A rapid method for determination of disialoganglioside GD3 in whey protein products by ultra performance liquid chromatography-tandem mass spectrometry was established.The extraction conditions(extraction agent ration and extraction volumes)and the further extraction(type and volume)were optimized,1 mL of the solution of samples was extracted by 4 mL chloroform-methanol(1∶2,V/V),the supernatant ex-tracted many times was mixed and was further extracted by 2 mL water.The mass spectrometry and chromatographic conditions(monitoring modes,columns and pH of mobile phases)were performed.Syncronis HILIC silica column a gradient elution of 0.01 mol/L ammonium acetate-acetonitrile(pH5.6)as the mobile phase were selected.Quantitative detection by precursor ion monitoring and qualitative diagnosis by multiplere-action monitoring(MRM)were used.The linear relationships of the disialoganglioside GD3 was good in the mass concentration range of 0.5-50.0μg/mL,with coefficients ofddeterminations(R2)＞0.99.The recovery were 87.3％-103.7％,the relative standard deviations(RSD)were 4.16％-8.95％,the minimum detectable values were 0.1 g/kg.The method with good linearity,repeatabilityand robustnesswas accurate and stable to deter-mine the concentration of disialoganglioside GD3.
维普
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