Abstract: Milk proteins are liable to react with lactose during thermal processing, causing changes in color, flavor and nutritional function. In order to understand the accuracy and applicability of front-face fluorescence spectroscopy, the extents of Maillard reaction of the milk samples with various degrees of heat treatments were measured by three Maillard reaction tests and front-face fluorescence spectroscopy (FFFS) respectively. A strong correlation was found between FFFS, furosine and hydroxymethylfurfural. Moreover, a good prediction of hydroxymethylfurfural concentration was got in commercial milk samples using this model. This work indicated that FFFS had the reliability and sensitivity to monitor and control the thermal processing of milk.