HIGH SENSITIVE MULTIRESIDUE ANALYSIS OF NON-STEROIDAL ANTI-INFLAMMATORY DRUGS RESIDUES IN MUSCLE, MILK AND PLASMA USING LIQUID CHROMATOGRAPHY COUPLED TO HIGH RESOLUTION MASS SPECTROMETRY

The aim of the present work is the development of a fast and reliable analytical multiresidue method for the confirmation of non-steroidal anti-inflammatory drugs residues in muscle, plasma and milk. The samples are extracted with organic solvent and purified with liquid-liquid extraction (LLE). The purified extract was analyzed by LC-HRMS. The method was validated in accordance with the criteria defined in Commission Decision 2002/657/EC, decision limit (CCα) values and detection capability (CCβ) values have been established for each compound. Recoveries of the methods, calculated spiking the samples in the range 0.1 - 750.0 µg Kg-1, were 80 to 95 % for muscle, 75 to 101% for milk and 87 to 97% for plasma. The precision (CV) ranged between 9.2 and 15.1% for muscle, 9.9 and 14.6% for milk and from 9.4 to 13.4% for plasma. Linearity for the analytes was calculated from 5.0 to 1000.0 µg kg-1. Under the Official Control Plan activity, several samples were found positive for Flunixin, Meloxicam and Carprofen residues in meat, milk and plasma. The main advantages of the presented method are its rapidity, the specificity, the good precision and recovery that make it very suitable to the confirmatory determination of non-steroidal anti-inflammatory drugs residues in food and plasma.