Corrigendum to "Influence of saliva on individual in-mouth aroma release from raw cabbage (Brassica oleracea var. capitata f. rubra L.) and links to perception" [Heliyon 4 (12) (December 2018) e01045].

[This corrects the article DOI: 10.1016/j.heliyon.2018.e01045.].

Influence of saliva on individual in-mouth aroma release from raw cabbage (Brassica oleracea var. capitata f. rubra L.) and links to perception.

Raw or minimally processed vegetables are popular for health reasons and for their unique textural and flavor attributes. While many aroma volatiles are produced in situ when plant tissues are mechanically disrupted, enzymes expressed in bacteria in oral microbiota such as cysteine-ß-lyase (EC 4.4.1.13) may also contribute to aroma formation in-mouth during consumption. Interactions between raw cabbage and fresh human saliva (n = 21) were measured ex vivo by real-time monitoring of sulfur volatile production by proton transfer reaction mass spectrometry (PTR-MS). Inter-individual differences in the concentration of sulfur volatiles from the breakdown of S-methyl-L-cysteine sulfoxide (SMCSO) in fresh cabbage by saliva were characterized and a 10-fold difference in the extent of sulfur volatile production was measured across individuals. The overall intensity and garlic odor of raw cabbage was positively correlated with the concentration of sulfur volatiles after incubation with fresh human saliva. A buildup of SMSCO-derived sulfur volatiles in vivo, over twenty repeated mouthfuls was demonstrated, indicating that these reactions can affect sensory perception within the timescale of eating. These findings show the perceived odor experienced when eating cabbage differs, thus resulting in a unique flavor experience between individuals.

Effects of Agar Gel Strength and Fat on Oral Breakdown, Volatile Release, and Sensory Perception Using in Vivo and in Vitro Systems.

The density and composition of a food matrix affect the rates of oral breakdown and in-mouth flavor release as well as the overall sensory experience. Agar gels of increasing concentration (1.0, 1.7, 2.9, and 5% agarose) with and without added fat (0, 2, 5, and 10%) were spiked with seven aroma volatiles. Differences in oral processing and sensory perception were systematically measured by a trained panel using a discrete interval time intensity method. Volatile release was measured in vivo and in vitro by proton transfer reaction mass spectrometry. Greater oral processing was required as agar gel strength increased, and the intensity of flavor-related sensory attributes decreased. Volatile release was inversely related to gel strength, showing that physicochemical phenomena were the main mechanisms underlying the perceived sensory changes. Fat addition reduced the amount of oral processing and had differential effects on release, depending on the fat solubility or lipophilicity of the volatiles.

In vitro measurement of volatile release in model lipid emulsions using proton transfer reaction mass spectrometry.

The presence of fat in food plays an important role in the way aroma is released during consumption and in the creation of the overall sensory impression. Fat acts as a reservoir for lipophilic volatile compounds and modulates the timing and delivery of aroma compounds in a unique manner. Despite considerable research, reproducible in vitro methods for measuring the effect of fat on volatile release are lacking. An open in vitro cell was used to simulate the open human naso-oropharygeal system and was interfaced with a proton transfer reaction mass spectrometer (PTR-MS) to examine some of the fundamental effects of fat on dynamic volatile release in liquid fat emulsions. Lipid emulsions with various fat contents (0-20%) and droplet sizes (0.25, 0.5, and 5.0 µM) were spiked with flavor volatiles representing a range of lipophilicity (K(o/w) = 1-1380). Preloaded syringes of spiked emulsion were injected into the cell, and temporal changes in release were measured under dynamic conditions. Significant differences in release curves were measured according to the lipid content of emulsions, the vapor pressure, and K(o/w) values of the volatile compounds. With increasing addition of fat, the critical volatile release parameters, maximum concentration (I(max)), time to maximum concentration (T(max)), and the integrated area under the concentration curve (AUC), were affected. The in vitro curves were reproducible and in agreement with theory and correlated with the preswallow phase of in vivo release data. An exponential model was used to calculate changes in mass transfer rates with increased fat addition.

Proton transfer reaction mass spectrometry and time intensity perceptual measurement of flavor release from lipid emulsions using trained human subjects.

The effect of the fat component of liquid emulsions on dynamic "in-nose" flavor release was examined using a panel of trained human subjects (n = 6), proton transfer reaction mass spectrometry (PTR-MS), and time intensity (TI) sensory evaluation. A rigorous breathing and consumption protocol was developed, which synchronized subjects' breathing cycles and also the timing of sample introduction. Temporal changes in volatile release were measured in exhaled nostril breath by real-time PTR-MS. Corresponding changes in the perceived odor intensity could also be simultaneously measured using a push button TI device. The method facilitated accurate examination of both "preswallow" and "postswallow" phases of volatile release and perception. Volatile flavor compounds spanning a range of octanol/water partition coefficient (K(o/w)) values (1-1380) were spiked into water (0% fat) or lipid emulsions with various fat contents (2, 5, 10, and 20% fat). Replicate samples for each fat level were consumed according to the consumption protocol by six subjects. Statistical comparisons were made at the individual level and across the group for the effects of changes in the food matrix, such as fat content, on both pre- and postswallow volatile release. Significant group differences in volatile release parameters including area under the concentration curve (AUC) and maximum concentration (I(max)) were measured according to the lipid content of emulsions and volatile K(o/w). In a second experiment, using single compounds (2-heptanone, ethyl butanoate, and ethyl hexanoate), significant decreases in both in-nose volatile release and corresponding perceived odor intensities were measured with increasing fat addition. Overall, the effect of fat on in vivo release conformed to theory; fat had little effect on compounds with low K(o/w) values, but increased for volatiles with higher lipophilicity. In addition, significant pre- and postswallow differences were observed in AUC and I(max), as a result of changing fat levels. In the absence of fat, more than half of the total amount of volatile was released in the preswallow phase. As the content of fat was increased in the emulsion systems, the ratio of volatile released postswallow increased compared to preswallow. These data may provide new insights into why low-fat and high-fat foods are perceived differently.

Effects of thermal denaturation on the solid-state structure and molecular mobility of glycinin.

The effects of moisture and thermal denaturation on the solid-state structure and molecular mobility of soy glycinin powder were investigated using multiple techniques that probe over a range of length and time scales. In native glycinin, increased moisture resulted in a decrease in both the glass transition temperature and the denaturation temperature. The sensitivity of the glass transition temperature to moisture is shown to follow the Gordon-Taylor equation, while the sensitivity of the denaturation temperature to moisture is modeled using Flory's melting point depression theory. While denaturation resulted in a loss of long-range order, the principal conformational structures as detected by infrared are maintained. The temperature range over which the glass to rubber transition occurred was extended on the high temperature side, leading to an increase in the midpoint glass transition temperature and suggesting that the amorphous regions of the newly disordered protein are less mobile. (13)C NMR results supported this hypothesis.

Structure and molecular mobility of soy glycinin in the solid state.

We report a multitechnique study of structural organization and molecular mobility for soy glycinin at a low moisture content (<30% w/w) and relate these to its glass-to-rubber transition. Small-angle X-ray scattering (SAXS), differential scanning calorimetry (DSC), Fourier transform infrared (FTIR) spectroscopy, and nuclear magnetic resonance (NMR) spectroscopy are used to probe structure and mobility on different length and time scales. NMR (approximately 10(-6) to 10(-3) s) reveals transitions at a higher moisture content (>17%) than DSC or SAXS, which sample for much longer times (approximately 10 to 10(3) s) and where changes are detected at >13% water content at 20 degrees C. The mobility transitions are accompanied by small changes in unit-cell parameters and IR band intensities and are associated with the enhanced motion of the polypeptide backbone. This study shows how characteristic features of the ordered regions of the protein (probed by SAXS and FTIR) and mobile segments (probed by NMR and DSC) can be separately monitored and integrated within a mobility transformation framework.

Processing of novel elevated amylose wheats: functional properties and starch digestibility of extruded products.

Different types of novel wheat lines with different starch contents and amylose/amylopectin ratios, relating to defined alterations in the number and activity of starch synthase IIa genes, were processed by pilot-plant extrusion. Two types of products were produced: pure wholemeal products and breakfast cereals made from wholemeal/maize blends. Lower apparent shear viscosity was obtained in the extruder with lower starch content and higher amylose/amylopectin ratio flours (SSIIa-deficient line). The bulk density of the products decreased with increasing extrusion temperature and was always higher for the triple-null line. The bulk density was not completely explained by the melt shear viscosity, suggesting the importance of the fillers (fibers, brans) in the process of expansion and structure acquisition. The different mechanical properties were explained by the density and by the material constituting the cell walls. Enzyme-resistant starch (RS) content and hydrolysis index (HI) were not correlated to the extrusion temperature, but RS was higher in pure wholemeal products and in the SSIIa-deficient line. These results are discussed in terms of starch molecular architecture and product microstructure.

Influence of storage conditions on the structure, thermal behavior, and formation of enzyme-resistant starch in extruded starches.

Starch structures from an extrusion process were stored at different temperatures to allow for molecular rearrangement (retrogradation); their thermal characteristics (DSC) and resistance to amylase digestion were measured and compared. The structure of four native and processed starches containing different amylose/amylopectin compositions (3.5, 30.8, 32, and 80% amylose content, respectively) before and after digestion was studied with small-angle X-ray scattering (SAXS) and X-ray diffraction (XRD). Rearrangement of the amylose molecules was observed for each storage condition as measured by the DSC endotherm at around 145 degrees C. The crystalline organization of the starches after processing and storage was qualitatively different to that of the native starches. However, there was no direct correlation between the initial crystallinity and the amount of enzyme-resistant starch (ERS) measured after in vitro digestion, and only in the case of high-amylose starch did the postprocess conditioning used lead to a small increase in the amount of starch remaining after the enzymatic treatment. From the results obtained, it can be concluded that retrograded amylose is not directly correlated with ERS and alternative mechanisms must be responsible for ERS formation.

Reexamining the egg-box model in calcium-alginate gels with X-ray diffraction.

The structure of the Ca--alginate junction zones was investigated with X-ray scattering on gels prepared with different methods. Fiber diffraction reveals the popular egg-box model may not be the only possible structure for the junction zones. The (001) reflection, which should be extinguished due to 2/1 helical conformation in the egg-box model, was observed. This was further confirmed by the measurements on Ca--alginate gel beads prepared at different pH where large pieces were formed through a relatively slow process, which leads to a higher crystallinity and a more perfect ordering. The results suggest a 3/1 helical conformation is more proper for Ca--alginate gels formed slowly. This does not exclude the possibility for the 2/1 helical conformation in fast gelatinized Ca--alginate in which the 2/1 helix is a metastable form. Comparing the X-ray scattering results of the fresh, dehydrated, and rehydrated gels, a reversible aggregation of junction zones is found during dehydration and rehydration. The different stabilities of initial bonds and bonds formed during drying are speculated to be the contribution of MG block or short G blocks in the junction zones.

Associative and segregative phase separations of gelatin/kappa-carrageenan aqueous mixtures.

The effects of ionic strength, temperature, and pH on the phase separation behavior of type B pigskin gelatin/sodium-type kappa-carrageenan aqueous mixtures were investigated. Depending on the different combinations of temperature and sodium chloride (NaCl) concentration, the mixtures showed compatible, associative, and segregative phase separation behaviors. Additionally, a coexistence of associative and segregative (associative-co-segregative) phase separations was expected at low temperature and low NaCl concentration. These different phase separation events were observed using confocal scanning laser microscopy. Moreover, it was found that the segregative phase separation when alone is induced by the ordering of kappa-carrageenan chains, while that in the coexistence region is induced by the ordering of gelatin chains. pH had a significant effect on the associative phase separation, resulting in morphologies changing from compatible solution to liquid coacervate and further to solid precipitate with decreasing pH. These were attributed to the dramatic changes of the charge density of amphoteric gelatin during the pH decrease.

Gelled emulsion particles for the controlled release of lipophilic volatiles during eating.

Gelled emulsion particles are discussed in relation to controlling the release of lipophilic volatiles in the mouth during eating, using a mass spectroscopic technique that enables real time measurement of volatiles on the breath. Our studies have demonstrated that by encapsulating triglyceride oil droplets within biopolymer gelled particles (70-5000 microm), the initial flavour release maxima were reduced by kinetically inhibiting the mass transfer of flavour through the particle. An important feature of this approach was that it was the oil droplets and not the volatiles that were encapsulated. Factors such as particle size, oil phase volume and the partition coefficient of the volatile all affected the rate of volatile release. To control the temporal release profile, gelled emulsion particles have been designed that break down in a controlled manner under physiological conditions in the mouth. The physiological 'trigger mechanisms' investigated included mechanical failure, melting and enzyme hydrolysis.