Spectral Degradation Markers in Lipid Profile of Whole Milk Powder during Storage

Whole milk powder is one of the most sought-after dairy ingredients due to its high nutritional value, long shelf life, and wide range of functional and technological properties. However, milk powder is rich in lipids, which makes it sensitive to oxidative and hydrolytic spoilage, resulting in the accumulation of milk fat degradation products and quality deterioration. New rapid, non-destructive testing methods can identify the early stages of spoilage in whole milk powder. This research evaluated the use of Raman spectroscopy for the early detection of spoilage in whole milk powder during storage.
The study featured samples of whole milk powder stored at 45 ± 2°C for 15 weeks, with analysis performed in 3-week increments. Raman spectra were recorded using a portable EnSpectr R785 Raman spectrometer (Russia). Changes in the fatty acid composition were analyzed using a Crystallux 4000M gas chromatograph (Russia).
The most informative spectral ranges included the regions at 325–370, 375–425, 800–900, and 2840–2970 cm–1. The highest statistical significance belonged to the range of 800–900 cm–1 (F = 7.36; p < 0.001), which reflected the structural transformations of the lipid-protein component of the milk matrix. Principal component analysis (PCA) showed the non linear nature of spectral changes during storage. Gas chromatography analysis revealed a relatively stable fatty acid composition, with the exception of palmitic, stearic, and oleic acid isomers. The strongest correlation with changes in fatty acid composition during storage was observed in the low-frequency range of 325–370 cm–1.
In conclusion, the 325–370 cm–1 region exhibited the closest correlations with the gas chromatography results, while the 800–900 cm–1 region had the highest statistical significance.

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