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

Publication date: 1 June 2017
Source:Talanta, Volume 168
Author(s): Fabiano Barreto, Cristina Ribeiro, Rodrigo Barcellos Hoff, Teresa Dalla Costa
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⁻¹ of formic acid and 1mmolL⁻¹ 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.

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