Native corn starch and pretreated corn starch were treated with α-amylase, glucoamylase and mixtures of both to generate starches with high porosity with conserved granular structure. Porous starches were characterized; particle size distribution analysis, nitrogen adsorption-desorption analysis, scanning electron microscopy, water and oil adsorption capacity, differential scanning calorimeter, X-ray diffraction and damaged starch techniques were used. The α-amylase/glucoamylase mixture at the highest dose was the best treatment to generate porous starches with interesting adsorption capacity and granular structure conservation. Selected starches were impregnated with chia oil using a vacuum. Pretreated corn starch modified with the α-amylase/glucoamylase mixture showed no significant differences on impregnation capacity compared with native starch with a similar enzyme treatment. The highest oxidative stability was achieved with pretreated porous starch impregnated with 10 to 25% chia oil, compared with the bulk oil (5.37 to 4.72 and 2.58 h, respectively). Results have demonstrated that vacuum impregnation could be a potential technique for the incorporation of oil in porous structures based on starch and porous starches obtained by enzymatic hydrolysis are a promising material for the incorporation and protection of oils susceptible to oxidation.

An organic-free method was applied to produce corn starch nanoparticles, which were designed to stabilize Pickering emulsions containing chia oil, the richest vegetable source of omega-3 fatty acids. The liquid stream resulting from a laboratory-scale mill assisted by zirconia beads was filtered, centrifuged and homogenized to prepare the continuous phase of the emulsions. Experiments were performed as follows: 24 h (milling time), 0.1–0.2 mm (beads’ diameter), 1600 rpm (impeller speed), 25% (volume occupied by the grinding media), 1–7% w/v (starch concentration) and 0–1% w/v of sodium dodecyl sulfate (SDS). Particle sizes in the obtained nanosuspensions were reduced from 376–432 nm to 160–200 nm after centrifugation and homogenization. The product formulated with 0.01% w/v of SDS showed the most stable particle size during storage. Hence, this latter formulation was selected to prepare Pickering emulsions. Oil droplets showed surface mean diameters and polydispersity indexes of 283.33 ± 1.53 nm and 1.36 ± 0.03, respectively, with no significant variations during storage for around two weeks. Finally, nanosuspensions containing 7% w/v of starch, and the above three concentrations of SDS, were filtered, centrifuged, homogenized and spray-dried to obtain redispersible powders able to stabilize Pickering emulsions. The most stable particle size after redispersion (385.83 ± 5.85 nm) was obtained with the highest concentration of SDS. Moreover, SEM images revealed the presence of round-shaped particles with sizes below 1 μm. These results highlight that wet-stirred media milling can be applied as a green-method to produce new food-grade starch nanoparticles, which are able to deliver bioactive compounds from chia oil.

Sustainable corn starch nanoparticles were prepared using media milling to stabilize omega-3-rich Pickering emulsions based on chia oil. The milling conditions were as follows: 24 h (milling time), 0.4–0.6 mm (bead diameter), 1600 rpm (impeller speed), 30% (volume occupied by the grinding media), 7% w/v (starch concentration), and 0, 0.07 and 1% w/v of sodium dodecyl sulfate (SDS). Nanosuspensions containing 7% w/v of starch and the three concentrations of SDS were filtered, centrifuged, homogenized, and spray-dried to obtain redispersible powders. The particle size ranges were 2288 ± 211, 385 ± 21, and 278 ± 11 nm with 0, 0.07 and 1% w/v of SDS, respectively. The most stable backscattering profiles obtained during a period of one week were observed with 0.07 and 1% w/v of SDS. Therefore, the surface dilatational rheology of these particles adsorbed at chia oil/water interfaces was studied. A rapid decrease in the interfacial tension within 1 h was obtained with 1% w/v of SDS (down to 3 mN/m). Moreover, the most stable particle size after redispersion was obtained with the highest concentration of SDS. Finally, Pickering emulsions were prepared, and significant coalescence was observed with 0 and 0.07% w/v of SDS (within a few minutes). Nonetheless, in the presence of 1% w/v of SDS, oil droplets showed mean diameters and polydispersity indexes of 280.13 ± 4.60 nm and 0.35 ± 0.02, respectively, with no significant variations during storage for around 1 month. The results show that wet-stirred media milling can be applied to produce sustainable, new food-grade starch nanoparticles able to deliver bioactive compounds from chia oil.