Determination of Metamizole Sodium in Goat Milk and Goat Milk Powder by UPLC-MS/MS
An analytical method was developed for the determination of metamizole sodium(4-aminoantipyrine,4-formylaminoantipyrine,4-acetamidoantipyrine and 4-methylaminoantipyrine)residues in goat milk and goat milk powder by UPLC-MS/MS.The samples were extracted with acetonitrile,concentrated by nitrogen,and mobile phases were formic acid water and formic acid acetonitrile.The identification and quantification of metamizole sodium residues were carried out by UPLC-MS/MS with multiple reaction monitoring in positive electrospray ionization.4-aminoantipyrine,4-formylaminoantipyrine and 4-acetaminoantipyrine were quantified by external standard method,and 4-methylaminoantipyrine was quantified by isotopic internal standard.The linearity of 4-aminoantipyrine in the range of 0-99.1 μg/L and the other three compounds in the range of 0-99.9 μg/L was good,with the correlation coefficients(R2)more than 0.995.The limits of quantification of 4-aminoantipyrine,4-formylaminoantipyrine,4-acetylaminoantipyrine,and 4-methylaminoantipyrine were 2.8,3.9,0.088,and 1.4 μg/kg,respectively.The recoveries ranged from 83.6％to 100.2％at spiked levels of about 5,10,20 and 50 μg/kg for goat milk,and 40,80,160 and 400 μg/kg for goat milk powder.The relative standard deviations of the precision was 0.3％-6.5％(n=6).The method was sensitive,accurate,fast and effective for the determination of metamizole sodium residues in goat milk and goat milk powder,which could be used for daily risk monitoring and market supervision.
metamizole sodiumgoat milkgoat milk powderultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
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