Effect of a Change in the CaCl₂/Pectin Mass Ratio on the Particle Size, Rheology and Physical Stability of Lemon Essential Oil/W Emulgels

A three-step (rotor-stator-microfluidization-rotor stator) protocol was used to prepare 15% lemon essential oil in water emulgels using a mixture of Tween 80 and Span 20 surfactants as low molecular mass emulsifiers and 0.4% low-methoxyl citrus peel pectin as a gelling agent. Ca² + was used as a gel-promoting agent. Different CaCl₂/pectin mass ratio values from 0.3 to 0.7 were used. Emulgels showed a microstructure consisting of oil droplets embedded in a sheared gel matrix, as demonstrated by bright field optical microscopy. Laser diffraction tests showed multimodal particle size distributions due to the coexistence of oil droplets and gel-like particles. Multiple light scattering tests revealed that the physical stability of emulgels was longer as the CaCl₂/pectin mass ratio decreased and that different destabilization mechanisms took place. Thus, incipient syneresis became more important with increasing CaCl₂ concentration, but a parallel creaming mechanism was detected for CaCl₂/pectin mass ratio values above 0.5. Dynamic viscoelastic and steady shear flow properties of the emulgels with the lowest and highest CaCl₂/pectin mass ratio values were compared as a function of aging time. The lowest ratio yielded an emulgel with enhanced connectivity among fluid units as indicated by its wider linear viscoelastic region, higher storage modulus, loss modulus and viscosity values, and more shear thinning properties than those of the emulgel formulated with the highest CaCl₂/pectin mass ratio. The evolution of the dynamic viscoelastic properties with aging time was consistent with the information provided by monitoring scans of backscattering as a function of sample height.