variation (CV) ranged between 1.39 and 28.66%, thus satisfying CODEX guidelines. In addition, inter-laboratory validation was conducted, and the resulting recoveries and CVs satisfied the CODEX guidelines; LOQ was established as 10 μg kg–1 for pig muscle and 5 μg kg–1 for the other samples. Therefore, the analysis method developed in this study can accurately and precisely screen for and quantify halquinol and its metabolites in livestock and fishery products.