Abstract: A proton nuclear magnetic resonance quantification called PULCON was established for determination of lactose and sucrose in infant formula milk powder. Using the known concentration of maleic acid as the external standard,the concentration of analyte in two NMR spectra could be correlated by the NMR principle of reciprocity. For the two analytes,the calibration curves established showed good linearity over the concentration range of 0.05 ~5.00(R2>0.999),and the average recoveries(n =3) were 100.19% ~103.21% with RSD of1. 79 % ~ 3. 57 %. The high universality, selectivity, non- standard and efficiency of the PULCON method demonstrated in this work suggested that this method could serve as a highly potential alternative for determination of lactose and sucrose in milk powder,compared with the current national food safety standard(GB 5413.5-2010).