Milk tablets are a popular dairy product in many Asian countries. This research aimed to develop an instant and rapid method for determining sucrose and lactose contents in milk tablets using near-infrared (NIR) spectroscopy. For the quantitative analysis, a training set composed of laboratory-scale milk samples was generated based on a central composite design (CCD) and used to establish partial least squares (PLS) regression for the predictions of sucrose and lactose contents resulting in R2 values of 0.9749 and 0.9987 with the corresponding root mean square error of calibration (RMSEC) values of 1.69 and 0.35. However, the physical difference between the laboratory-scale powder and the final product milk tablet samples resulted in spectral deviations that dramatically affected the predictive performance of the PLS models. Therefore, calibration transfer methods called direct standardization (DS) and piecewise direct standardization (PDS) were used to adjust the NIR spectra from the real milk tablet samples before the quantitative prediction. Using high-performance liquid chromatography (HPLC) as a reference method, the developed NIR-chemometric model could be used to instantly predict the sugar contents in real milk tablets by producing root mean square error of prediction (RMSEP) values for sucrose and lactose of 5.04 and 4.22 with Q2 values of 0.7973 and 0.9411, respectively, after the PDS transformation.
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