Near-Infrared Spectroscopy Coupled with Chemometrics and Artificial Neural Network Modeling for Prediction of Emulsion Droplet Diameters

Abstract

There is increased interest in the food industry for emulsions as delivery systems to preserve the stability of sensitive biocompounds with the aim of improving their bioavailability, solubility, and stability; maintaining their texture; and controlling their release. Emulsification in continuously operated microscale devices enables the production of emulsions of controllable droplet sizes and reduces the amount of emulsifier and time consumption, while NIR, as a nondestructive, noninvasive, fast, and efficient technique, represents an interesting aspect for emulsion investigation. The aim of this work was to predict the average Feret droplet diameter of oil-in-water and oil-in-aqueous mint extract emulsions prepared in a continuously operated microfluidic device with different emulsifiers (PEG 1500, PEG 6000, and PEG 20,000) based on the combination of near-infrared (NIR) spectra with chemometrics (principal component analysis (PCA) and partial least-squares (PLS) regression) and artificial neural network (ANN) modeling. PCA score plots for average preprocessed NIR spectra show the specific grouping of the samples into three groups according to the emulsifier used, while the PCA analysis of the emulsion samples with different emulsifiers showed the specific grouping of the samples based on the amount of emulsifier used. The developed PLS models had higher R2 values for oil-in-water emulsions, ranging from 0.6863 to 0.9692 for calibration, 0.5617 to 0.8740 for validation, and 0.4618 to 0.8692 for prediction, than oil-in-aqueous mint extract emulsions, with R2 values that were in range of 0.8109–0.8934 for calibration, 0.5017–0.6620, for validation and 0.5587–0.7234 for prediction. Better results were obtained for the developed nonlinear ANN models, which showed R2 values in the range of 0.9428–0.9917 for training, 0.8515–0.9294 for testing, and 0.7377–0.8533 for the validation of oil-in-water emulsions, while for oil-in-aqueous mint extract emulsions R2 values were higher, in the range of 0.9516–0.9996 for training, 0.9311–0.9994 for testing, and 0.8113–0.9995 for validation.