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Mass Spectrometric Approaches to Study Protein Structure and Interactions in Lyophilized Powders

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Integrated Analytical Approach to Identify Whey Permeate Powder Caking: Revealing Internal Structure Using X-Ray

Marek Szołtysik¹, Nesa Dibagar², Małgorzata Serowik³

¹Department of Functional Food Products Development, Faculty of Biotechnology and Food Science, Wrocław University of Environmental and Life Sciences, 37a Chełmońskiego Str., 51-630 Wrocław, Poland.

Molecules (Basel, Switzerland)

|May 27, 2026

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Caking in whey permeate powders (WPPs) is linked to moisture. Higher water activity and altered particle size distribution in caked WPPs correlate with structural changes, including particle clustering and solid bridging.

Area of Science:

Food Science
Materials Science
Powder Technology

Background:

Caking is a major stability issue for whey permeate powders (WPPs).
It arises from moisture-induced structural changes during storage and handling.
Understanding these changes is crucial for maintaining powder quality.

Purpose of the Study:

To investigate the physical, morphological, and microstructural properties of caked WPPs.
To identify key characteristics differentiating caked WPPs from free-flowing powders.
To explore the relationship between moisture, powder structure, and caking.

Main Methods:

Characterization of five commercial WPP samples.
Analysis of dry matter content, water activity (a_w), particle size distribution (PSD), bulk density, porosity, and color.

Keywords:

caking behavior dairy-based powder instability lactose recrystallization micro-CT

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Mass Spectrometric Approaches to Study Protein Structure and Interactions in Lyophilized Powders

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$Crystallization of Proteins on Chip by Microdialysis for In Situ X-ray Diffraction Studies$

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X-ray micro-computed tomography (micro-CT) for microstructural analysis.

Main Results:

Caked WPP (WPP2) showed higher a_w (0.261), lower bulk density (676 kg/m^3), higher porosity (0.569), and coarser PSD compared to free-flowing powders.
WPP2 exhibited a higher yellowness index (44.45), indicating altered light scattering.
Micro-CT revealed enlarged particle clusters, solid bridging, heterogeneous pores, and reduced void connectivity in WPP2.

Conclusions:

Integrated analysis combining conventional methods and micro-CT provides comprehensive insights into WPP caking.
Moisture-related properties significantly influence the internal powder structure and caking behavior.
Microstructural changes like particle clustering and solid bridging are key indicators of caking in WPPs.