Multivariate near-infrared and Raman spectroscopic quantifications of the crystallinity of lactose in whey permeate powder

The use of near-infrared (NIR) and Fourier transform Raman spectroscopy for quantification of crystalline lactose content in whey permeate powder was investigated using chemometric methods. Sample sets consisting of binary mixtures of crystalline (50.0-98.0%) and amorphous lactose and process whey permeate samples with different amounts of crystalline lactose (75.0-95.5%) added were analyzed. The best results for quantification of crystallinity were obtained by partial least squares (PLS) regression on NIR data in five selected intervals in the range 1100-2498 nm. Data analysis on the total sample set of 35 samples yielded a prediction error (root mean square error of cross validation) of 0.627%. The corresponding result for Raman spectroscopy in the range 3500-100 cm−1 was 1.62%. Interval-PLS regression was used for the selection of relevant spectral intervals as well as for improving the spectral interpretation. Alternating regression was used to show that the amorphous lactose preparation contained only a negligible amount of crystalline lactose.