Improved determination of quinolones in milk at their MRL levels using LC-UV,LC-FD,LC-MS and LC-MS/MS and validation in line with regulation 2002/657/EC

摘要

This paper reports the multi-residue determination of quinolones included in the European Union regulations(marbofloxacin,ciprofloxacin,danofloxacin,enrofloxacin and flumequine)in bovine milk,using liquid chromatography with ultraviolet(LC-UV),fluorescence(LC-FD),mass spectrometry(LC-MS)and tandem mass spectrometry detection(LC-MS/MS).The methods were validated,in line with EU requirements(Commission Decision 2002/657/EC).Linearity,decision limit(CC alpha),detection capability(CC beta),detection limit(LOD),quantification limits(LOQ),recoveries,precision,selectivity and stability were determined and adequate results were obtained.Recoveries higher than 80% were obtained for all quinolones.The methods developed were used to quantify enrofloxacin and its main metabolite,ciprofloxacin,in milk from animals treated with enrofloxacin.