Microencapsulation facilitates incorporating bioactive
volatile
compounds into products throughout the food, health, and cosmetics
industries. To minimize the number of ingredients when microencapsulating
volatile oils, we examined surfactant-free encapsulation of d-limonene in cross-linked alginate microcapsules (CLAMs) via in situ
cross-linking during spray drying. Surfactant-free CLAMs (SF-CLAMs)
were prepared by forming a Pickering d-limonene emulsion
stabilized by calcium carbonate nanoparticles (CaCO3-NPs),
combining with alginates, and then spray drying. CaCO3-NPs
served as both the emulsifier and the reservoir of alginate cross-linking
agent. SF-CLAMs, with a volatile retention of 73.1 ± 4.7% and
total limonene content of 13.6 ± 8.6% (w/w, d.b.), exhibited
core–shell morphology where CaCO3-NPs surrounded
large emulsion cores (∼5 μm) encased in densely cross-linked
alginate shells. Limonene was fully retained for up to 4 h in SF-CLAMs
in water at 37 °C. Moreover, microencapsulation in SF-CLAMs minimized
release in simulated gastric fluid (2.2 ± 0.3% in 2 h) while
fully releasing in simulated gastric fluid at 37 °C.