Characterization of spray dried powders by near infrared spectroscopy
Tu, Zhiyang (Stan)
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Permalink
https://hdl.handle.net/2142/120352
Description
Title
Characterization of spray dried powders by near infrared spectroscopy
Author(s)
Tu, Zhiyang (Stan)
Issue Date
2023-04-11
Director of Research (if dissertation) or Advisor (if thesis)
Lee, Youngsoo
Department of Study
Food Science & Human Nutrition
Discipline
Food Science & Human Nutrition
Degree Granting Institution
University of Illinois at Urbana-Champaign
Degree Name
M.S.
Degree Level
Thesis
Keyword(s)
Spray Drying
NIR spectroscopy
PLS regression
microencapsulation
Abstract
The process control of spray drying is a complicated and time consuming process involving various drying parameters as well as product characteristics. The emergence of portable NIR provides opportunities for rapid inline analysis of spray dried products and hence enhances the process control of spray drying and promotes the qualities of spray dried products.
The overall objective of this study was to characterize physico-chemical properties of spray dried products by near infrared (NIR) spectroscopy. A portable miniature NIR spectrometer with wavelength range 1650 nm to 2400 nm was evaluated as a rapid analytical tool. The analysis of protein content, moisture content, and peroxide value in spray dried products by NIR was investigated. Chemometric techniques were applied and evaluated for enhancing the precision and accuracy of NIR analysis.
The first specific objective was to assess the performance of NIR protein predictive models built on a sample set with a wide range of protein contents applied to a sample set with a focused range of protein content. Two sample sets, one with widely distributed protein content (8.6% to 22.8%) and the other one with narrowly distributed protein content (13.0% to 15.6%) were prepared for NIR calibration models. A total of 41 microencapsulation delivery systems were spray dried, characterized for protein content, and scanned for NIR spectra. It was found that models built on a widely distributed sample set can characterize samples with narrowly distributed protein contents with good precision and accuracy
The second specific objective was to compare a portable miniature NIR spectrometer and a benchtop NIR spectrometer for establishing NIR predictive models for moisture content of spray dried microencapsulation delivery system. The results showed that the portable NIR spectrometer achieved comparable analytical results as the benchtop spectrometer. The portable NIR spectrometer was a promising tool for rapid moisture analysis for spray dried samples and process control of spray drying.
The third specific objective was to characterize the primary lipid oxidation of spray dried flaxseed oil microcapsules by NIR spectroscopy. Flaxseed oil microcapsules were formulated, spray dried, and stored at 60 °C to accelerate the oxidation. The portable NIR spectrometer was used to collect NIR spectra. The NIR calibration models for peroxide value achieved good linear fitting (coefficient of determination, R2) and low prediction errors (root mean square errors in validation). NIR spectroscopy has the potential for rapid analysis of primary lipid oxidation in flaxseed oil microcapsules, which may enhance control of product quality.
The findings in this study demonstrated that NIR spectroscopy is a reliable tool for the analysis of moisture content, protein content, and peroxide value in spray dried products. Inline applications of NIR spectroscopy can improve process control of spray drying and product qualities of spray dried powders.
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