Air-filled microcapsules were prepared by freeze-drying different oil-in-wa
ter emulsions containing biodegradable polyester as the wall-forming materi
al. The aim of this work was to find an acceptable formulation with respect
to the microcapsule suspension and the stability of the emulsion during th
e production process. The influence of various formulation parameters (conc
entrations of mannitol, polymer, and surfactant; pH; oil-in-water phase rat
io) was investigated in a factorial design. The results were treated by ord
inary least-square (OLS) regression and partial least-square regression (PL
SR). In a previous work, air-filled microcapsules were successfully made us
ing human serum albumin as the surfactant in the emulsion (1). In the prese
nt work, a new block copolymer based on poly(ethylene glycol) (PEG) was imp
lemented as the surfactant to replace human serum albumin. It was found tha
t the new block copolymer is a suitable replacement for human serum albumin
. The concentration of the polymer in water and the concentration of the su
rfactant ain the oil phase and the interaction between these variables had
a significant influence on the stability of the emulsion at 60 degrees C. A
surfactant concentration of approximately 2% (w/w) in water was necessary
when the concentration of the wall-forming polymer was below 5% (w/v) in (-
)-camphene. The concentration of the polymer in the oil phase influenced th
e yield, measured as the volume concentration of particles in suspension pe
r milligram of polymer added and as acoustic effect per milligram of polyme
r. Low levels of polymer concentration in (-)-camphene (<5% w/v) gave the h
ighest yield. Excess polymer in the oil phase did nor form microcapsules, b
ut precipitated in the suspension or was included in the wall of the microc
apsules. Addition of mannitol protected the microcapsules from being destro
yed during freeze-drying and resulted in freeze-dried products with few cra
cks, little shrinkage, and higher suspension yield.