Corn fiber product and process of preparing the same

Abstract

The present disclosure relates to a corn fiber product and a process for preparing the same. The process comprises the steps of providing a corn fiber containing material; humidifying the corn fiber containing material at a relative humidity and a humidifying temperature of less than 100°C to obtain a humidified material; and drying the humidified material to obtain the corn fiber product. The corn fiber product has content of one or more volatile compounds reduced as compared to an equivalent untreated corn fiber product.

Description

CORN FIBER PRODUCT AND PROCESS OF PREPARING THE SAMECROSS REFERENCE

[0001] This application claims the benefit of United States Provisional Application No. 63 / 572,975, filed April 2, 2024, which is hereby incorporated by reference in its entirety.FIELD OF INVENTION

[0002] This invention relates to the field of plant fiber products, in particular corn fiber products.BACKGROUND

[0003] Many ingredients refined from plants, such as plant proteins and plant fibers, have undesirable flavor characteristics due to the volatile and relatively small organic compounds bound to the surfaces. The perceived “off-flavor” often limits the application of such ingredients in making food products like baked goods, ready-to-eat cereals, nutrition bars, pasta, and snack foods.

[0004] Many of these ingredients have been through prior aqueous, alkane, or aqueous alcohol processing steps followed by high temperature evaporation processes; however, such ingredients still retain these compounds with undesirable flavors. Other ingredients are processed through dry processes that provide less potential for volatile compound removal. Proteins derived from plants are especially prone to this problem, but some relatively unrefined plant fibers and some animal- derived proteins experience off-flavors as well. Removal of these compounds results in an ingredient that is much less intensely flavored and thus more suitable for use in common foods.

[0005] Therefore, a plant fiber product (e.g., corn fiber product) having a reduced flavor intensity and an improved process for preparing such product are needed.SUMMARY

[0006] The present disclosure provides a process for preparing a com fiber product comprising the steps of providing a com fiber containing material; humidifying the corn fiber containing material at a relative humidity and a humidifying temperature of less than 100°C to obtain a humidified material; and drying the humidified material to obtain the corn fiber product. The resulting com fiber product has a reduced volatile compound content as compared to an equivalent untreated com fiber product.

[0007] The present disclosure also provides a process for reducing volatile compound content of a corn fiber product comprising the steps of humidifying a corn fiber containing material at a relative humidity from 50 to 100% and a humidifying temperature of less than 100°C to obtain ahumidified material; and drying the humidified material at a drying temperature from 50 to 90°C to obtain the corn fiber product. The resulting com fiber product has a reduced volatile compound content as compared to an equivalent untreated corn fiber product.

[0008] The present disclosure also provides a corn fiber product having content of one or more volatile compounds reduced as compared to an equivalent untreated corn fiber product.BRIEF DESCRIPTION OF THE FIGURES

[0009] The drawings illustrate generally, by way of example, but not by way of limitation, various aspects discussed in the present document.

[0010] Figure 1 shows the overall flavor intensity of treated and untreated corn fiber samples. The blind reference sample (triangle) has a concentration of 3.0% but has been moved to improve visibility. The data callouts indicate the temperature / relative humidity / time conditions during humidification.

[0011] Figure 2 is a log-log plot (log2(treated / untreated) against loglO(treated)) that shows changes in relative concentrations of volatile compounds in the samples that are humidified but not dried. Numbers in the upper left of each panel represent the treatment condition. Treatments 2 and 8 are replicates that are plotted together; treatment 2 is the lighter symbol while treatment 8 is the darker symbol. The top part of each panel shows that volatile compounds whose relative concentrations are increased because of the treatment, and the bottom part shows that concentrations of volatile compounds are decreased due to the treatment.

[0012] Figure 3 is a log-log plot (log2(treated / untreated) against loglO(treated)) that shows relative changes in concentrations of volatile compounds in the samples that are humidified and dried. Numbers in the upper left of each panel represent the treatment condition. Treatments 2 and 8 are replicates that are plotted together; treatment 2 is the lighter symbol while treatment 8 is the darker symbol. The top part of each panel shows that volatile compounds whose relative concentrations are increased because of the treatment, and the bottom part shows that concentrations of volatile compounds are decreased due to the treatment.

[0013] Figure 4 is a log-log plot (log2(treated / untreated) against loglO(treated)) that shows changes in concentrations of volatile compounds, as a function of initial concentration, in the samples. Numbers in the upper left of each panel represent the treatment condition. The top part of each panel shows that volatile compounds whose relative concentrations are increased because of the treatment, and the bottom part shows that concentrations of volatile compounds are decreased due to the treatment.DETAILED DESCRIPTION

[0014] Reference will now be made in detail to certain aspects of the disclosed subject matter. While the disclosed subject matter will be described in conjunction with the enumerated claims, it will be understood that the exemplified subject matter is not intended to limit the claims to the disclosed subject matter.

[0015] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one skilled in the art to which this invention belongs. As used herein, each of the following terms has the meaning associated with it as defined below.

[0016] Unless expressly stated, ppm (parts per million), percentage, and ratios are based on a dry weight basis. Percentage based on a dry weight basis is also referred to as wt% below .

[0017] The term "for example," "for instance," "such as," or "including" as used herein is meant to introduce examples that further clarify more general subject matter. Unless otherwise specified, these examples are provided only as an aid for understanding the applications illustrated in the present disclosure and are not meant to be limiting in any fashion.

[0018] As used herein, “room temperature” or “RT” refers to a temperature between 20°C to 25°C.

[0019] In the processes described herein, the acts can be carried out in any order without departing from the principles of the disclosure, except when a temporal or operational sequence is explicitly recited. Furthermore, specified acts can be carried out concurrently unless explicit claim language recites that they be carried out separately. For example, a claimed act of doing X and a claimed act of doing Y can be conducted simultaneously within a single operation, and the resulting process will fall within the literal scope of the claimed process.

[0020] Described herein is a com fiber product and a process of preparing the com fiber product. The corn fiber product has less flavor intensity and is suitable for use as a protein source for incorporation into foods for human and / or animal consumption.Process for preparing a corn fiber product

[0021] The present disclosure provides a process for preparing a com fiber product. The process comprises the steps of humidifying a com fiber containing material at a relative humidity and a humidifying temperature of less than 100°C to obtain a humidified material; and drying the humidified material to obtain the corn fiber product. The resulting corn fiber product has one or more improved attributes as compared to an equivalent untreated corn fiber product; preferably, the one or more improved attributes may include, but may not be limited to, a reduced volatile compound content.

[0022] As described herein, an “equivalent untreated corn fiber product” refers to an equivalent corn fiber product that has not been subjected to any process of the instant invention as describedin the present disclosure. An “equivalent com fiber product” refers to a corn fiber product prepared from the same starting material used in the instant invention (e.g., corn fiber from the same batch).

[0023] The com fiber containing material serves as a starting material to the process and may include, but may not be limited to, corn fibers recovered from dry mill process or wet mill process. A high fiber ingredient can be created by milling the pericarp of com kernels recovered from milling of corn kernels moistened to between 10 and 20 wt% moisture followed by air classification or sifting, and then further ground, with or without a prior cooking step, to a powder. This is partially milled corn. A com fiber can also be recovered from a wet milling process. In the wet mill process, corn kernels can be steeped in water for a period such as 20 to 40 hours, partially ground, and centrifuged to remove the germ, followed by a separation on a screen or centrifuge to separate the coarse fiber components from the fine protein and starch components. The fiber can be pasteurized, dried, and ground. This is fibrous material recovered from conventional corn milling, which can be known as corn gluten feed.

[0024] In one aspect, corn bran can be used as an example of the com fiber containing material and fed into the process to prepare the corn fiber product.

[0025] In one aspect, the corn fiber containing material can have a protein content of at least 1 wt%, or at least 5 wt%; for example, the com fiber containing material can have a protein content in a range from 5 to 10 wt% on a dry basis. The corn fiber containing material can have a fiber content of at least 1 wt%, or at least 5 wt%; for example, the corn fiber containing material can have a fiber content in a range from 60 to 80 wt%, or from 65 to 70 wt% on a dry basis.

[0026] In the humidifying step, the corn fiber containing material can be exposed to an atmosphere comprising, preferably a high relative humidity, more preferably a high relative humidity and a high humidifying temperature, to liberate and remove a substantial fraction of compounds (e.g., organic compounds, volatile compounds), which are responsible for causing flavor perceptions. The removed compounds may include, but may not be limited to, organic compounds, volatile compounds, or any combinations thereof. Preferably, moisture content of the resulting humidified material is not increased by the humidifying step.

[0027] In one aspect, the humidifying step at high relative humidity is more effective at elevated humidifying temperatures, but the humidifying temperature is not desirably to exceed 100°C. Preferably, steam is not to be used in the humidifying step to avoid degradation of the starting material.

[0028] Preferably, the atmosphere contacting the corn fiber containing material should be exchanged so that the liberated compounds can be swept away, but air velocity should be kept low enough to prevent the corn fiber containing material itself from being swept away. In other words,the air velocity should be maintained low enough to only remove the liberated compounds but not the com fiber containing material itself.

[0029] The relative humidity at the humidifying step can be 50%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 99%, or 100%. In one aspect, the relative humidity can be at least 50% or at most 100%. Examples of the relative humidity may include, but may not be limited to, a range from 50 to 100%, from 60 to 100% , from 60 to 99%, from 60 to 90%, from 60 to 80%, from 70 to 100%, from 70 to 99%, from 70 to 90%, or from 70 to 80%.

[0030] The humidifying temperature at the humidifying step can be 55°C, 60°C, 70°C, 80°C, 90°C, or 95°C. In one aspect, the humidifying temperature can be at least 55°C or at most 95°C. Examples of the humidifying temperature may include, but may not be limited to, a range from 55 to 95°C, from 55 to 90°C, from 60 to 95°C, from 60 to 90°C, from 70 to 95 °C, from 70 to 90°C, from 70 to 85°C, or from 70 to 80°C.

[0031] In one aspect, the humidifying step is carried out by passing humidified or warmed air to deliver water to the corn fiber containing material over one or more static beds, or one or more fluid beds. A fluid bed system that can improve air-particle contact and mass transfer may be desired. Preferably, water is uniformly delivered and distributed over the com fiber containing material; more preferably, water is delivered in a form of a vapor; even more preferably, water delivered is not in a form of liquid water or not in a form of steam.

[0032] The humidifying period for humidifying the corn fiber containing material is a function of humidifying temperature, relative humidity, surface area of the starting material, particle size of the starting material, or any combinations thereof. In one aspect, the humidifying period can be 10 minutes, 15 minutes, 30 minutes, 45 minutes, 60 minutes, 75 minutes, or 90 minutes. For example, the humidifying period can be in a range from 10 to 90 minutes, from 15 to 75 minutes, or from 30 to 60 minutes. In one aspect, the humidifying period can be at most 90 minutes.

[0033] The humidified material can be de-humidified in the drying step to obtain the final com fiber product. The drying step can be carried out at a drying temperature for a drying period to obtain the com fiber product. If excess moisture is absorbed by the humidified material, gentle drying can remove the excess moisture and restore and / or establish the desired moisture content in the corn fiber product.

[0034] The drying temperature can be less than 100°C and can be 50°C, 55°C, 60°C, 70°C, 75°C, 85°C, or 90°C. In one aspect, the drying temperature can be at least 50°C or at most 90°C. Examples of the drying temperature may include, but may not be limited to, a range from 50 to 90°C, from 50 to 85°C, from 60 to 90°C, from 60 to 85°C, from 70 to 95°C, from 70 to 90°C, or from 70 to 85°C.

[0035] The drying period can be 5 minutes, 8 minutes, 10 minutes, 15 minutes, 20 minutes, or 25 minutes. For example, the drying period can be in a range from 5 to 25 minutes, from 8 to 20 minutes, from 10 to 15 minutes. In one aspect, the drying period can be at least 5 minutes. In another aspect, the drying period can be at most 25 minutes.

[0036] The relative humidity at the drying step can be 0%, from 0 to 0.5%, from 0.5% to 1%, or at least 1%.

[0037] In one aspect, each of the humidifying step and the drying step can be performed for one or more than one time, preferably for at least two times, more preferably for two times. Preferably, the humidifying step and the drying step can be carried out as a cycle and the cycle can be performed for one or more than one time, preferably for at least two times, more preferably for two times.

[0038] The com fiber product obtained from the process as described above has content of one or more volatile compounds reduced as compared to an equivalent untreated com fiber product. Preferably, the content of one or more volatile compounds in the corn fiber product can be reduced by at least 1%, at least 5%, at least 10%, at least 25%, at least 50%, at least 75%, at least 90%, at least 95%, or at least 98% as compared to an equivalent untreated com fiber product. More preferably, the content of one or more volatile compounds in the com fiber product can be reduced by 100% as compared to an equivalent untreated com fiber product.Process for reducing volatile compound content of a corn fiber product

[0039] The present disclosure provides a process for reducing volatile compound content of a corn fiber product. Preferably, off-notes of the corn fiber product are reduced by the process of the instant invention.

[0040] As described herein, an “off-note”, “off-taste”, or “off-flavor” is an undesirable and / or unwanted flavor (e.g., taste, odor) present in food products. An “off-note” can be originated from raw materials and / or derived from chemical changes during food processing and storage. Examples of compounds generating “off-note” may include, but may not be limited to, aldehydes, ketones, alcohols, carboxylic acids, sulfur-containing compounds, heterocyclic compounds, or other small volatile compounds.

[0041] The process comprises a step of humidifying a corn fiber containing material at a relative humidity from 50 to 100% and a humidifying temperature of less than 100°C to obtain a humidified material. The humidified material is then dried at a drying temperature from 50 to 90°C to obtain the com fiber product. The resulting corn fiber product has content of one or more volatile compounds reduced by at least 1%, at least 5%, at least 10%, at least 25%, at least 50%, at least 75%, at least 90%, at least 95%, or at least 98% as compared to an equivalent untreatedcorn fiber product. Preferably, the resulting com fiber product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated corn fiber product; in other words, the resulting corn fiber product can be completely free of one or more volatile compounds.

[0042] The corn fiber containing material may include, but may not be limited to, fibers recovered from dry mill process or wet mill process.

[0043] During the humidifying step, the corn fiber containing material is humidified at a relative humidity in a range from 50 to 100%, from 60 to 99%, or from 70 to 99%, and at a humidifying temperature in a range from 55 to 95°C, from 60 to 95°C, or from 70 to 95°C. The corn fiber containing material is humidified for a humidifying period in a range from 10 to 90 minutes, from 15 to 75 minutes, or from 30 to 60 minutes.

[0044] The humidified material is dried at a drying temperature in a range from 50 to 90°C, from 60 to 90°C, or from 70 to 90°C, for a drying period in a range from 5 to 25 minutes, from 8 to 20 minutes, or from 10 to 15 minutes to obtain the corn fiber product.

[0045] In one aspect, each of the humidifying step and the drying step can be performed for one or more than one time, preferably for at least two times, more preferably for two times. Preferably, the humidifying step and the drying step can be carried out as a cycle and the cycle can be performed for one or more than one time, preferably for at least two times, more preferably for two times.

[0046] In one aspect, no purification step may be required to separate starch out from the corn fiber containing material before the material is fed to the process. In another aspect, no enzymatic step may be required in any process of the instant invention described in the present disclosure.

[0047] In another aspect, no alcohol washing step may be required in any process of the instant invention described in the present disclosure.Corn fiber product

[0048] The com fiber product of the present invention has content of one or more volatile compounds reduced as compared to an equivalent untreated com fiber product. Thus, the corn fiber product may have one or more off-notes partially or completely removed. In other words, the content of one or more volatile compounds in the corn fiber product described in this disclosure is reduced, preferably completely eliminated, as compared to an equivalent untreated corn fiber product. Volatile compounds are substances present in a corn fiber product that may impart a flavor (e.g., an earthy flavor, a savory flavor, a meaty flavor, a brothy flavor, a grainy flavor, a cereal flavor, a malty flavor, a toasted flavor, a beany flavor, a green flavor, or any combinations thereof) to the product. Examples of the volatile compounds may include, but may not be limitedto, furan, pyran, organic acid, aldehyde, alcohol, ketone, pyrazine, lactone, thiol, sulfide, or any combinations thereof.

[0049] Preferably, the volatile compounds may include, but may not be limited to, hexanal, heptanal, benzaldehyde, 2-heptenal, 2-pentyl-furan, 2-ethyl-6-methyl-pyrazine, l-octen-3-ol, 4- m ethyl- 1 -pentanol, 2-ethyl-l -hexanol, 4-ethyl-benzaledhyde, octanal, 2-hexanol, or any combinations thereof.

[0050] In one aspect, the com fiber product of the present invention has content of one or more volatile compounds reduced by at least 1%, at least 5%, at least 10%, at least 25%, at least 50%, at least 75%, at least 90%, at least 95%, or at least 98% as compared to an equivalent untreated corn fiber product. Preferably, the corn fiber product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated corn fiber product.

[0051] Preferably, the corn fiber product of the present invention may be prepared by any process described in the present disclosure.

[0052] In one aspect, attributes other than the volatile compound content of the com fiber product prepared by any process of the instant invention described in the present disclosure may be improved as compared to an equivalent untreated corn fiber product.Examples

[0053] The invention is further described in detail by reference to the following experimental examples. These examples are provided for purposes of illustration only and are not intended to be limiting unless otherwise specified. Thus, the invention should in no way be constmed as being limited to the following examples, but rather should be constmed to encompass any and all variations which become evident as a result of the teaching provided herein.Example 11.1. Materials and Method

[0054] Approximately 5g samples of a wet mill corn fiber (Cargill Incorporated) was weighed and placed in shallow aluminum weigh boats. Then, the samples were treated by a humidifying step and a drying step. Boats were placed in an Unox combi oven set for the humidification treatment conditions described in Table 1. Six samples were prepared for each humidification treatment condition (“treatment condition”). At the end of the humidification phase, three samples were removed, exactly weighed, transferred to vials and frozen. The remaining three samples were heated in the oven for 12 minutes at 70°C and 0% relative humidity to remove water. After the drying step, the treated samples were exactly weighed, placed in vials and frozen until analysis.

[0055] Initial moisture content was estimated using quadruplicate measurements with a moisture balance.Table 1

[0056] For sensory analysis, single samples of about 40g wet mill com fiber were placed in larger aluminum pans and exposed to the same treatment conditions described in Table 1. At the end of the humidification phase, samples were transferred to mylar bags and frozen without any drying treatment.

[0057] A reference curve was created by suspending untreated material at a ratio of 5g material with 95g water and allowing the suspension to steep at room temperature for about 10 minutes. The solution was centrifuged and the supernatant was pulled through a 0.2-micron polyethersulfone (PES) membrane in a sterile vessel. Similar solutions were also prepared at concentrations of 0.1, 0.5, 1.0, 2.0, and 3.0%. These samples were tasted blindly and independently by a trained panel (6 people) who were asked to place the reference standards on a line scale. The panel did not specifically know what the standards represented. The panel leader then reviewed the data of the composite samples for panel agreement of sample intensity rank order and the software assigned numerical values of 0 to 100. Panelists that were deemed outliers were removed and an average of their numerical values was taken for the remaining panelists. Those average values became the scale values of 0 to 100 for the reference standards and were anchored on the line accordingly for the remainder of the tests.

[0058] The panel was then given three blind untreated samples (concentrations of 0.5%, 2.5%, and 4%) as a validation testing to ensure the panel was aligned and could reproduce their data. The panelists were asked to place these samples on the line scale where the standards had alreadybeen placed by the panel leader based on the panelists’ averages. If the panel showed agreement and alignment with the established standards, the testing progressed. They were then presented with the treated and untreated materials at 3.0% concentration and asked to place each of the samples on the line scale using the standards which were already anchored on the line based on the initial values from the establishment testing. This resulted in an intensity measurement that is an overall flavor intensity value. The response curve (Figure 1) can be used to compute an equivalent concentration (by rearrangement of the regression equation) that reflects the degree of dilution of the untreated material required to match intensity. Because of the non-linear response of intensity to concentration, the apparent concentration may decrease disproportionately compared to the direct intensity.1.2. Results and Discussion1.2.1 Moisture Gain

[0059] The moisture after the humidification was a function of the humidifying temperature, relative humidity (RH), and humidification period (overall analysis of variance using backward elimination in a 2-factor interaction analysis, p<0.0001). The maximum moisture observed was about 12% and the minimum was about 1%. In high temperatures and dry conditions, the samples lost weight.Table 2

[0060] As observed in in Table 2, which shows the mean moisture (%) before and after humidifying, there was a significant difference in moisture after the humidifying step. The moisture before and after drying had a correlation coefficient of 0.93. Subsequent analyses were adjusted to a moisture-free basis using the observed moistures for individual samples.1.2,2 Sensory Analysis

[0061] The panel successfully placed blind references at the appropriate flavor intensity relative to the established scale. Table 3 below shows the relationship between treatment conditions, perceived flavor intensity, and equivalent concentration of treated solutions of corn fiber. Some treatments had a significant effect on the overall flavor intensity values (in a scale of 0 to 100 - with 0 being the least intense and 100 being the most intense) measured by the sensory panel. For example, treatment conditions 2 and 8 had lower intensities. Samples in Table 3 designated with “n / a” had higher flavor intensity than the untreated sample.Table 31.2,3 Untargeted GC / MS Analysis

[0062] General effects of treatments on volatile compounds in the samples can be detected using untargeted GC / MS methods. For example, general changes to the population of volatilecompounds can be detected by the untargeted GC / MS methods. Such volatile compounds may be responsible for carrying flavors (e.g., off-note flavors). This approach is based on the fingerprinting of volatiles on gas chromatography (GC) and hi-resolution mass spectrometric (MS) identification. The overall purpose is to look at the volatile composition of the various samples and compare the different experimental treatments to look for differences and patterns.

[0063] Though untargeted GC / MS does not provide exact quantitative data, it does provide relative comparative potential. Every compound identified has an associated area count, which is the mass abundance of the fragment ions from the compounds, which can be a relative proxy for concentration. Since different compounds have different sensitivities, one compound cannot be compared to another, but one compound can be compared to itself provided a similar mass fragmentation process was conducted across the samples. Even in this case, the responsiveness may not be perfectly linear, but it is approximately linear.

[0064] Principal Component Analysis (PCA) was performed on both pre-drying and post-drying samples in order to investigate the impact of treatment conditions on the concentration of unidentified compounds. The results showed that the high temperature and high humidity treatment caused the samples to be distinctly different from the other treatment conditions, leading to a different fingerprint of volatile compounds. Further analysis revealed that a larger number of volatiles that were decreased in relative concentration caused the high temperature and high humidity samples to cluster differently.

[0065] Figure 2 shows the effect of humidification alone on the profile of volatile compounds, in which compounds that showed less than 2-fold change were excluded from the visualization. Generally, many more compounds are decreased in concentration than increased. Increased concentrations are more likely to arise from compounds that are in low concentration in the untreated sample. As observed, treatment conditions 5 and 10 seem to affect more compounds than treatment conditions 1 and 7.

[0066] Figure 3 shows the comparable information for those samples that were humidified and then dried.

[0067] One further way to understand the effect of treatment is to count the number of volatile compounds that show two-fold concentration decreases (down) or increases (up). Table 4 shows how most treatment conditions before drying favor decreasing concentrations over increasing concentrations but drying makes this effect essentially universal. Drying caused many additional volatile compounds to decrease in concentration.Table 41.2.4 Targeted GC / FID Analysis

[0068] Treated and untreated samples collected before and after drying were analyzed for about 30 analytes using a calibrated GC / FID method. Not all compounds in the calibration set appear in the samples.

[0069] A study on the distribution of calibrated compounds in the untreated samples shows that about 93% of the mass of these compounds are associated with hexanal, thiophene, 2-pentyl furan, and benzaldehyde. The overall flavor intensity observed in Table 3 may correlate to one or more of the above compounds. Some of the flavor intensity may arise from compounds that are not part of the standard set. In any event, it may be important to understand that overall flavor intensity may be dominated by a subset of the compounds present and analyzed and include influences from compounds that were present but not analyzed.

[0070] Modeling of the effect of treatment conditions resulted in significant relationships for many of the compounds detected. The effect of drying overcame the effect of conditions in a few cases, but overall, the effect of conditions during humidification appears to dominate the change in concentration. Humidifying temperature and relative humidity may be the dominant factors in which both parameters contribute to the main and interaction effects.

[0071] A study on the response of the concentrations of volatile compounds to humidifying temperature and relative humidity shows that the concentrations of most compounds are decreased by at least 20% after humidification. Drying clearly had a benefit for decreasing volatilecompounds such as benzaldehyde, l-octen-3-ol, and 2-octanone. Except for o-tolualdehyde, high humidity tends to decrease concentrations of volatile compounds.

[0072] Table 5 summarizes the effect of different humidification conditions on the percent of quantified compounds changed significantly in concentration. Drying clearly had a dramatic effect on the measured volatile compound concentrations. More compounds were decreased in more conditions and the number of compounds that increased in concentration were decreased.Table 51.2,5 Conclusion

[0073] The following observations can be drawn from the above studies:

[0074] - Exposure of corn fiber to high humidifying temperature and relative humidity can significantly decrease the overall flavor intensity.

[0075] - The decline in flavor intensity was not easily related to a change in any single volatile compound but a combination of volatile compounds.

[0076] - A large number of volatile compounds decreased in concentration as indicated by untargeted GC / MS. A smaller number of compounds increased in concentration.

[0077] - The concentration of most quantitated compounds (from GC / FID analysis using quantitative standards) was negatively correlated with the amount of moisture adsorbed during the humidification.

[0078] - Most compounds tracked in quantitative analysis showed sensitivity to conditions during humidification. Generally, high humidity favored decreased concentrations, before and after drying.

[0079] - Drying had a significant effect on the concentration of numerous volatile compounds. Compounds that were not decreased in concentration after humidification alone, could be decreased in the subsequent drying step. Expressed another way, drying effects were the strongest when the humidification effect was the weakest.Example 22.1 Materials and Method

[0080] About 5g samples of the fine com fiber (Cargill Incorporated) was weighed into a preweighed aluminum weighing dish. Triplicate samples were placed in a Combi-oven for 60 minutes at 40°C or 90°C and 100% relative humidity (humidified samples). A matching set of samples was prepared (reference samples), and both the humidified samples and reference samples were placed in the Combi-oven for 20 minutes at 80°C and 0% relative humidity to obtain treated samples and dried-only samples, respectively. One untreated sample, three treated samples, and three dried-only samples were placed in gas-tight vials and stored in the dark at room temperature until analysis.2.2 Results and Discussion

[0081] Humidification treatment at 90°C and 100% relative humidity was associated with a 2-fold decrease in almost half of the compounds detected by the untargeted GC / MS method. In contrast, drying alone removed about one-third of the detected compounds. Table 6 below shows the number of compounds that were increased or decreased at least 2-fold in concentration by humidification and drying or drying alone (with a<0.05). Column “Total” refers to the total number of compounds detected in the untreated samples. H&D indicates humidified and dried treatment (i.e., treated samples). OD indicates dried only treatment (i.e., dried-only samples).Table 6Example 33.1 Materials and Method

[0082] About 5g samples of corn bran (Cargill Incorporated) were weighed and placed in shallow aluminum weigh boats. Then, the samples were treated by a humidifying step and a drying step. Boats were placed in an Cheftop combi oven set for the humidification conditions described inTable 7. The samples were heated in the oven for 12 minutes at 70°C and 0% relative humidity to remove water. After the drying step, the treated samples were exactly weighed, placed in vials and frozen until analysis.

[0083] Initial sample moisture was estimated using quadruplicate measurements with a moisture balance.Table 7

[0084] For sensory analysis, single samples of about 40g corn bran were placed in larger aluminum pans and exposed to the same humidification conditions described in Table 7. After humidification, the treated samples were transferred to mylar bags and frozen without any drying.

[0085] A reference curve was created by suspending untreated material at a concentration of 7.0% in water and allowing the suspension to steep at room temperature for about 10 minutes. The suspension was then centrifuged, and the supernatant pulled through a 0.2-micron polyethersulfone (PES) membrane in a sterile vessel. Reference standards of 0.25, 0.5, 0.75, 1.0, 3.0, and 5.0% were prepared by serially diluting the 7.0% stock solution with water. These samples were tasted blindly and independently by a trained panel (12 people) who were asked to place the reference standards on a line scale. The panel did not specifically know what the standards represented. The panel leader then reviewed the data looking for panel agreement on sample intensity rank order and the software assigned numerical values (0-100). The data from panelists that were deemed outliers were removed and an average of the assigned numerical values was taken for the remaining panelists. Those average values then became the scale values (0-100) for the reference standards and were anchored on the line accordingly for the remainder of the tests.

[0086] The panel was then given three sets of samples which included four blind untreated samples and the treated samples. The four blind untreated samples (known to the scientists: 0.75%, 1.5%, 3.0% and 5.0%) were prepared by diluting the 7.0% stock solution with water and were used to ensure the panel was aligned and could reproduce their data. The treated samples were prepared at 5.0% concentration. After tasting a sample, the panelists were asked to place thesample on the scale based on intensity, using the scale anchors they established in the previous step. With each set of samples, the panel leader used the blind samples to ensure that the panel showed agreement and alignment with the established standards before progressing to the next set of samples. The placement on the line scale provided an output of an intensity measurement that was an overall specific intensity value, which reflects that the panel is assessing the intensity level of the treated samples compared to the intensity of the reference anchors created from the same untreated material.3.2 Results and Discussion3,2, 1 Sensory analysis

[0087] The panel successfully placed blind references at the appropriate flavor intensity relative to the established scale. Table 8 below shows the relationship between treatment conditions, perceived flavor intensity, and equivalent concentration of treated solutions of com bran. Some treatments showed a reduction of the overall flavor intensity values (in scale of 0 to 100: with 0 being the least intense and 100 being the most intense) measured by the sensory panel. For example, treatment conditions 4 and 5 achieved a decrease in flavor intensity equivalent about 35% decrease in the overall flavor intensity.Table 83,2,2 Untargeted GC / MS analysis

[0088] General effects of treatments on volatile compounds can be detected using untargeted GC / MS methods. For example, general changes to the population of volatile compounds can be detected by the untargeted GC / MS methods. Such volatile compounds may be responsible for carrying flavors (e.g., off-note flavors). This approach is based on the fingerprinting of volatilecompounds via gas chromatography (GC) and mass spectrometric (MS) identification. The overall purpose is to look at the volatile composition of the various samples and compare the different experimental treatments to look for differences and patterns.

[0089] Though untargeted GC / MS does not provide exact quantitative data, it does provide relative comparative potential. Every compound identified has an associated area count, which is the mass abundance of the fragment ions from the compounds, which can be a relative proxy for concentration. Since different compounds have different sensitivities, one compound cannot be compared to another, but one compound can be compared to itself provided a similar mass fragmentation process was conducted across the samples. Even in this case, the responsiveness may not be perfectly linear, but it is approximately linear.

[0090] Principal Component Analysis (PCA) was performed on both pre-drying and post-drying samples in order to investigate the impact of treatment conditions on the concentration of unidentified compounds. The results showed that the high temperature and high humidity treatment caused the samples to be distinctly different from the other treatment conditions, leading to a different fingerprint of volatile compounds. Further analysis revealed that a larger number of volatiles that were decreased in relative concentration caused the high temperature and high humidity samples to cluster differently.

[0091] Figure 4 shows the effect of treatment on the profile of volatile compounds, in which compounds that showed less than 2-fold change were excluded from the visualization. A total of about 468 compounds were identified in the samples. Generally, many more compounds were decreased in concentration than increased. Increased concentrations were more likely to arise from compounds that were in low concentration in the untreated sample.

[0092] One further way to understand the effect of treatment is to count the number of volatile compounds that show two-fold concentration decreases (down) or increases (up). Table 9 shows how most treatment conditions favor decreasing concentrations over increasing concentrations, and how high relative humidity treatment favor the concentration decrease the most.Table 93,2.3 Targeted GC / FID analysis

[0093] Samples of treated and untreated samples were analyzed for about 25 analytes using a calibrated GC / FID method. Not all compounds in the calibration set appear in the samples. Table 10 shows the distribution of calibrated compounds in the untreated samples. About 98% of the mass of these compounds are associated with hexanal, 2-ethyl-l -hexanol, 2-ethyl-6-methyl- pyrazine, 4-methyl-l -pentanol, l-octen-3-ol, 2-pentyl-furan, 1 -pentanol, heptanal, benzaldehyde, 4-ethyl-benzaldehyde, and 2-heptenal. Because different compounds have quite different flavor and aroma potencies, this does not mean that the sensory experience depends on just these compounds. An integrated flavor perception might be more dependent on the combination and concentrations of compounds than concentration of any single compound. In any event, it may be important to understand that overall chemical response may be dominated by a subset of the compounds present and analyzed.Table 10

[0094] The treatment process drastically reduces volatile compounds and can change the overall composition of these individual volatile compounds. Table 11 shows the com bran volatile composition (of tracked compounds) after humidifying at 90°C at 100% RH for 60 minutes. The dominance of hexanal in the composition has diminished and other minor compounds are more resistant to removal and have increased comparatively, such as benzaldehyde and octanal.Table 11

[0095] Tables 12 and 13 show the percentage reduction of major volatile compounds after treatment as compared to the untreated samples. For the treatment producing Table 11, hexanal was removed at 71.4%, while benzaldehyde and l-octen-3-ol were more resistant to removal at 16.4% and 0.4%, respectively.

[0096] The “All Peaks” column refers to the sum of all detected volatile species in the sample, both calibrated and uncalibrated. This is indicative of the total volatile composition change, regardless of individual compounds decreasing or increasing at a given processing condition.Table 12Table 13

[0097] Table 14 shows the simple correlation coefficients between the humidifying temperature, relative humidity (RH), and humidifying period and the observed concentrations of compounds after the treatment. “All peaks” is a sum of all peaks detected, both calibrated and not, including the entire volatile composition of the sample. Correlations show that relative humidity has the largest impact on reduction in volatile species. Humidifying temperature has a negative correlation for most compounds, showing that lower humidifying temperature results in higher reductions.Table 143,2,4 Conclusion

[0098] The following observations can be drawn from the above studies:

[0099] - Relative humidity was positively correlated to most volatile compound reduction, showing higher relative humidity resulted in greater reduction of volatile compounds.

[0100] - Humidifying temperature was negatively correlated to most volatile compound reduction, showing lower humidifying temperature resulted in greater reduction of volatile compounds.

[0101] - Treatment condition of high humidifying temperature and low relative humidity (90°C / 60RH) had the lowest volatile compound reduction as seen in the GC / FID and GC / MS analyses.Clauses describing the invention

[0102] Clause 1. A process for preparing a com fiber product, comprising the steps of: a. providing a corn fiber containing material; b. humidifying the corn fiber containing material at a relative humidity and a humidifying temperature of less than 100°C to obtain a humidified material; and c. drying the humidified material to obtain the corn fiber product; wherein the corn fiber product has a reduced volatile compound content as compared to an equivalent untreated corn fiber product.

[0103] Clause 2. The process of any of the preceding clauses, wherein the relative humidity in the humidifying step is in a range from 50 to 100%.

[0104] Clause 3. The process of any of the preceding clauses, wherein the humidifying temperature is in a range from 55 to 95°C.

[0105] Clause 4. The process of any of the preceding clauses, wherein the humidifying temperature is less than 100°C.

[0106] Clause 5. The process of any of the preceding clauses, wherein the com fiber containing material is humidified for a humidifying period in a range from 10 to 90 minutes, from 15 to 75 minutes, or 30 to 60 minutes.

[0107] Clause 6. The process of any of the preceding clauses, wherein in the humidifying step, the relative humidity is in a range from 60 to 100%, the humidifying temperature is in a range from 60 to 90°C; and the humidifying period is in a range from 30 to 90 minutes.

[0108] Clause 7. The process of any of the preceding clauses, wherein water is uniformly delivered and distributed over the com fiber containing material in the humidifying step.

[0109] Clause 8. The process of any of the preceding clauses, water delivered in the humidifying step is in a form of a liquid water or a vapor.

[0110] Clause 9. The process of any of the preceding clauses, water delivered in the humidifying step is not in a form of steam.[OHl] Clause 10. The process of any of the preceding clauses, wherein the humidified material is dried at drying temperature in a range from 50 to 90°C.

[0112] Clause 11. The process of any of the preceding clauses, wherein the humidified material is dried for a drying period in a range from 5 to 25 minutes, from 8 to 20 minutes, or from 10 to 15 minutes.

[0113] Clause 12. The process of any of the preceding clauses, wherein each of the humidifying step and the drying step is performed for one or more than one time, preferably for at least two times, more preferably for two times.

[0114] Clause 13. A process for reducing volatile compound content of a com fiber product, comprising the steps of: a. humidifying a corn fiber containing material at a relative humidity from 50 to 100% and a humidifying temperature of less than 100°C to obtain a humidified material; and b. drying the humidified material at a drying temperature from 50 to 90°C to obtain the corn fiber product; wherein the corn fiber product has a reduced volatile compound content as compared to an equivalent untreated corn fiber product.

[0115] Clause 14. A process for reducing volatile compound content of a com fiber product, consisting of the steps of: a. humidifying a corn fiber containing material at a relative humidity from 50 to 100% and a humidifying temperature of less than 100°C to obtain a humidified material; and b. drying the humidified material at a drying temperature from 50 to 90°C to obtain the corn fiber product; wherein the corn fiber product has a reduced volatile compound content as compared to an equivalent untreated corn fiber product.

[0116] Clause 15. The process of any of clauses 13 to 14, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.

[0117] Clause 16. The process of any of the clauses 13 to 15, wherein the corn fiber containing material is humidified for a humidifying period in a range from 10 to 90 minutes, from 15 to 75 minutes, or 30 to 60 minutes.

[0118] Clause 17. The process of any of the clauses 13 to 16, wherein in the humidifying step, the relative humidity is in a range from 60 to 100%, the humidifying temperature is in a range from 60 to 90°C; and the humidifying period is in a range from 30 to 90 minutes.

[0119] Clause 18. The process of any of clauses 13 to 17, wherein water is uniformly delivered and distributed over the corn fiber containing material in the humidifying step.

[0120] Clause 19. The process of any of clauses 13 to 18, water delivered in the humidifying step is in a form of a liquid water or a vapor.

[0121] Clause 20. The process of any of clauses 13 to 19, water delivered in the humidifying step is not in a form of steam.

[0122] Clause 21. The process of any of clauses 13 to 20, wherein the humidified material is dried at a drying temperature in a range from 50 to 90°C.

[0123] Clause 22. The process of any of clauses 13 to 21, wherein the humidified material is dried for a drying period in a range from 5 to 25 minutes, from 8 to 20 minutes, or from 10 to 15 minutes.

[0124] Clause 23. The process of any of clauses 13 to 22, wherein each of the humidifying step and the drying step is performed for one or more than one time, preferably for at least two times, more preferably for two times.

[0125] Clause 24. The process of any of the preceding clauses, wherein the corn fiber product has content of one or more volatile compounds reduced by a range from 20 to 100%, preferably from 55 to 100%, more preferably from 70 to 100%, as compared to an equivalent untreated com fiber product.

[0126] Clause 25. The process of any of the preceding clauses, wherein the com fiber product does not comprise or consist of corn bran.

[0127] Clause 26. The process of any of the preceding clauses, wherein the humidifying step does not comprise or consist of a condition of the humidifying temperature being at 90°C and the relative humidity being at 60%.

[0128] Clause 27. A corn fiber product prepared by the process of any of the preceding clauses.

[0129] Clause 28. A com fiber product having content of one or more volatile compounds reduced as compared to an equivalent untreated com fiber product.

[0130] Clause 29. The corn fiber product of any of clauses 27 to 28, having content of one or more volatile compounds reduced by a range from 10 to 100%, preferably from 55 to 100%, more preferably from 70 to 100%, as compared to an equivalent untreated com fiber product.

[0131] Clause 30. The com fiber product of any of clauses 27 to 29, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, furan, pyrazine, and alcohol.

[0132] Clause 31. The com fiber product of any of clauses 27 to 30, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, benzaldehyde, 2- heptenal, 2-pentyl-furan, 2-ethyl-6-methyl-pyrazine, l-octen-3-ol, 4-methyl-l -pentanol, 2-ethyl- 1 -hexanol, 4-ethyl-benzaledhyde, octanal, 2-hexanol, and any combinations thereof.

[0133] Clause 32. The com fiber product of any of clauses 27 to 31, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, benzaldehyde, 2- heptenal, 2-pentyl-furan, 2-ethyl-6-methyl-pyrazine, l-octen-3-ol, 4-methyl-l -pentanol, and any combinations thereof.

[0134] Clause 33. The corn fiber product of any of clauses 27 to 32, having content of hexanal reduced by a range from 30 to 80%, preferably from 60 to 80%, more preferably from 70 to 80%, as compared to an equivalent untreated com fiber product.

[0135] Clause 34. The corn fiber product of any of clauses 27 to 33, having content of hexanal reduced by at least 30%, preferably at least 60%, or more preferably at least 65%, as compared to an equivalent untreated corn fiber product.

[0136] Clause 35. The corn fiber product of any of clauses 27 to 34, having content of heptanal reduced by a range from 15 to 70%, preferably from 50 to 70%, more preferably from 55 to 70%, as compared to an equivalent untreated com fiber product.

[0137] Clause 36. The corn fiber product of any of clauses 27 to 35, having content of heptanal reduced by at least 15%, preferably at least 50%, or more preferably at least 55%, as compared to an equivalent untreated corn fiber product.

[0138] Clause 37. The corn fiber product of any of clauses 27 to 36, having content of benzaldehyde reduced by a range from 10 to 80%, preferably from 60 to 80%, more preferably from 65 to 80%, as compared to an equivalent untreated com fiber product.

[0139] Clause 38. The corn fiber product of any of clauses 27 to 37, having content of benzaldehyde reduced by at least 10%, preferably at least 60%, or more preferably at least 65%, as compared to an equivalent untreated com fiber product.

[0140] Clause 39. The corn fiber product of any of clauses 27 to 38, having content of 2-heptenal reduced by a range from 15 to 50%, preferably from 20 to 50%, more preferably from 25 to 50%, as compared to an equivalent untreated com fiber product.

[0141] Clause 40. The corn fiber product of any of clauses 27 to 39, having content of 2-heptenal reduced by at least 15%, preferably at least 20%, or more preferably at least 25%, as compared to an equivalent untreated corn fiber product.

[0142] Clause 41. The com fiber product of any of clauses 27 to 40, having content of 2-pentyl- furan reduced by a range from 60 to 95%, preferably from 70 to 95%, more preferably from 80 to 95%, as compared to an equivalent untreated corn fiber product.

[0143] Clause 42. The com fiber product of any of clauses 27 to 41, having content of 2-pentyl- furan reduced by at least 60%, preferably at least 70%, or more preferably at least 80%, as compared to an equivalent untreated corn fiber product.

[0144] Clause 43. The com fiber product of any of clauses 27 to 42, having content of 2-ethyl-6- methyl-pyrazine reduced by a range from 10 to 50%, preferably from 20 to 50%, more preferably from 30 to 50%, as compared to an equivalent untreated com fiber product.

[0145] Clause 44. The com fiber product of any of clauses 27 to 43, having content of 2-ethyl-6- methyl-pyrazine reduced by at least 10%, preferably at least 20%, or more preferably at least 30%, as compared to an equivalent untreated com fiber product.

[0146] Clause 45. The com fiber product of any of clauses 27 to 44, wherein the com fiber product does not comprise or consist of corn bran.

Claims

CLAIMSWhat is claimed is:

1. A process for preparing a com fiber product, comprising the steps of: a. providing a corn fiber containing material; b. humidifying the com fiber containing material at a relative humidity and a humidifying temperature of less than 100°C to obtain a humidified material; and c. drying the humidified material to obtain the corn fiber product; wherein the corn fiber product has a reduced volatile compound content as compared to an equivalent untreated corn fiber product.

2. The process of any of the preceding claims, wherein the relative humidity in the humidifying step is in a range from 50 to 100%.

3. The process of any of the preceding claims, wherein the humidifying temperature is in a range from 55 to 95°C.

4. The process of any of the preceding claims, wherein the com fiber containing material is humidified for a humidifying period in a range from 10 to 90 minutes, from 15 to 75 minutes, or 30 to 60 minutes.

5. The process of any of the preceding claims, wherein the humidified material is dried at drying temperature in a range from 50 to 90°C.

6. The process of any of the preceding claims, wherein the humidified material is dried for a drying period in a range from 5 to 25 minutes, from 8 to 20 minutes, or from 10 to 15 minutes.

7. The process of any of the preceding claims, wherein each of the humidifying step and the drying step is performed for one or more than one time, preferably for at least two times, more preferably for two times.

8. A process for reducing volatile compound content of a corn fiber product, comprising the steps of: a. humidifying a com fiber containing material at a relative humidity from 50 to 100% and a humidifying temperature of less than 100°C to obtain a humidified material; and b. drying the humidified material at a drying temperature from 50 to 90°C to obtain the corn fiber product; wherein the corn fiber product has a reduced volatile compound content as compared to an equivalent untreated corn fiber product.

9. The process of claim 8, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.

10. The process of any of claims 8 to 9, wherein each of the humidifying step and the drying step is performed for one or more than one time, preferably for at least two times, more preferably for two times.

11. A com fiber product prepared by the process of any of the preceding claims.

12. A com fiber product having content of one or more volatile compounds reduced as compared to an equivalent untreated corn fiber product.

13. The corn fiber product of any of claims 11 to 12, having content of one or more volatile compounds reduced by a range from 10 to 100%, preferably from 55 to 100%, more preferably from 70 to 100%, as compared to an equivalent untreated com fiber product.

14. The corn fiber product of any of claims 11 to 13, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, furan, pyrazine, and alcohol.

15. The corn fiber product of any of claims 11 to 14, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, benzaldehyde, 2- heptenal, 2-pentyl-furan, 2-ethyl-6-methyl-pyrazine, l-octen-3-ol, 4-m ethyl- 1 -pentanol, 2- ethyl-1 -hexanol, 4-ethyl-benzaledhyde, octanal, 2-hexanol, and any combinations thereof.

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