Simultaneous detection of quinolone and sulfonamide residues in milk by HPLC-MS
OBJECTIVE To establish a test method for the determination of residues of two quinolones enrofloxacin(ENR)and norfloxacin(NOR)and one sulfadiazine(SD)in milk by HPLC-MS in order to maintain the quality of milk.METHODS The aqueous phase was 0.1％formic acid aqueous solution and the organic phase was 0.1％formic acid acetonitrile.The mass spectrometry and chromatographic conditions were optimized and the quantification was performed by external standard method.RESULTS The concentrations of ENR,NOR and SD in the range of 10.00～l00.0ng·mL-1,10.00～150.00ng·mL-1 and 20.00～250.00ng·mL-1 were linear with R2 of 0.988,0.944 and 0.947.The recoveries were in the range of 90％～105％with the relative standard deviations(RSD,n=12)of 16％,9.4％and 9.6％at the spiked levels of ENR,NOR and SD of 25,100 and 1OOng·mL-1,and the limits of detection(LOD)of the method were 8.48,2.09 and 1.87ng·mL-1 and the limits of quantification(LOQ)were 9.94,9.78 and 15.35ng·mL-1.CONCLUSION The method has the advantages of high sensitivity and selectivity,and is suitable for the simultaneous determination of quinolone and sulfonamide residues in milk.
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