Due to the rapid development of the corn-to-ethanol industry, the demand for process monitoring has led to the gradual substitution of traditional analytical techniques with fast and non-destructive methods such as near infrared spectroscopy. In this study, the feasibility of using Fourier transform–near infrared technology as an analytical tool to predict operational parameters (dry solids, starch, carbohydrate, and ethanol content) was investigated. Corn flour, liquefied mash, fermented mash, and distiller’s dried grains with solubles were selected to represent the feedstock, two intermediate products, and one primary co-product of corn-to-ethanol plants, respectively. Multivariate partial least square calibration models were developed to correlate near infrared spectra to the corresponding analytical values. The validation results indicate that near infrared models can be developed that will predict various parameters accurately (root mean square error of prediction: 0.16–1.14%, residual predictive deviation: 3.0–6.3). Measurement of starch or carbohydrate content in corn flour or distiller’s dried grains with solubles is challenging due to low accuracy of wet chemistry methods as well as sample complexity. The study demonstrated that near infrared spectroscopy, a high-throughput analytical technique, has the potential to replace the enzymatic assay.
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