Protein product and process of preparing the same
A humidification and drying process effectively reduces volatile compounds in protein ingredients, addressing flavor issues and enhancing their use in food products.
Patent Information
- Application Number
- PCT/US2025/022523
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-04-02
- Filing Date
- 2025-04-01
- Publication Date
- 2025-10-09
AI Technical Summary
Many plant and non-plant protein ingredients have undesirable flavor characteristics due to volatile organic compounds, limiting their application in food products, despite prior processing methods that fail to effectively remove these compounds.
A process involving humidification at controlled humidity and temperature followed by drying is used to reduce volatile compound content in protein products, resulting in a product with reduced flavor intensity.
The process significantly decreases volatile compound content by up to 100%, improving the flavor profile and suitability of protein products for food applications.
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Figure US2025022523_09102025_PF_FP_ABST
Abstract
Description
PROTEIN PRODUCT AND PROCESS OF PREPARING THE SAMECROSS REFERENCE
[0001] This application claims the benefit of United States Provisional Application No. 63 / 572,961, filed April 2, 2024, which is hereby incorporated by reference in its entirety.FIELD OF INVENTION
[0002] This invention relates to the field of protein products.BACKGROUND
[0003] Many ingredients refined from plants, such as plant proteins and plant fibers, as well as non-plant ingredients (e.g., dairy proteins), have undesirable flavor characteristics due to the volatile and relatively low molecular weight organic compounds bound to the surfaces. The perceived “off-flavor” often limits the application of such ingredients in making food products like meat substitute products, cheese substitutes, ready-to-eat cereals, nutrition bars, conventional processed meats, and confectionary coatings.
[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. 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 protein 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 protein product comprising the steps of providing a protein containing material; humidifying the protein 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 protein product. The resulting protein product has a reduced volatile compounds content as compared to an equivalent untreated protein product.
[0007] The present disclosure also provides a process for reducing volatile compound content of a protein product comprising the steps of humidifying a protein 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 protein product. The resulting protein product has reduced volatile compound content as compared to an equivalent untreated protein product.
[0008] The present disclosure also provides a protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated protein 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 a plot of log2(treated / untreated) against log lO(untreated). Results for 40°C are shown on the left. Results for 90°C are shown on the right. Scales are identical in different plots. Panels show (A) soy flour, (B) soy protein concentrate, (C) textured soy concentrate, (D) soy protein isolate 1, (E) faba bean isolate, (F) corn protein isolate, (G) vital wheat gluten, (H) rice protein concentrate, (I) sunflower protein concentrate, (K) potato protein isolate, (L) milk protein isolate, (M) sodium caseinate, and (N) egg white protein isolate.
[0011] Figure 2 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 whey protein isolate (WPI) 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.
[0012] Figure 3 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 caseinate protein 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.
[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 almond protein 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 protein product and a process of preparing the protein product. The protein 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 protein product
[0021] The present disclosure provides a process for preparing a protein product. The process comprises the steps of humidifying a protein 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 protein product. The resulting protein product has one or more improved attributes as compared to an equivalent untreated protein 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 protein product” refers to an equivalent protein product (e.g., a plant protein product) that has not been subjected to any process of theinstant invention as described in the present disclosure. An “equivalent protein product” refers to a protein product prepared from the same starting material used in the instant invention.
[0023] In one aspect, an “equivalent untreated whey protein product” refers to an equivalent whey protein product that has not been subjected to any process of the instant invention as described in the present disclosure. An “equivalent whey protein product” refers to a whey protein product prepared from the same starting material used in the instant invention.
[0024] In one aspect, an “equivalent untreated caseinate protein product” refers to an equivalent caseinate protein product that has not been subjected to any process of the instant invention as described in the present disclosure. An “equivalent caseinate protein product” refers to a caseinate protein product prepared from the same starting material used in the instant invention.
[0025] In one aspect, an “equivalent untreated almond protein product” refers to an equivalent almond protein product that has not been subjected to any process of the instant invention as described in the present disclosure. An “equivalent almond protein product” refers to an almond protein product prepared from the same starting material used in the instant invention.
[0026] The protein containing material serves as a starting material to the process may be a plant protein containing material or a non-plant protein containing material.
[0027] The plant protein containing material can include a plant protein that may include, but may not be limited to, legume protein (e.g., soy protein, faba protein, pea protein, lentil protein, chickpea protein, bean (Phaseolus) protein, mung bean protein), composite proteins (e.g., sunflower protein), cereal proteins (e.g., wheat protein, corn protein, rice protein), nightshade proteins (e.g., potato protein), cucurbit proteins (e.g., pumpkin protein, watermelon protein), mustard proteins (e.g., canola or rapeseed protein), knotweed proteins (e.g., buckwheat protein), pigweed proteins (e.g., amaranth protein, quinoa protein), duckweed proteins (e.g., lemna protein), nut proteins (e.g., almond protein), or any combinations thereof.
[0028] Preferably, the plant protein material can include a plant protein with different concentrations (e.g., flours, concentrates, isolates, powdered proteins, textured proteins) obtained from different botanical sources that may include, but may not be limited to, legume (e.g., soy, faba, pea), composite (e.g., sunflower), cereal (e.g., wheat, corn, rice), nightshade (e.g., potato), cucurbit (e.g., pumpkin, watermelon), mustard (e.g., canola or rapeseed protein), knotweed (e.g., buckwheat), pigweed (e.g., amaranth, quinoa), duckweed (e.g., lemna), nut (e.g., almond), or any combinations thereof.
[0029] In one aspect, the plant protein containing material can have a protein concentration in a range from 10 to 90 wt% on a dry basis; preferably, the plant protein containing material can have a protein concentration of at least 50 wt% on a dry basis.
[0030] The non-plant protein containing material can include a non-plant protein that may include, but may not be limited to, egg white protein, dairy protein, or any combinations thereof. Dairy protein may include, but may not be limited to, whey protein, caseinate protein, or any combinations thereof.
[0031] In the humidifying step, the protein 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.
[0032] 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.
[0033] Preferably, the atmosphere contacting the protein 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 protein 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 protein containing material itself.
[0034] 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%.
[0035] 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.
[0036] In one aspect, the humidifying step is carried out by passing humidified or warmed air to deliver water to the protein 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 protein containing material; morepreferably, 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.
[0037] The humidifying period for humidifying the protein 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.
[0038] The humidified material can be de-humidified in the drying step to obtain the final protein product. The drying step can be carried out at a drying temperature for a drying period to obtain the protein 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 protein product.
[0039] 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.
[0040] 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.
[0041] The relative humidity at the drying step can be 0%, from 0 to 0.5%, from 0.5% to 1%, or at least 1%.
[0042] 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.
[0043] The protein product obtained from the process as described above may be a plant protein product or a non-plant protein product. Preferably, the protein product has content of one or more volatile compounds reduced as compared to an equivalent untreated protein product. Preferably, the content of one or more volatile compounds in the protein 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 protein product. More preferably, thecontent of one or more volatile compounds in the protein product can be reduced by 100% as compared to an equivalent untreated protein product.
[0044] Preferably, the content of one or more volatile compounds in the protein product can be reduced by a range from 20 to 100%, more preferably from 55 to 100%, or even more preferably from 70 to 100%, as compared to an equivalent untreated protein product.
[0045] The plant protein product may include, but may not be limited to, a legume protein product, a composite protein product, a cereal protein product, a nightshade protein product, a cucurbit protein product, a mustard protein product, a knotweed protein product, a pigweed protein product, a duckweed protein product, a nut protein product, or any combinations thereof.
[0046] The non-plant protein product may include, but may not be limited to, egg white protein product, dairy protein product, or any combinations thereof.Process for reducing volatile compound content of a protein product
[0047] The present disclosure provides a process for reducing volatile compound content of a protein product. Preferably, off-notes of the protein product are reduced by the process of the instant invention.
[0048] 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.
[0049] The process comprises a step of humidifying a protein 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 protein product. The resulting protein 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 untreated protein product. Preferably, the resulting protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated protein product; in other words, the resulting protein product can be completely free of one or more volatile compounds.
[0050] Preferably, the protein product has content of one or more volatile compounds reduced by a range from 20 to 100%, more preferably from 55 to 100%, or even more preferably from 70 to 100%, as compared to an equivalent untreated protein product.
[0051] The protein product may be a plant protein product or a non-plant protein product.
[0052] The protein containing material serves as a starting material may be a plant protein containing material or a non-plant protein containing material.
[0053] The plant protein product may include, but may not be limited to, a legume protein product, a composite protein product, a cereal protein product, a nightshade protein product, a cucurbit protein product, a mustard protein product, a knotweed protein product, a pigweed protein product, a duckweed protein product, a nut protein product, or any combinations thereof.
[0054] The non-plant protein product may include, but may not be limited to, an egg white protein product, a dairy protein product, or any combinations thereof.
[0055] The plant protein containing material can include a plant protein that may include, but may not be limited to, legume protein (e.g., soy protein, faba protein, pea protein, lentil protein, chickpea protein, bean (Phaseolus) protein, mung bean protein), composite proteins (e.g., sunflower protein), cereal proteins (e.g., wheat protein, corn protein, rice protein), nightshade proteins (e.g., potato protein), cucurbit proteins (e.g., pumpkin protein, watermelon protein), mustard proteins (e.g., canola or rapeseed protein), knotweed proteins (e.g., buckwheat protein), pigweed proteins (e.g., amaranth protein, quinoa protein), duckweed proteins (e.g., lemna protein), nut proteins (e.g., almond protein), or any combinations thereof.
[0056] In one aspect, the plant protein containing material can have a protein concentration in a range from 10 to 90 wt% on a dry basis; preferably, the plant protein containing material can have a protein concentration of at least 50 wt% on a dry basis.
[0057] The non-plant protein containing material can include a non-plant protein that may include, but may not be limited to, egg white protein, dairy protein, or any combinations thereof. Dairy protein may include, but may not be limited to, whey protein, caseinate protein, or any combinations thereof.
[0058] During the humidifying step, the protein 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 protein 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.
[0059] 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 protein product.
[0060] 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 beperformed for one or more than one time, preferably for at least two times, more preferably for two times.
[0061] In one aspect, no purification step may be required to separate fibers and starch out from the protein 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.
[0062] In one aspect, no alkaline treatment step may be required in any process of the instant invention described in the present disclosure. In another aspect, no alcohol washing step may be required in any process of the instant invention described in the present disclosure.Protein product
[0063] The protein product of the present invention has content of one or more volatile compounds reduced as compared to an equivalent untreated protein product. Thus, the protein 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 protein product described in this disclosure is reduced, preferably completely eliminated, as compared to an equivalent untreated protein product. Volatile compounds are substances present in a protein 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 limited to, furan, pyran, organic acid, aldehyde, alcohol, ketone, pyrazine, lactone, thiol, sulfide, or any combinations thereof.
[0064] In one aspect, the protein 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 protein product. Preferably, the protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated protein product.
[0065] Preferably, the content of one or more volatile compounds in the protein product can be reduced by a range from 20 to 100%, more preferably from 55 to 100%, or even more preferably from 70 to 100%, as compared to an equivalent untreated protein product.
[0066] The protein product may be a plant protein product or a non-plant protein product.
[0067] The plant protein product may include, but may not be limited to, a legume protein product, a composite protein product, a cereal protein product, a nightshade protein product, a cucurbit protein product, a mustard protein product, a knotweed protein product, a pigweed protein product, a duckweed protein product, a nut protein product, or any combinations thereof.
[0068] The non-plant protein product may include, but may not be limited to, egg white protein product, dairy protein product, or any combinations thereof.
[0069] Preferably, the protein product of the present invention may be prepared by any process described in the present disclosure.
[0070] In one aspect, attributes other than the volatile compound content of the protein product prepared by any process of the instant invention described in the present disclosure may be improved as compared to an equivalent untreated protein product.Examples
[0071] 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 construed as being limited to the following examples, but rather should be construed to encompass any and all variations which become evident as a result of the teaching provided herein.Example 11.1. Materials and Method
[0072] Materials being treated by a humidifying step and a drying step in this study are summarized in Table 1.Table 1
[0073] About 5g of material was weighed into a pre-weighed 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.1.2. Results and Discussion1.2.1 Humidification
[0074] Samples gained from about 7% to about 13% moisture in the humidification phase (Table 2). Samples gained about 9.3% at 40°C and about 8.6% at 90°C; this was significantly different (a=0.008) and presumably due to less condensation of moisture at higher temperature in samples that absorbed less moisture.Table 21.2.2 Untargeted GC / MS Analysis
[0075] 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 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 volatile compounds 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.
[0076] Not all these volatile compounds influence flavor. The flavor experience may be the consequence of concentrations and ratios of volatile compounds that individually would not seem to be relevant or prominent but together produce a flavor experience.
[0077] 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.
[0078] A simple way of comparing treatments is to count the number of volatile compounds that show a greater than 2-fold concentration change as a result of the treatments. Tables 3 and 4 show that dozens to hundreds of compounds can change in concentration by at least 2-fold (up or down) and show a significant difference (alpha<0.05) from the untreated sample.Table 3*H&D indicates humidified and dried treatment (i.e., treated samples)**0D indicates dried only treatment (i.e., dried-only samples)Table 4*H&D indicates humidified and dried treatment (i.e., treated samples)**0D indicates dried only treatment (i.e., dried-only samples)
[0079] A plot of the change in concentration versus the initial concentration illustrates the relationship between the direction and extent of change and the initial concentration (Figures 1 A to IN). Data was included in the Figures 1 A to IN if there was a significant difference between the treatment and the untreated samples - irrespective of the size of the difference. There were numerous instances in which statistically significant change occurred (meaning the change had low variance) even though the relative difference between treatments was small.
[0080] Different materials showed quite different patterns of change. Faba bean and both soy protein isolate (SPI) samples illustrated a common pattern of increases in initially low concentration compounds and decreases in the most concentrated. Each of Figures 1A to IN has a fixed vertical scale to show the difference in magnitude of response of different materials.
[0081] The full range of change was set to show all results in terms of doubling. Com protein isolate illustrated this full range with at least one compound increasing about 1,000-fold and another decreasing about 99.9%. An observation of -2 on this scale represents about 75% decrease, so many of these “small” changes were actually large. Generally, deeper decreases were observed in the humidified and dried cases compared to the dried-only cases. Again generally, the greatest increases were associated with compounds with low initial concentrations while the greatest decreases were observed in the compounds initially at moderate to high concentration.
[0082] The overall approach to data analysis used here allows a comparison of the direction of movement of individual compounds in the two treatment conditions. Table 5 shows the percent of compounds that were decreased in both treatments or increased in both treatments (with a<0.05). The “Total” data reflected the entire set of compounds selected for analysis. The data was sorted by the peak area of the compounds in the untreated sample - the bottom 10% by area was excluded (the subsequent results are reflected as “Top90”).
[0083] Generally, when treated at 40°C, a small number of compounds were increased by both drying-only or humidification and drying. Faba bean isolate was relatively unique in showing a strong decrease from both conditions at 40°C. In contrast, at 90°C, there were few instances of both treatments causing concentration increases, but there were numerous examples of decreases from both treatments. However, this was still a small subset of compounds decreased by humidification and drying at 90°C (as compared with Tables 3 and 4).Table 51.2.3 Conclusion
[0084] The following observations can be drawn from the above studies:
[0085] - Some materials were more sensitive to the effect of humidification than others. This was most evident at lower temperature. Almost all the ingredients treated in these experiments showed a dramatic decrease in the concentration of many compounds when treated at 90°C.
[0086] - The responses to high humidity and 90°C conditions were observed in a diverse set of materials including protein flours, protein concentrates, protein isolates, powdered proteins, and textured proteins. Materials had their origins in cereals, legumes, composites, and nightshades, chicken eggs, and bovine milk. It was likely that the effect of high humidity treatment at elevated temperature is general across solid materials.Example 22.1 Materials and Method
[0087] A sample of corn protein isolate (Cargill Incorporated) was placed into a 2-liter fluted flask and mounted on a rotary evaporator. The liquid refill inlet tube of the rotary evaporator was attached to a neoprene hose that was in turn attached to a bubbler. Nitrogen gas was fed throughthe bubbler and subsequently into the flask. Vapor exited through the condenser, which was left open to the air. The condenser was set to -10°C. The bubbler was placed in a hot water bath which was maintained between 70 and 80°C. The rate of nitrogen flow was vigorous, but unmeasured.
[0088] The rotation rate of the flask was 28 rpm, which was enough for the powdered isolate to mix; then nitrogen flow was started. After 90 minutes, triplicate sub-samples were analyzed for loss on drying (LOD) using a vacuum oven at 110°C overnight to dry the sub-samples.
[0089] Initial water uptake was slow but then accelerated. Consistent with the slow uptake, during the early phases of humidification, the interior of the flask looked dusty or foggy. At about one hour, the material appeared to become moist enough to agglomerate and the interior wall of the flask became clearer.
[0090] The flask was returned to the rotary evaporator, but now the configuration was changed. The nitrogen feed was removed, a water bath was placed to heat the flask, and the condenser was connected to a vacuum pump. The material was dried with the bath temperature at about 70°C, pressure at about 105 mbar, and rotation rate about 50 rpm. The dehumidification was left undisturbed for 90 minutes under these conditions. Samples were taken again for LOD and residual ethanol concentration. The remaining sample was placed in a gas tight jar and stored at RT for later analyses.2.2 Results and Discussion
[0091] Residual ethanol concentration was measured by weighing approximately 100 mg of material into a GC headspace vial, adding 1 mL ultrapure water including lOOpL of an Internal Standard (500ppm 1 -Propanol in water). The headspace vial was agitated and heated at 80°C, then the headspace gas was sampled using a gastight syringe and injected into the GC for analyses. Volatile species including ethanol were separated using a blood alcohol column and hydrogen as a carrier gas. Concentration of ethanol was determined by comparing peak area to a standard curve. Other peaks appearing in the chromatogram were estimated by comparison to the internal standard signal. Peaks associated with ethyl acetate and acetaldehyde were previously identified, but there were several unidentified peaks. The condensate collected during processing had an aroma like the corn protein isolate ingredient itself.
[0092] Percentages of concentration reduction of ethanol, acetaldehyde, ethyl acetate, and the four unidentified peaks after humidification and dehumidification (in one cycle), as compared to the concentration in the starting material, were shown in Table 6. UV1 to UV4 represented volatiles of some of the unidentified peaks.Table 6Example 33.1 Materials and Method
[0093] Approximately 5g samples of com protein isolate (CPI) (Cargill Incorporated), pea protein isolate (PPI) (Cargill Incorporated), and textured soy flour (TSF) (Cargill Incorporated) were weighed and placed in shallow aluminum weigh boats. Boats were placed in a Unox combi oven set for humidification treatment conditions of either (a) 90°C, 30 minutes, and 100% relative humidity or (b) 60°C, 60 minutes, and 75% relative humidity (80% relative humidity for 30 minutes and 70% relative humidity for the remaining 30 minutes). Six samples were prepared for each 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 dried samples were exactly weighed, placed in vials and frozen until analysis.
[0094] For sensory analysis, single samples of about 40g CPI were placed in larger aluminum pans and exposed to the same treatment conditions. At the end of the humidification phase, samples were transferred to mylar bags and frozen without any drying treatment.
[0095] 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 0.25, 0.5, 1.0, 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.
[0096] The panel was then given 3 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 already been 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 was an overall flavor intensity value. The response curve can be used to compute an equivalent concentration (by rearrangement of the regression equation) that reflected 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.3.2 Results and Discussion
[0097] As shown in Table 7, the treatments caused a substantial decrease in the flavor intensity (%).Table 7
[0098] Treated and untreated samples collected before drying were analyzed using a calibrated GC method. Not all compounds in the calibration set appear in the samples. As the results in Table 8 show, significant decreases in the concentrations of these compounds (%) were observed in the more intense treatment.Table 8*l-pentanol was not observed in the untreated TSF.Example 44.1 Materials and Method
[0099] Approximately 5g samples of whey protein isolate (WPI) (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 in Table 9. The samples were heated in the oven for 12 minutes at 75°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.Table 94.2 Results and Discussion4,2.1 Untargeted GC / MS analysis
[0100] 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 volatile compounds 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.
[0101] 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.
[0102] 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.
[0103] Figure 2 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 822 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.
[0104] 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 10 shows how most treatment conditions favor decreasing concentrations.Table 104,2.2 Targeted GC / FID analysis
[0105] 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 11 shows the distribution of calibrated compounds in the untreated samples. About 90% of the mass of these compounds are associated with hexanal, l-octen-3-ol, 4-methyl-l -pentanol, 2-ethyl- 6-methyl-pyrazine, 2-ethyl-l -hexanol, benzaldehyde, heptanal, and 4-ethyl-benzaldehyde. 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 11
[0106] The treatment process drastically reduces volatile compounds and can change the overall composition of these individual volatile compounds. Table 12 shows the WPI volatile composition (of tracked compounds) after humidifying at 90°C at 100% RH for 90 minutes. Whereas hexanal was the major species in the composition prior to treatment, it has diminished, and other minor compounds are more resistant to removal and have increased comparatively, such as benzaldehyde and l-octen-3-ol.Table 12
[0107] Table 13 shows the percentage reduction of major volatile compounds after treatment as compared to the untreated sample. For the treatment producing Table 12, hexanal was removedat 81.4%, while benzaldehyde and l-octen-3-ol were more resistant to removal at -10.1% and 6.2%, respectively.
[0108] 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 conditionTable 13
[0109] 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. Effects of both humidifying temperature and humidifying period are more dependent on the relative humidity of the treatment. For example, higher humidifying temperature, lower relative humidity conditions tended to increase certain volatile concentrations, while high humidifying temperature, high relative humidity conditions were the best at reducing volatile concentrations.
[0110] Certain classes of volatile compounds appear more resistant to high relative humidity conditions, such as alcohols, 2-hexanol, l-octen-3-ol, 2-ethyl-l -hexanol, and 4-methyl-l-pentanol. All of these volatile compounds have lower correlations with RH than most species and the “All Peaks” summation.[OHl] Some volatile compounds have a stronger negative correlation to the humidifying temperature, such as benzaldehyde, 2-ethyl-6-methyl-pyrazine, and dimethyl disulfide, indicating that higher humidifying temperature conditions result in the formation of these species.Table 144,2,3 Conclusion
[0112] The following observations can be drawn from the above studies:
[0113] - A large number of volatile compounds decreased in concentration as indicated by untargeted GC / MS. A relatively small number of compounds increased in concentration.
[0114] - The changes in concentration found in untargeted analyses were dominated by the change in concentration of the more prominent compounds.
[0115] - Most volatile compounds tracked in quantitative analysis showed sensitivity to conditions during humidification. Generally, high humidity favored decreased concentrations after treatment.
[0116] - The highest degree of removal of most volatile compounds was under high relative humidity and high humidifying temperature conditions.Example 55.1 Materials and Method
[0117] Approximately 5g samples of caseinate protein (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 in Table 15. 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.Table 155.2 Results and Discussion5,2, 1 Untargeted GC / MS analysis
[0118] 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 volatile compounds 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.
[0119] 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.
[0120] 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.
[0121] Figure 3 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 425 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.
[0122] 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 16 shows how most treatment conditions favor decreasing concentrations over increasing concentrations but relative humidity makes this effect essentially universal.Table 165,2.2 Targeted GC / FID analysis
[0123] 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 17 shows the distribution of calibrated compounds in the untreated samples. About 92% of the mass of these compounds are associated with 4-methyl-l -pentanol, 2-ethyl-6-methyl-pyrazine, 1- octen-3-ol, 2-ethyl-2-hexanol, benzaldehyde, hexanal, 4-ethyl-benzaldehyde, octanal, and heptanal. 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 17
[0124] The treatment process drastically reduces volatile compounds and can change the overall composition of these individual volatile compounds. Table 18 shows the caseinate protein volatile composition (of tracked compounds) after humidifying at 90°C at 100% RH for 90 minutes. Certain compounds (hexanal, heptanal, and 2-heptanone) in the composition have diminished significantly and other compounds are more resistant to removal and have increased comparatively, such as 2-ethyl-6-methyl-pyrazine and l-octen-3-ol.Table 18
[0125] Tables 19 and 20 show the percentage reduction of major volatile compounds after treatment as compared to the untreated samples. For the treatment producing Table 18, hexanal was removed at 63.0%, while 2-ethyl-6-methyl-pyrazine and l-octen-3-ol were more resistant to removal at 19.0% and 27.5%, respectively.
[0126] 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 19Table 20
[0127] Table 21 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. Effects of both humidifying temperature andhumidifying period are more dependent on the relative humidity of the treatment. For example, higher humidifying temperature, lower relative humidity conditions tended to increase certain volatile concentrations, while high humidifying temperature, high relative humidity conditions were the best at reducing volatile concentrations.
[0128] Certain classes of volatile compounds appear more resistant to high relative humidity conditions, such as pyrazines and alcohols seem to be more resistant to removal and were more similar across all treatments.Table 215,2,3 Conclusion
[0129] The following observations can be drawn from the above studies:
[0130] - A large number of volatile compounds decreased in concentration as indicated by untargeted GC / MS. A relatively small number of compounds increased in concentration.
[0131] - The changes in concentration found in untargeted analyses were dominated by the change in concentration of the more prominent compounds.
[0132] - Most volatile compounds tracked in quantitative analysis showed sensitivity to conditions during humidification. Generally, high humidity favored decreased concentrations after treatment.
[0133] - The highest degree of removal of most volatile compounds was under high relative humidity and high humidifying temperature conditions.Example 66.1 Materials and Method
[0134] Approximately 5g samples of almond protein (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 in Table 22. The samples were heated in the oven for 20 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.Table 226.2 Results and Discussion6,2, 1 Untargeted GC / MS analysis
[0135] 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 volatile compounds 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.
[0136] 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 isthe 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.
[0137] 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.
[0138] 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 567 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.
[0139] 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). As per Table 23, the highest number of volatile compounds were removed when the treatment done in the higher percentages of relative humidity.Table 2362.2 Targeted GC / FID analysis
[0140] 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 24 shows the distribution of calibrated compounds in the untreated samples. About 94% of the mass of these compounds are associated with benzaldehyde, hexanal, 2-ethyl-l -hexanol, 2-ethyl- 6-methyl-pyrazine, octanal, l-octen-3-ol, 4-methyl-l -pentanol, and heptanal. 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 24
[0141] The treatment process drastically reduces volatile compounds and can change the overall composition of these individual volatile compounds. Table 25 shows the almond protein volatile composition (of tracked compounds) after humidifying at 90°C at 100% RH for 90 minutes. The dominance of benzaldehyde in the composition has diminished and other minor compounds are more resistant to removal and have increased comparatively, such as 2-ethyl-6-methyl-pyrazine and octanal.Table 25
[0142] Tables 26 and 27 show the percentage reduction of major volatile compounds after treatment as compared to the untreated sample. For the treatment producing Table 25, benzaldehyde was removed at 96.3%, while 2-ethyl-6-methyl-pyrazine and octanal were more resistant to removal at 7.4% and 74.1%, respectively.
[0143] 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 26Table 27
[0144] Table 28 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. Effects of both humidifying temperature and humidifying period are more dependent on the relative humidity of the treatment. For example, higher humidifying temperature, lower relative humidity conditions tended to increase certain volatile concentrations, while high humidifying temperature, high relative humidity conditions were the best at reducing volatile concentrations.Table 286,2,3 Conclusion
[0145] The following observations can be drawn from the above studies:
[0146] - A large number of volatile compounds decreased in concentration as indicated by untargeted GC / MS. A relatively small number of compounds increased in concentration.
[0147] - The changes in concentration found in untargeted analyses were dominated by the change in concentration of the more prominent compounds.
[0148] - Most volatile compounds tracked in quantitative analysis showed sensitivity to conditions during humidification. Generally, high humidity favored decreased concentrations after treatment.
[0149] - The highest degree of removal of most volatile compounds was under high relative humidity and high humidifying temperature conditions.Clauses describing the invention
[0150] Clause 1. A process for preparing a protein product, comprising the steps of: a. providing a protein containing material; b. humidifying the protein 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 protein product; wherein the protein product has a reduced volatile compound content as compared to an equivalent untreated protein product.
[0151] Clause 2. The process of clause 1, wherein the protein containing material is a plant protein containing material or a non-plant protein containing material.
[0152] Clause 3. The process of any of the preceding clauses, wherein the plant protein containing material comprises plant protein selected from the group consisting of legume protein, composite protein, cereal protein, nightshade protein, cucurbit protein, mustard protein, knotweed protein, pigweed protein, duckweed protein, nut protein, and any combinations thereof.
[0153] Clause 4. The process of any of the preceding clauses, wherein the plant protein containing material comprises plant protein selected from the group consisting of soy protein, faba protein, pea protein, lentil protein, chickpea protein, bean protein, mung bean protein, sunflower protein, wheat protein, corn protein, rice protein, potato protein, pumpkin protein, watermelon protein, canola or rapeseed protein, buckwheat protein, amaranth protein, quinoa protein, lemna protein, almond protein, and any combinations thereof.
[0154] Clause 5. The process of any of the preceding clauses, wherein the non-plant protein containing material comprises non-plant protein selected from the group consisting of egg white protein, dairy protein, and any combinations thereof.
[0155] Clause 6. The process of any of the preceding clauses, wherein the protein product is a plant protein product or a non-plant protein product.
[0156] Clause 7. The process of any of the preceding clauses, wherein the relative humidity is in a range from 50 to 100%.
[0157] Clause 8. The process of any of the preceding clauses, wherein the humidifying temperature is in a range from 55 to 95°C.
[0158] Clause 9. The process of any of the preceding clauses, wherein the protein 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.
[0159] Clause 10. The process of any of the preceding clauses, wherein the humidified material is dried at a drying temperature in a range from 50 to 90°C.
[0160] 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.
[0161] 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.
[0162] Clause 13. A process for reducing volatile compound content of a protein product, comprising the steps of:a. humidifying a protein 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 protein product; wherein the protein product has a reduced volatile compound content as compared to an equivalent untreated protein product.
[0163] Clause 14. The process of clause 13, wherein the protein containing material is a plant protein containing material or a non-plant protein containing material.
[0164] Clause 15. The process of any of clauses 13 to 14, wherein the plant protein containing material comprises plant protein selected from the group consisting of legume protein, composite protein, cereal protein, nightshade protein, cucurbit protein, mustard protein, knotweed protein, pigweed protein, duckweed protein, nut protein, and any combinations thereof.
[0165] Clause 16. The process of any of clauses 13 to 15, wherein the plant protein containing material comprises plant protein selected from the group consisting of soy protein, faba protein, pea protein, lentil protein, chickpea protein, bean protein, mung bean protein, sunflower protein, wheat protein, corn protein, rice protein, potato protein, pumpkin protein, watermelon protein, canola or rapeseed protein, buckwheat protein, amaranth protein, quinoa protein, lemna protein, almond protein, and any combinations thereof.
[0166] Clause 17. The process of any of clauses 13 to 16, wherein the non-plant protein containing material comprises non-plant protein selected from the group consisting of egg white protein, dairy protein, and any combinations thereof.
[0167] Clause 18. The process of any of clauses 13 to 17, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.
[0168] Clause 19. The process of any of clauses 13 to 18, wherein the protein 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 protein product.
[0169] Clause 20. The process of any of clauses 13 to 19, wherein the protein product is plant protein product or non-plant protein product.
[0170] Clause 21. The process of any of clauses 13 to 20, 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.
[0171] Clause 22. A protein product prepared by the process of any of the preceding clauses.
[0172] Clause 23. A protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated protein product.
[0173] Clause 24. The protein product of any of clauses 22 to 23, having 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 protein product.
[0174] Clause 25. The plant product of any of clauses 22 to 24, wherein the protein product is a plant protein product or a non-plant protein product.
[0175] Clause 26. A whey protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated whey protein product.
[0176] Clause 27. A whey protein product prepared by the process of any of clauses 1 to 21.
[0177] Clause 28. The whey protein product of any of clauses 26 to 27, having 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 whey protein product.
[0178] Clause 29. The whey protein product of any of clauses 26 to 28, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, alcohol, and pyrazine.
[0179] Clause 30. The whey protein product of any of clauses 26 to 29, wherein the one or more volatile compounds are selected from the group consisting of hexanal, benzaldehyde, l-octen-3- ol, dimethyl disulfide, octanal, 2-4-nonadienal, 4-ethyl-benzaledhyde, 2-ethyl-l -hexanol, 2- hexanol, 4-m ethyl- 1 -pentanol, 2-ethyl-6-methyl-pyrazine, heptanal, and any combinations thereof.
[0180] Clause 31. The whey protein product of any of clauses 26 to 30, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, benzaldehyde, octanal, l-octen-3-ol, 2-ethyl-l -hexanol, and any combinations thereof.
[0181] Clause 32. The whey protein product of any of clauses 26 to 31, having content of hexanal reduced by a range from 50 to 85%, preferably from 60 to 85%, more preferably from 70 to 85%, as compared to an equivalent untreated whey protein product.
[0182] Clause 33. The whey protein product of any of clauses 26 to 32, having content of hexanal reduced by at least 60%, preferably at least 70%, or more preferably at least 80%, as compared to an equivalent untreated whey protein product.
[0183] Clause 34. The whey protein product of any of clauses 26 to 33, having content of heptanal reduced by a range from 50 to 85%, preferably from 60 to 85%, more preferably from 65 to 85%, as compared to an equivalent untreated whey protein product.
[0184] Clause 35. The whey protein product of any of clauses 26 to 34, having content of heptanal reduced by at least 60%, preferably at least 65%, or more preferably at least 80%, as compared to an equivalent untreated whey protein product.
[0185] Clause 36. The whey protein product of any of clauses 26 to 35, having content of benzaldehyde reduced by a range from 25 to 50%, preferably from 30 to 50%, more preferably from 35 to 50%, as compared to an equivalent untreated whey protein product.
[0186] Clause 37. The whey protein product of any of clauses 26 to 36, having content of benzaldehyde reduced by at least 30%, preferably at least 35%, or more preferably at least 40%, as compared to an equivalent untreated whey protein product.
[0187] Clause 38. The whey protein product of any of clauses 26 to 37, having content of octanal reduced by a range from 30 to 70%, preferably from 40 to 70%, more preferably from 60 to 70%, as compared to an equivalent untreated whey protein product.
[0188] Clause 39. The whey protein product of any of clauses 26 to 38, having content of benzaldehyde reduced by at least 30%, preferably at least 40%, or more preferably at least 60%, as compared to an equivalent untreated whey protein product.
[0189] Clause 40. The whey protein product of any of clauses 26 to 39, having content of 1-octen- 3-ol reduced by a range from 10 to 25%, preferably from 15 to 25%, more preferably from 18 to 25%, as compared to an equivalent untreated whey protein product.
[0190] Clause 41. The whey protein product of any of clauses 26 to 40, having content of 1-octen- 3-ol reduced by at least 10%, preferably at least 15%, or more preferably at least 18%, as compared to an equivalent untreated whey protein product.
[0191] Clause 42. The whey protein product of any of clauses 26 to 41, having content of 2-ethyl- 1 -hexanol reduced by a range from 45 to 65%, preferably from 50 to 65%, more preferably from 55 to 65%, as compared to an equivalent untreated whey protein product.
[0192] Clause 43. The whey protein product of any of clauses 26 to 42, having content of 2-ethyl- 1-hexanol reduced by at least 45%, preferably at least 50%, or more preferably at least 55%, as compared to an equivalent untreated whey protein product.
[0193] Clause 44. A caseinate protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated caseinate protein product.
[0194] Clause 45. A caseinate protein product prepared by the process of any of clauses 1 to 21.
[0195] Clause 46. The caseinate protein product of any of clauses 44 to 45, having 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 whey protein product.
[0196] Clause 47. The caseinate protein product of any of clauses 44 to 46, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, alcohol, and pyrazine.
[0197] Clause 48. The caseinate protein product of any of clauses 44 to 47, wherein the one or more volatile compounds are selected from the group consisting of hexanal, 2-ethyl-6-methyl-pyrazine, l-octen-3-ol, heptanal, benzaldehyde, octanal, 4-ethyl-benzaledhyde, 2-heptanone, 4- m ethyl- 1 -pentanol, and any combinations thereof.
[0198] Clause 49. The caseinate protein product of any of clauses 44 to 48, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, benzaldehyde, octanal, 4-ethyl-benzaledhyde, 2-heptanone, 2-ethyl-6-methyl-pyrazine, 1-octen- 3-ol, 4-m ethyl- 1 -pentanol, and any combinations thereof.
[0199] Clause 50. The caseinate protein product of any of clauses 44 to 49, having content of hexanal reduced by a range from 50 to 80%, preferably from 60 to 80%, more preferably from 70 to 80%, as compared to an equivalent untreated caseinate protein product.
[0200] Clause 51. The caseinate protein product of any of clauses 44 to 50, having content of hexanal reduced by at least 60%, preferably at least 65%, or more preferably at least 70%, as compared to an equivalent untreated caseinate protein product.
[0201] Clause 52. The caseinate protein product of any of clauses 44 to 51, having content of heptanal reduced by a range from 55 to 90%, preferably from 65 to 90%, more preferably from 70 to 90%, as compared to an equivalent untreated caseinate protein product.
[0202] Clause 53. The caseinate protein product of any of clauses 44 to 52, having content of heptanal reduced by at least 70%, preferably at least 75%, or more preferably at least 80%, as compared to an equivalent untreated caseinate protein product.
[0203] Clause 54. The caseinate protein product of any of clauses 44 to 53, having content of benzaldehyde reduced by a range from 40 to 70%, preferably from 45 to 70%, more preferably from 50 to 70%, as compared to an equivalent untreated caseinate protein product.
[0204] Clause 55. The caseinate protein product of any of clauses 44 to 54, having content of benzaldehyde reduced by at least 45%, preferably at least 50%, or more preferably at least 55%, as compared to an equivalent untreated caseinate protein product.
[0205] Clause 56. The caseinate protein product of any of clauses 44 to 55, having content of octanal reduced by a range from 35 to 80%, preferably from 40 to 80%, more preferably from 45 to 80%, as compared to an equivalent untreated caseinate protein product.
[0206] Clause 57. The caseinate protein product of any of clauses 44 to 56, having content of octanal reduced by at least 40%, preferably at least 60%, or more preferably at least 70%, as compared to an equivalent untreated caseinate protein product.
[0207] Clause 58. The caseinate protein product of any of clauses 42 to 57, having content of 4- ethyl-benzaldehyde reduced by a range from 50 to 80%, preferably from 55 to 80%, more preferably from 60 to 80%, as compared to an equivalent untreated caseinate protein product.
[0208] Clause 59. The caseinate protein product of any of clauses 42 to 58, having content of 4- ethyl-benzaldehyde reduced by at least 55%, preferably at least 60%, or more preferably at least 65%, as compared to an equivalent untreated caseinate protein product.
[0209] Clause 60. The caseinate protein product of any of clauses 44 to 59, having content of 2- heptanone reduced by a range from 75 to 95%, preferably from 80 to 95%, more preferably from 85 to 95%, as compared to an equivalent untreated caseinate protein product.
[0210] Clause 61. The caseinate protein product of any of clauses 44 to 60, having content of 2- heptanone reduced by at least 75%, preferably at least 80%, or more preferably at least 85%, as compared to an equivalent untreated caseinate protein product.
[0211] Clause 62. The caseinate protein product of any of clauses 44 to 61, having content of 2- ethyl-6-methyl-pyrazine reduced by a range from 10 to 30%, preferably from 15 to 30%, more preferably from 20 to 30%, as compared to an equivalent untreated caseinate protein product.
[0212] Clause 63. The caseinate protein product of any of clauses 44 to 62, having content of 2- ethyl-6-methyl-pyrazine reduced by at least 10%, preferably at least 15%, or more preferably at least 20%, as compared to an equivalent untreated caseinate protein product.
[0213] Clause 64. The caseinate protein product of any of clauses 44 to 63, having content of 1- octen-3-ol reduced by a range from 15 to 40%, preferably from 20 to 40%, more preferably from 25 to 40%, as compared to an equivalent untreated caseinate protein product.
[0214] Clause 65. The caseinate protein product of any of clauses 44 to 64, having content of 1- octen-3-ol reduced by at least 15%, preferably at least 20%, or more preferably at least 25%, as compared to an equivalent untreated caseinate protein product.
[0215] Clause 66. The caseinate protein product of any of clauses 42 to 65, having content of 4- m ethyl- 1 -pentanol reduced by a range from 20 to 45%, preferably from 25 to 45%, more preferably from 30 to 45%, as compared to an equivalent untreated caseinate protein product.
[0216] Clause 67. The caseinate protein product of any of clauses 44 to 66, having content of 4- m ethyl- 1 -pentanol reduced by at least 20%, preferably at least 25%, or more preferably at least 30%, as compared to an equivalent untreated caseinate protein product.
[0217] Clause 68. An almond protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated almond protein product.
[0218] Clause 69. An almond protein product prepared by the process of any of clauses 1 to 21.
[0219] Clause 70. The almond protein product of any of clauses 68 to 69, having 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 almond protein product.
[0220] Clause 71. The almond protein product of any of clauses 68 to 70, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, alcohol, and pyrazine.
[0221] Clause 72. The almond protein product of any of clauses 68 to 71, wherein the one or more volatile compounds are selected from the group consisting of benzaldehyde, hexanal, 4-ethyl- benzaledhyde, octanal, l-octen-3-ol, 2-hexanol, 2-ethyl-l -hexanol, heptanal, 4-m ethyl- 1- pentanol, 2-ethyl-6-methyl-pyrazine, and any combinations thereof.
[0222] Clause 73. The almond protein product of any of clauses 68 to 72, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, benzaldehyde, octanal, 2-ethyl-6-methyl-pyrazine, l-octen-3-ol, 2-ethyl-l -hexanol, and any combinations thereof.
[0223] Clause 74. The almond protein product of any of clauses 68 to 73, having content of hexanal reduced by a range from 50 to 90%, preferably from 55 to 90%, more preferably from 60 to 90%, as compared to an equivalent untreated almond protein product.
[0224] Clause 75. The almond protein product of any of clauses 68 to 74, having content of hexanal reduced by at least 60%, preferably at least 65%, or more preferably at least 70%, as compared to an equivalent untreated almond protein product.
[0225] Clause 76. The almond protein product of any of clauses 68 to 75, having content of heptanal reduced by a range from 50 to 90%, preferably from 55 to 90%, more preferably from 60 to 90%, as compared to an equivalent untreated almond protein product.
[0226] Clause 77. The almond protein product of any of clauses 68 to 76, having content of heptanal reduced by at least 60%, preferably at least 65%, or more preferably at least 70%, as compared to an equivalent untreated almond protein product.
[0227] Clause 78. The almond protein product of any of clauses 68 to 77, having content of benzaldehyde reduced by a range from 70 to 99%, preferably from 75 to 99%, more preferably from 80 to 99%, as compared to an equivalent untreated almond protein product.
[0228] Clause 79. The almond protein product of any of clauses 68 to 78, having content of benzaldehyde reduced by at least 70%, preferably at least 80%, or more preferably at least 90%, as compared to an equivalent untreated almond protein product.
[0229] Clause 80. The almond protein product of any of clauses 68 to 79, having content of octanal reduced by a range from 45 to 85%, preferably from 50 to 85%, more preferably from 55 to 85%, as compared to an equivalent untreated almond protein product.
[0230] Clause 81. The almond protein product of any of clauses 68 to 80, having content of octanal reduced by at least 50%, preferably at least 60%, or more preferably at least 70%, as compared to an equivalent untreated almond protein product.
[0231] Clause 82. The almond protein product of any of clauses 68 to 81, having content of 2- ethyl-6-methyl-pyrazine reduced by a range from 10 to 30%, preferably from 12 to 30%, more preferably from 15 to 30%, as compared to an equivalent untreated almond protein product.
[0232] Clause 83. The almond protein product of any of clauses 68 to 82, having content of 2- ethyl-6-methyl-pyrazine reduced by at least 10%, preferably at least 15%, or more preferably at least 20%, as compared to an equivalent untreated almond protein product.
[0233] Clause 84. The almond protein product of any of clauses 68 to 83, having content of 1- octen-3-ol reduced by a range from 65 to 95%, preferably from 70 to 95%, more preferably from 75 to 95%, as compared to an equivalent untreated almond protein product.
[0234] Clause 85. The almond protein product of any of clauses 68 to 84, having content of 1- octen-3-ol reduced by at least 70%, preferably at least 75%, or more preferably at least 80%, as compared to an equivalent untreated almond protein product.
[0235] Clause 86. The almond protein product of any of clauses 68 to 85, having content of 2- ethyl-1 -hexanol reduced by a range from 25 to 95%, preferably from 30 to 95%, more preferably from 55 to 95%, as compared to an equivalent untreated almond protein product.
[0236] Clause 87. The almond protein product of any of clauses 68 to 86, having content of 2- ethyl-1 -hexanol reduced by at least 25%, preferably at least 55%, or more preferably at least 80%, as compared to an equivalent untreated almond protein product.
Claims
CLAIMSWhat is claimed is:
1. A process for preparing a protein product, comprising the steps of: a. providing a protein containing material; b. humidifying the protein 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 protein product; wherein the protein product has a reduced volatile compound content as compared to an equivalent untreated protein product.
2. The process of claim 1, wherein the protein containing material is a plant protein containing material or a non-plant protein containing material.
3. The process of any of the preceding claims, wherein the plant protein containing material comprises plant protein selected from the group consisting of legume protein, composite protein, cereal protein, nightshade protein, cucurbit protein, mustard protein, knotweed protein, pigweed protein, duckweed protein, nut protein, and any combinations thereof.
4. The process of any of the preceding claims, wherein the plant protein containing material comprises plant protein selected from the group consisting of soy protein, faba protein, pea protein, lentil protein, chickpea protein, bean protein, mung bean protein, sunflower protein, wheat protein, com protein, rice protein, potato protein, pumpkin protein, watermelon protein, canola or rapeseed protein, buckwheat protein, amaranth protein, quinoa protein, lemna protein, almond protein, and any combinations thereof.
5. The process of any of the preceding claims, wherein the non-plant protein containing material comprises non-plant protein selected from the group consisting of egg white protein, dairy protein, and any combinations thereof.
6. The process of any of the preceding claims, wherein the protein product is a plant protein product or a non-plant protein product.
7. The process of any of the preceding claims, wherein the relative humidity in the humidifying step is in a range from 50 to 100%.
8. The process of any of the preceding claims, wherein the humidifying temperature is in a range from 55 to 95°C.
9. The process of any of the preceding claims, wherein the protein 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.
10. The process of any of the preceding claims, wherein the humidified material is dried at a drying temperature in a range from 50 to 90°C.
11. 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.
12. 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.
13. A process for reducing volatile compound content of a protein product, comprising the steps of: a. humidifying a protein 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 protein product; wherein the protein product has a reduced volatile compound content as compared to an equivalent untreated protein product.
14. The process of claim 13, wherein the protein containing material is a plant protein containing material or a non-plant protein containing material.
15. The process of any of claims 13 to 14, wherein the plant protein containing material comprises plant protein selected from the group consisting of legume protein, composite protein, cereal protein, nightshade protein, cucurbit protein, mustard protein, knotweed protein, pigweed protein, duckweed protein, nut protein, and any combinations thereof.
16. The process of any of claims 13 to 15, wherein the plant protein containing material comprises plant protein selected from the group consisting of soy protein, faba protein, pea protein, lentil protein, chickpea protein, bean protein, mung bean protein, sunflower protein, wheat protein, com protein, rice protein, potato protein, pumpkin protein, watermelon protein, canola or rapeseed protein, buckwheat protein, amaranth protein, quinoa protein, lemna protein, almond protein, and any combinations thereof.
17. The process of any of claims 13 to 16, wherein the non-plant protein containing material comprises non-plant protein selected from the group consisting of egg white protein, dairy protein, and any combinations thereof.
18. The process of any of claims 13 to 17, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.
19. The process of any of claims 13 to 18, wherein the protein 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 protein product.
20. The process of any of claims 13 to 19, wherein the protein product is plant protein product or non-plant protein product.
21. The process of any of claims 13 to 20, 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.
22. A protein product prepared by the process of any of the preceding claims.
23. A protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated protein product.
24. The protein product of any of claims 22 to 23, having 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 protein product.
25. The plant product of any of claims 22 to 24, wherein the protein product is a plant protein product or a non-plant protein product.
Citation Information
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