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• Starch-chitosan-Pluronic® F127 blends form microparticle powders by spray drying.
• The powders have low hydrophilicity, reflected in a low water activity.
• The microparticles showed a bowl-shaped morphology.
• The biopolymer blend with F127 at 3% (w/v) has the best yield.
• The biopolymer blend with F127 at 3% (w/v) showed the best thermal stability.
Using biopolymers as wall materials in spray drying poses challenges, particularly in attaining flowability and thermal stability among their physicochemical properties. This paper addresses these challenges by preparing microparticles using a blend of starch–chitosan and a poloxamer, commercially named Pluronic® F127. We aimed to elucidate the effects of varying poloxamer concentrations on the resulting particles through the spray drying technique. Blends with a poloxamer concentration of 3% (w/v) demonstrated a notably higher yield, especially when compared to those with 0% and 1% concentrations. Microparticles with 3% and 5% (w/v) poloxamer displayed a narrower particle size distribution, with the 3% blend showing a superior yield attributed to arrangements of blend components that improve flowability. X-ray diffraction analysis showcased the characteristic peaks of A-type starch form, with shifts suggesting enhanced interactions between components. Microparticles with increased poloxamer content showed elevated thermal degradation temperatures, with the 3% blend registering a significant rise, opening avenues for encapsulating heat-sensitive bioactive. This study primarily focuses on the preparation and basic characterization of microparticles. It underscores the potential of blends with optimal poloxamer concentrations in microencapsulation, emphasizing further research to harness their capabilities thoroughly.