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A reliable LC-MS/MS method with high sensitivity was developed and validated for the determination of dipyrone (DIP) metabolites in goat muscle, fat, liver, and kidney samples. Analytes were extracted using acetonitrile mixed with ammonia solution. After dehydration and evaporation to dryness, extracts were purified using an Oasis MAX cartridge. Chromatographic separation was performed on a hydrophilic interaction liquid chromatography column. The analytes were then detected using triple-quadrupole mass spectrometry in positive electrospray ionization and multiple reaction monitoring mode. Calibration plots were constructed using matrix-matched standards and showed good linearity. Limits of quantification for 4-methylaminoantipyrine (MM), 4-formylaminoantipyrine (FAA), and 4-acetylaminoantipyrone (AAA) ranged from 0.41 mu kg(-1) to 6 mu g kg(-1), while those for 4-aminoantipyrone (AA) ranged from 10 mu g kg(-1) to 125 mu g kg(-1) in all tissues. The developed method was successfully applied in the determination of DIP metabolite residues in actual goat tissues. (C) 2015 Elsevier Ltd. All rights reserved.