Abstract:

A method for the determination of metabolite residues of dipyrone, 4-formylaminoantipyrine （FAA）, 4-aminoantipyrine （AA） and 4-methylaminoantipyrine （MAA） in bovine muscle and pork muscle has been developed. Homogenized muscle sample was extracted with Na2SO4-Na2SO3 solution. After filtration, the extract was cleaned-up by a C18 solid phase extraction cartridge. Prepared sample was determined using high performance liquid chromatography under the following conditions: Inertsil ODS-3 column, methanol and water as mobile phase with gradient elution, detection wavelength of 265 nm. FAA was quantified by external standard method, while AA and MAA were quantified by internal standard method using isopropylaminoantipyrine as internal standard. Limits of detection of FAA was 12.5 μg/L, while those of AA and MAA were 15.0 μg/L and 20.0 μg/L, respectively. The limit of detection of this method was 50 μg/L for all the three metabolites. The recoveries of FAA, AA and MAA were 81.3%-92.5%, 82.0%-96.0%, and 80.4%-90.6%, respectively, at the spiked levels of 50-400 μg/kg. The relative standard deviations of the method were less than 7%.

Key words: bovine muscle, dipyrone, metabolites, pork muscle , high performance liquid chromatography （HPLC）