Pterostilbene (PTE) grapeseed oil emulsion was prepared by spray drying. The effects of spray drying temperature (100 °C–180 °C) on the physical properties, encapsulation efficiency of PTE, and volatile organic compounds were studied. The microcapsule powder formed at 140 °C had a high yield (53.14%), good particle integrity, and small powder particle size, and the corresponding reconstituted emulsion had a small droplet size. With the spray drying temperature increasing from 100 to 180 °C, the encapsulation efficiency of PTE in microcapsule powder decreased from 74.6% to 55.2%. The results of electronic nose and GC-IMS showed that the aroma components of grapeseed oil, such as 2-methyl butyraldehyde, 3-methyl butyraldehyde, acetone, butanone, ethanol, and 1-hexanol were well preserved after emulsification and spray drying. The results of this study are expected to promote the development of PTE-containing grapeseed oil microcapsule products for functional foods.
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