Protein bars have become a popular option among consumers to increase protein content in their diets. Since there is a large market for protein bars, many factors must be considered when creating a protein bar that both satisfies consumers and has a long shelf-life. Hardening and textural changes in protein bars are some of the most common modes of shelf-life failure in this product category. When the typical product creation timeline from formulation to launch can be as short as 3-6 months and with added pressure from executives to quickly launch another new product afterwards, product development scientists simply do not have time to test the full shelf life of their product before release. For this reason, it is imperative that rapid methods for detecting bar hardness and predicting shelf life of bar formulations are developed. The objective of this research is to utilize calorimetric techniques to rapidly detect and identify bar hardening reactions. Six different protein bar formulations were studied, with each containing a combination of either whey protein isolate (WPI), milk protein isolate (MPI), or partially hydrolyzed whey protein isolate (HWPI), reducing-sugar, non-reducing sugar, and vegetable shortening. All bars were stored at 45°C and ambient humidity for 21 d. Isothermal microcalorimetry (IMC) was used to evaluate bar hardening-related reactions and was compared to objective and subjective hardness measurements. Hardness, color, water activity, moisture content, and sensory evaluation were measured at d 1, 7, 14, and 21. The results of this study indicate that isothermal calorimetry may be used to narrow down bar hardening reactions and points to Maillard browning as a main driver of hardening. These techniques may be used to predict bar shelf life, if Maillard browning is used as the basis for hardening. Furthermore, this research highlights the importance of ingredient selection during bar formulation to minimize hardening.

Master of Science / Food Science Institute / J. Scott Smith / Carboxymethyllysine (CML) and other advanced glycation end products (AGEs) have been shown to affect diseases such as diabetes, cancer, and Alzheimer’s by inducing oxidative stress, inflammation, and tissue damage. CML is formed in foods through Maillard browning reactions and through various mechanisms that are affected by time, temperature, pH, water activity, trace metals, and antioxidants. Natural antioxidants can be found in plant and fruit extracts, as well as in spices. The research contained herein is in two parts. The first part includes preliminary work, which examines the percent recovery of CML from various solid phase extraction columns, the analysis of CML in maple syrup, barbeque sauce, honey, and infant formula. The data show that solid phase extraction with a C-18 cartridge produced the highest percent recovery when using a CML standard at 100 ppb, with a recovery of 69%. Furthermore, the analysis of the syrups and sauces is inconclusive, due to the very low levels of CML detected in the infant formula, and the complications due to the high levels of reducing sugars. The second part of the research examines the effect that cinnamon, onion, garlic, black pepper, and rosemary have on CML levels in biscuits. The data show that all of the spices inhibit the formation of CML, at each of the 0.5%, 1%, and 2% levels used in the experiment, by a minimum of 3% in 2% onion samples and a maximum of 79% in 0.5% cinnamon samples when looking at the cumulative data. When looking subsets of the data, the CML inhibition was a minimum of 59% in 2% onion samples and a maximum of 74% in 0.5% cinnamon samples. Other trends can be observed in the chroma values in the CML color data, which suggest that chroma values decrease as the spice level increases, but these are not statistically significant. They may be due to color from the spices themselves, or to the chemical changes in the Maillard reaction.

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