Determination of Ampicillin and Its Metabolites in Eggs by UPLC-MS/MS
A method of ultra high performance liquid chromatography tandem mass spectrometry was developed for the simultaneous determination of ampicillin and its main metabolites including ampicillin acid and ampicillin diketopiperazine in eggs.After extracted by acetonitrile:water(70∶30,V/V)and concentrated by rotary evaporation,the sample solution was purified by SAX solid phase extraction column,and injected into the UPLC-MS/MS system to be tested.The results showed a good linear relationship between the range of 1 to 200 ng/g concentrations for ampicillin,ampicillin acid and ampicillin diketopiperazine.The detection and quantification limit of ampicillin and its metabolites in eggs were 0.5 ng/g and 1.0 ng/g,respectively.The recoveries of ampicillin and its metabolites were 84.0%～96.2%,85.6%～96.4%and 89.2%～95.8%,and the coefficients of variation within and between the batches were less than 10%at the concentraion range of 1.0 ng/g to 100.0 ng/g.In stability experiments,the results also showed low-temperature storage stability and freeze-thaw stability of the compounds in different concentrations in eggs.The actual sample testing results show that after taking ampicillin,the eggs produced by laying hens can detect ampicillin,ampicillin acid,and ampicillin diketopiperazine,and the residual amount and residual time of ampicillin acid and ampicillin diketopiperazine are higher than those of the ampicillin.The technical indicators of this method can meet the requirements of residue testing.And the method has good reproducibility,and meets the relevant regulations of testing residues on veterinary drugs,which is suitable for for the simultaneous determination of ampicillin and its metabolites in eggs.Ampicillin,ampicillin acid,and ampicillin diketopiperazine can be detectde in the eggs produced by laying hens afeter taking ampicillin,and the residual amount and residual time of ampicillin acid and ampicillin diketopiperazine are higher than ampicillin.The technical indicators of this method can meet the requirements of residue testing,which indicates the established method is suitable for the simultaneous determination of ampicillin and its metabolites in eggs.
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