A simple and high-throughput method for determination and confirmation of 14 coccidiostats in poultry muscle and eggs using liquid chromatography - quadrupole linear ion trap - tandem mass spectrometry (HPLC-QqLIT-MS/MS): Validation according to European Union 2002/657/EC.

A simple and fast quantitative and confirmatory multi-residue method was developed and validated for the determination of 14 coccidiostats residues in poultry muscle and eggs using liquid chromatography-tandem mass spectrometry (LC/MS-MS). The compounds were analyzed in a single run including lasalocid A, maduramicin, monensin, narasin, salinomycin, semduramicin, robenidine, diclazuril, toltrazuril, trimethoprim, clopidol, amprolium, diaveridine and nicarbazin (as the marker residue dinitrocarbanilide). A low-cost extraction and clean up procedure was optimized without the need of solid-phase extraction. Samples were extracted with acetonitrile followed by low-temperature clean up. Chromatographic separation was achieved using a C18 column, using water and acetonitrile, both containing 5mmolL of formic acid and 1mmolL ammonium acetate, as mobile phase. Coccidiostats were ionized in negative and positive mode and monitored simultaneously. The method was fully validated according with Commission Decision 2002/657/EC and was applied for >100 samples from the Brazilian National Residue Control Plan (NRCP). Parameters as precision, reproducibility, trueness, CCα and CCβ were determined. Trueness values were within the range 73-115%. Precision (repeatability and intermediate precision) ranged from 0.4% to 21% and intralaboratory reproducibility ranged from 6.3% to 27%, depending on matrix.