Journal Article
Validation Studies
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A confirmatory method for the simultaneous extraction, separation, identification and quantification of Tetracycline, Sulphonamide, Trimethoprim and Dapsone residues in muscle by ultra-high-performance liquid chromatography-tandem mass spectrometry according to Commission Decision 2002/657/EC.

A rapid confirmatory multi-residue method for the analysis of tetracyclines, sulphonamides, trimethoprim and dapsone by UPLC-MS/MS is described. The method is able to quantify and confirm the following 19 compounds, oxytetracycline, tetracycline, chlortetracycline, doxycycline, sulfadiazine, sulfathiazole, sulfapyridine, trimethoprim, sulfamerazine, sulfamethizole, sulfamethazine, sulfamethoxypyridazine, sulfamonomethoxine, sulfachlorpyridazine, dapsone, sulfamethoxazole, sulfisoxazole, sulfaquinoxaline and sulfadimethoxine. Samples are extracted with 0.1M EDTA and acetonitrile, which is then evaporated under a stream of nitrogen and reconstituted in water. Following centrifugation and filtering, an aliquot is analysed by UPLC-MS/MS using positive electrospray ionisation and multiple reaction monitoring. The method is deemed rapid as all analytes are extracted by a single extraction technique, with no solid-phase extraction clean up required. Validation is according to Commission Decision 2002/657/EC and was carried out for bovine, porcine, ovine and poultry species. Specificity, recovery, repeatability, reproducibility, CCalpha and CCbeta data is presented.

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