Peppermint essential oil is encapsulated by inverse ionotropic gelation in core–shell systems, composed of alginate (ALG) alone or alginate with shellac gum (SHL) and/or carrageenan (CRG). A mixture design approach is used to evaluate the correlation between the formulation composition and some properties of the final products. Immediately after the preparation, capsules appear rounded with a smooth and homogeneous surface, having a similar particle size ranging from 3.8 mm to 4.5 mm. The drying process, carried out at 40 °C in an oven for 3 h, reduces capsules’ diameters by at least 50% and has a negative impact on the shape of the systems because they lose their regular shape and their external membrane partially collapses. The peppermint essential oil content of dried capsules is between 14.84% and 33.75%. The swelling behaviour of the systems is affected by the composition of their outer shell. When the external membrane is composed of alginate and shellac gum, the capsule ability to swell is lower than that of the systems containing alginate alone. The swelling ratio reaches 31% for alginate capsules but does not exceed 21% if shellac is present. Differently, when the second polymer of the shell is carrageenan, the swelling ability increases as a function of polymer concentration and the swelling ratio reaches 360%. In the case of systems whose outer membrane is a polymeric ternary mixture, the swelling capacity increases or decreases according to the concentrations of the individual polymers. The obtained results suggest that carrageenan could be a useful excipient to increase the swelling behaviour of the systems, while shellac gum makes the system shell more hydrophobic. The use of a mixture design (i.e., the use of ternary diagrams and related calculations), in which each single component is chosen to provide specific properties to the final mixture, could be the right approach to develop improved formulations with a tailored essential oil release profile.
Spray congealing technique was exploited to produce solid lipid microparticles (SLMp) loaded with a highly water-soluble drug (metoclopramide hydrochloride) dissolved in the aqueous phase of a water in oil (W/O) emulsion. The use of an emulsion as starting material for a spray congealing treatment is not so frequent. Moreover, for this application, a W/O emulsion with a drug dissolved in water is a totally novel path. A ternary diagram was built to optimize the emulsion composition, a factorial design was used to identify the factors affecting the properties of the microparticles and a Design of Experiment strategy was applied to define the impact of process conditions and formulation variables on the SLMp properties. SLMp were characterized by particle size distribution, morphology, residual moisture, drug content, release behavior, FT-IR analysis and XRPD. The obtained microparticles presented a spherical shape, particle size distribution between 54–98 µm depending on atomizing pressure used during the production step and 2–5% residual moisture 4 days after the preparation. XRPD analysis revealed that lipid polymorphic transition alfa-beta occurs depending on the presence of water. In vitro drug release tests highlighted that all the formulations had a reduced release rate compared to the drug alone. These results suggest that spray congealing of a W/O emulsion could be proposed as a good strategy to obtain SLMp with a high loading of a hydrophilic drug and able to control its release rate.
The ionotropic gelation technique was chosen to produce vitamin D3-loaded microparticles starting from oil-in-water (O/W) Pickering emulsion stabilized by flaxseed flour: the hydrophobic phase was a solution of vitamin D3 in a blend of vegetable oils (ω6:ω3, 4:1) composed of extra virgin olive oil (90%) and hemp oil (10%); the hydrophilic phase was a sodium alginate aqueous solution. The most adequate emulsion was selected carrying out a preliminary study on five placebo formulations which differed in the qualitative and quantitative polymeric composition (concentration and type of alginate selected). Vitamin D3-loaded microparticles in the dried state had a particle size of about 1 mm, 6% of residual water content and excellent flowability thanks to their rounded shape and smooth surface. The polymeric structure of microparticles demonstrated to preserve the vegetable oil blend from oxidation and the integrity of vitamin D3, confirming this product as an innovative ingredient for pharmaceutical and food/nutraceutical purposes.
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