WO2025212640A1 - Corn protein product and process of preparing the same - Google Patents

Corn protein product and process of preparing the same

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Publication number
WO2025212640A1
WO2025212640A1 PCT/US2025/022530 US2025022530W WO2025212640A1 WO 2025212640 A1 WO2025212640 A1 WO 2025212640A1 US 2025022530 W US2025022530 W US 2025022530W WO 2025212640 A1 WO2025212640 A1 WO 2025212640A1
Authority
WO
WIPO (PCT)
Prior art keywords
protein product
corn protein
humidifying
com
drying
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
PCT/US2025/022530
Other languages
French (fr)
Inventor
Yara Licceth BENAVIDES PAZ
Alexandra Jean FIEGEL
Daniel Scott GASPARD
Mohammad Sharif KHAN
Erika Lyn MCCONVILLE
Michael Alan Mortenson
Michael Arthur PORTER
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cargill Inc
Original Assignee
Cargill Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cargill Inc filed Critical Cargill Inc
Publication of WO2025212640A1 publication Critical patent/WO2025212640A1/en
Pending legal-status Critical Current
Anticipated expiration legal-status Critical

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Classifications

    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/14Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J1/00Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
    • A23J1/16Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from waste water of starch-manufacturing plant or like wastes
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23JPROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
    • A23J3/00Working-up of proteins for foodstuffs
    • A23J3/14Vegetable proteins

Definitions

  • This invention relates to the field of plant protein products, in particular corn protein products.
  • a plant protein product e.g., corn protein product
  • a reduced flavor intensity and an improved process for preparing such product are needed.
  • the present disclosure provides a process for preparing a corn protein product comprising the steps of providing a corn protein containing material; humidifying the corn protein containing material at an elevated 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 protein product.
  • the resulting com protein product has a reduced volatile compound content as compared to an equivalent untreated com protein product.
  • the present disclosure also provides a corn protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated corn protein product.
  • Figure 1 shows the overall flavor intensity of treated and untreated com protein isolate (CPI) 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.
  • 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 represented by the lighter symbols while treatment 8 is represented by the darker symbols. 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.
  • Figure 4 shows the response of overall flavor intensity as a function of humidificationdrying cycles.
  • Figure 5 shows the changes in total peak area as a function of humidification- drying cycles.
  • Figures 6A to 6D show the response of the detected volatile compounds, expressed in ppm, found in CPI samples to the number of humidification-drying cycles.
  • Figures 7A to 7E show the response of the detected volatile compounds, expressed as a percentage of the initial concentration, found in CPI samples to the number of humidificationdrying cycles.
  • Figure 8 is a log-log plot (log2(treated/untreated) against loglO(treated)) that shows changes in concentrations of volatile compounds in the CPI samples that have undergone one (upper left), two (upper right), four (lower left), and six (lower right) humidification-drying cycles.
  • ppm parts per million
  • percentage percentage
  • ratios are based on a dry weight basis. Percentage based on a dry weight basis is also referred to as wt% below .
  • room temperature or “RT” refers to a temperature between 20°C to 25°C.
  • RT room temperature
  • 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.
  • specified acts can be carried out concurrently unless explicit claim language recites that they be carried out separately.
  • 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.
  • the present disclosure provides a process for preparing a com protein product.
  • the process comprises the steps of humidifying a com protein containing material at an elevated 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 protein product.
  • the resulting corn protein product has one or more improved attributes as compared to an equivalent untreated corn protein product; preferably, the one or more improved attributes may include, but may not be limited to, a reduced volatile compound content.
  • the corn protein containing material serves as a starting material to the process and may include, but may not be limited to, textured com flour, textured com protein concentrate, com protein isolate, corn protein concentrate, or any combinations thereof.
  • the corn protein containing material can have a protein concentration in a range from 10 to 90 wt% on a dry basis; preferably, the corn protein containing material can have a protein concentration of at least 50 wt% on a dry basis.
  • the com 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.
  • moisture content of the resulting humidified material is not increased by the humidifying step.
  • 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.
  • steam is not to be used in the humidifying step to avoid degradation of the starting material.
  • 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%.
  • 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.
  • the humidifying period for humidifying the corn 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.
  • the humidifying period can be 10 minutes, 15 minutes, 30 minutes, 45 minutes, 60 minutes, 75 minutes, or 90 minutes.
  • the humidifying period can be in a range from 10 to 90 minutes, from 15 to 75 minutes, or from 30 to 60 minutes.
  • the humidifying period can be at most 90 minutes.
  • the humidified material can be de-humidified in the drying step to obtain the final corn protein product.
  • the drying step can be carried out at a drying temperature for a drying period to obtain the corn 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 corn protein product.
  • 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.
  • the drying period can be 5 minutes, 8 minutes, 10 minutes, 15 minutes, 20 minutes, or 25 minutes.
  • the drying period can be in a range from 5 to 25 minutes, from 8 to 20 minutes, from 10 to 15 minutes.
  • the drying period can be at least 5 minutes. In another aspect, the drying period can be at most 25 minutes.
  • the relative humidity at the drying step can be 0%, from 0 to 0.5%, from 0.5% to 1%, or at least 1%.
  • 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.
  • 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.
  • the corn protein product obtained from the process as described above has content of one or more volatile compounds reduced as compared to an equivalent untreated corn protein product.
  • the content of one or more volatile compounds in the corn 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 corn protein product.
  • the com protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated corn protein product
  • the content of one or more volatile compounds in the com 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 com protein product.
  • the present disclosure provides a process for reducing volatile compound content of a com protein product.
  • off-notes of the corn protein product are reduced by the process of the instant invention.
  • 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.
  • the process comprises a step of humidifying a com 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 com protein product.
  • the resulting corn 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 corn protein product.
  • the resulting com protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated com protein product; in other words, the resulting com protein product can be completely free of one or more volatile compounds.
  • the com 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 corn protein product.
  • the corn protein containing material may include, but may not be limited to, textured corn flour, textured com protein concentrate, corn protein isolate, corn protein concentrate, or any combinations thereof.
  • the corn protein containing material can have a protein content in a range from 10 to 90 wt% on a dry basis; preferably, the corn protein containing material can have a protein concentration of at least 50 wt% on a dry basis.
  • the com 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 corn 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.
  • 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 protein product.
  • 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.
  • 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.
  • no purification step may be required to separate fibers and starch out from the com protein containing material before the material is fed to the process.
  • no enzymatic step may be required in any process of the instant invention described in the present disclosure.
  • no alkaline treatment step may be required in any process of the instant invention described in the present disclosure.
  • no alcohol washing step may be required in any process of the instant invention described in the present disclosure.
  • the com protein product of the present invention has content of one or more volatile compounds reduced as compared to an equivalent untreated com protein product.
  • the corn protein product may have one or more off-notes partially or completely removed.
  • the content of one or more volatile compounds in the corn protein product described in this disclosure is reduced, preferably completely eliminated, as compared to an equivalent untreated corn protein product.
  • Volatile compounds are substances present in a com 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
  • 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
  • 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.
  • the volatile compounds may include, but may not be limited to, hexanal, heptanal, 2-heptanone, 2-pentyl-furan, benzaldehyde, heptenal, l-octen-3-ol, octanal, 2-octanone, 2-butyl-furan, 2-ethyl-l-hexanol, thiophene, 2-hexanol, 2-hexanone, 2-methyl-pentanal, 2- methyl-thiophene, 2-nonanone, 2-propyl-furan, 4-ethyl-benzaledhyde, 2-ethyl-pyrazine, o- tolualdehyde, or any combinations thereof.
  • the corn 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 corn protein product.
  • the com protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated com protein product.
  • the corn protein product of the present invention may be prepared by any process described in the present disclosure.
  • attributes other than the volatile compound content of the corn protein product prepared by any process of the instant invention described in the present disclosure may be improved as compared to an equivalent untreated corn protein product.
  • CPI corn protein isolate
  • Cargill Incorporated corn protein isolate
  • Table 1 Approximately 5g samples of corn protein isolate (CPI) (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.
  • CPI corn protein isolate
  • 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.
  • PES polyethersulfone
  • 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.
  • 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 0%. In high temperatures and dry conditions, the samples lost weight.
  • PCA Principal Component Analysis
  • 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 the largest number of compounds.
  • Figure 3 shows the comparable information for those samples that were humidified and then dried. While about 1,350 compounds were identified in the samples that were humidified but not dried, about 850 compounds were identified in the samples that were humidified and then dried.
  • Columns 1 to 3 represent number of compounds having significant changes in concentration between untreated samples and humidified-only samples, between untreated samples and humidified and dried samples, and between humidified-only samples and humidified and dried samples, respectively. Except for treatment condition 1 (30°C, 100% relative humidity, and 30 min), half or more of the compounds measured showed a significant change as compared to the untreated (which was assumed to be invariant) before drying (column 1) and after (column 2) drying. Many compounds changed significantly in concentration with drying (column 3) as compared to those before drying.
  • Samples of corn protein isolate (CPI) (Cargill Incorporated) were weighed out. Duplicate samples of about 70g were prepared for ultimate sensory analysis. Triplicate samples of about 5g were prepared for chemical analysis. Samples were weighed into pre-weighed aluminum pans suitable for the sample weight.
  • CPI corn protein isolate
  • 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.
  • PES polyethersulfone
  • the panel was then given three blind samples (concentrations of 0.5%, 2.5%, and 4%) as a validation testing to ensure the panel was aligned and could reproduce their data, they 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 is an overall flavor intensity value.
  • the response curve can be used to compute an apparent 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.
  • Figure 4 shows that two cycles of humidification-drying lead to a lower overall intensity than one cycle, but that additional cycles beyond the second cycle either have minimal benefit or a detrimental effect on the overall intensity as measured by intensity scores.
  • Clause 2 The process of clause 1, wherein the com protein containing material is selected from the group consisting of textured corn flour, textured corn protein concentrate, com protein isolate, com protein concentrate, and any combinations thereof.
  • Clause 7 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.
  • water delivered in the humidifying step is in a form of a liquid water or a vapor.
  • 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.
  • Clause 14 A process for reducing volatile compound content of a corn protein product, comprising the steps of: a. humidifying a com 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 corn protein product; wherein the com protein product has a reduced volatile compound content as compared to an equivalent untreated corn protein product.
  • Clause 16 The process of any of clauses 14 to 15, wherein the com protein containing material is selected from the group consisting of textured corn flour, textured corn protein concentrate, com protein isolate, com protein concentrate, and any combinations thereof.
  • Clause 17 The process of any of clauses 14 to 16, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.
  • Clause 18 The process of any of the clauses 14 to 17, wherein the com 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.
  • Clause 19 The process of any of the clauses 14 to 18, 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.
  • Clause 20 The process of any of clauses 14 to 19, wherein water is uniformly delivered and distributed over the corn protein containing material in the humidifying step.
  • Clause 23 The process of any of clauses 14 to 22, wherein the humidified material is dried at a drying temperature in a range from 50 to 90°C.
  • Clause 24 The process of any of clauses 14 to 23, 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.
  • Clause 25 The process of any of clauses 14 to 24, 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.
  • Clause 26 The process of any of the preceding clauses, wherein the com 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 soy protein product.
  • Clause 27 A corn protein product prepared by the process of any of the preceding clauses.
  • Clause 28 A com protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated com protein product.
  • Clause 29 The corn protein product of any of clauses 27 to 28, 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 corn protein product.
  • Clause 30 The corn protein product of any of clauses 27 to 29, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, ketone, furan, alcohol, and pyrazine.
  • Clause 42 The com protein product of any of clauses 27 to 41, having content of 2-pentyl- furan reduced by at least 90%, at least 95%, or at least 96% as compared to an equivalent untreated corn protein product.
  • Clause 44 The corn protein product of any of clauses 27 to 43, having content of benzaldehyde reduced by a range from 15 to 90%, from 25 to 80%, or from 35 to 70% as compared to an equivalent untreated corn protein product.
  • Clause 45 The corn protein product of any of clauses 27 to 44, having content of benzaldehyde reduced by at least 35%, at least 50%, at least 60%, or at least 65% as compared to an equivalent untreated corn protein product.
  • Clause 51 The corn protein product of any of clauses 27 to 50, having content of 1-octen- 3-ol reduced by at least 20%, at least 70%, at least 90%, or at least 95% as compared to an equivalent untreated corn protein product.
  • Clause 52 The corn protein product of any of clauses 27 to 51, having content of 1-octen- 3-ol reduced by at least 20% after one cycle of humidifying step and the drying step, at least 70% after two cycles of humidifying step and the drying step, at least 90% after four cycles of humidifying step and the drying step, or at least 95% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.
  • Clause 53 The corn protein product of any of clauses 27 to 52, having content of octanal reduced by a range from 15 to 85%, from 20 to 80%, or from 25 to 75% as compared to an equivalent untreated corn protein product.
  • Clause 54 The corn protein product of any of clauses 27 to 53, having content of octanal reduced by at least 25%, at least 50%, at least 70%, or at least 75% as compared to an equivalent untreated com protein product.
  • Clause 56 The corn protein product of any of clauses 27 to 55, having content of 2- octanone reduced by a range from 60 to 99%, from 70 to 95%, or from 80 to 90% as compared to an equivalent untreated corn protein product.
  • Clause 57 The corn protein product of any of clauses 27 to 56, having content of 2- octanone reduced by at least 70%, at least 75%, at least 80%, or at least 85% as compared to an equivalent untreated corn protein product.
  • Clause 59 The corn protein product of any of clauses 27 to 58, having content of thiophene reduced by a range from 80 to 99%, from 90 to 99%, or from 95 to 99% as compared to an equivalent untreated corn protein product.
  • Clause 64 The com protein product of any of clauses 27 to 63, having content of 2-hexanol reduced by at least 60% after one cycle of humidifying step and the drying step, at least 65% after two cycles of humidifying step and the drying step, or at least 75% after six cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.

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Abstract

The present disclosure relates to a corn protein product and a process for preparing the same. The process comprises the steps of providing a corn protein containing material; humidifying the corn protein containing material at an elevated 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 protein product. The corn protein product has content of one or more volatile compounds reduced as compared to an equivalent untreated corn protein product.

Description

CORN PROTEIN PRODUCT AND PROCESS OF PREPARING THE SAME
CROSS REFERENCE
[0001] This application claims the benefit of United States Provisional Application No. 63/572,965, 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 protein products, in particular corn protein 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 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 plant protein product (e.g., corn 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 corn protein product comprising the steps of providing a corn protein containing material; humidifying the corn protein containing material at an elevated 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 protein product. The resulting com protein product has a reduced volatile compound content as compared to an equivalent untreated com protein product.
[0007] The present disclosure also provides a process for reducing volatile compound content of a com protein product comprising the steps of humidifying a corn 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 drying the humidified material at a drying temperature from 50 to 90°C to obtain the com protein product. The resulting com protein product has a reduced volatile compound content as compared to an equivalent untreated com protein product.
[0008] The present disclosure also provides a corn protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated corn 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 the overall flavor intensity of treated and untreated com protein isolate (CPI) 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 represented by the lighter symbols while treatment 8 is represented by the darker symbols. 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 represented by the lighter symbols while treatment 8 is represented by the darker symbols. 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 shows the response of overall flavor intensity as a function of humidificationdrying cycles.
[0014] Figure 5 shows the changes in total peak area as a function of humidification- drying cycles.
[0015] Figures 6A to 6D show the response of the detected volatile compounds, expressed in ppm, found in CPI samples to the number of humidification-drying cycles. [0016] Figures 7A to 7E show the response of the detected volatile compounds, expressed as a percentage of the initial concentration, found in CPI samples to the number of humidificationdrying cycles.
[0017] Figure 8 is a log-log plot (log2(treated/untreated) against loglO(treated)) that shows changes in concentrations of volatile compounds in the CPI samples that have undergone one (upper left), two (upper right), four (lower left), and six (lower right) humidification-drying cycles.
DETAILED DESCRIPTION
[0018] 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.
[0019] 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.
[0020] 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 .
[0021] 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.
[0022] As used herein, “room temperature” or “RT” refers to a temperature between 20°C to 25°C. [0023] 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.
[0024] Described herein is a corn protein product and a process of preparing the com protein product. The corn 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 corn protein product
[0025] The present disclosure provides a process for preparing a com protein product. The process comprises the steps of humidifying a com protein containing material at an elevated 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 protein product. The resulting corn protein product has one or more improved attributes as compared to an equivalent untreated corn protein product; preferably, the one or more improved attributes may include, but may not be limited to, a reduced volatile compound content.
[0026] As described herein, an “equivalent untreated com protein product” refers to an equivalent corn protein product that has not been subjected to any process of the instant invention as described in the present disclosure. An “equivalent corn protein product” refers to a corn protein product prepared from the same starting material used in the instant invention (e g., a com protein isolate from the same batch).
[0027] The corn protein containing material serves as a starting material to the process and may include, but may not be limited to, textured com flour, textured com protein concentrate, com protein isolate, corn protein concentrate, or any combinations thereof. In one aspect, the corn protein containing material can have a protein concentration in a range from 10 to 90 wt% on a dry basis; preferably, the corn protein containing material can have a protein concentration of at least 50 wt% on a dry basis.
[0028] In the humidifying step, the com 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.
[0029] 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.
[0030] Preferably, the atmosphere contacting the corn 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 corn 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 corn protein containing material itself.
[0031] 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%.
[0032] 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.
[0033] In one aspect, the humidifying step is carried out by passing humidified or warmed air to deliver water to the corn 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 corn protein 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.
[0034] The humidifying period for humidifying the corn 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.
[0035] The humidified material can be de-humidified in the drying step to obtain the final corn protein product. The drying step can be carried out at a drying temperature for a drying period to obtain the corn 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 corn protein product.
[0036] 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.
[0037] 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.
[0038] The relative humidity at the drying step can be 0%, from 0 to 0.5%, from 0.5% to 1%, or at least 1%. [0039] 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.
[0040] The corn protein product obtained from the process as described above has content of one or more volatile compounds reduced as compared to an equivalent untreated corn protein product. Preferably, the content of one or more volatile compounds in the corn 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 corn protein product. More preferably, the com protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated corn protein product
[0041] Preferably, the content of one or more volatile compounds in the com 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 com protein product.
Process for reducing volatile compound content of a corn protein product
[0042] The present disclosure provides a process for reducing volatile compound content of a com protein product. Preferably, off-notes of the corn protein product are reduced by the process of the instant invention.
[0043] 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.
[0044] The process comprises a step of humidifying a com 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 com protein product. The resulting corn 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 corn protein product. Preferably, the resulting com protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated com protein product; in other words, the resulting com protein product can be completely free of one or more volatile compounds.
[0045] Preferably, the com 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 corn protein product.
[0046] The corn protein containing material may include, but may not be limited to, textured corn flour, textured com protein concentrate, corn protein isolate, corn protein concentrate, or any combinations thereof. In one aspect, the corn protein containing material can have a protein content in a range from 10 to 90 wt% on a dry basis; preferably, the corn protein containing material can have a protein concentration of at least 50 wt% on a dry basis.
[0047] During the humidifying step, the com 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 corn 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.
[0048] 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 protein product.
[0049] 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.
[0050] In one aspect, no purification step may be required to separate fibers and starch out from the com 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.
[0051] 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.
Corn protein product
[0052] The com protein product of the present invention has content of one or more volatile compounds reduced as compared to an equivalent untreated com protein product. Thus, the corn 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 corn protein product described in this disclosure is reduced, preferably completely eliminated, as compared to an equivalent untreated corn protein product. Volatile compounds are substances present in a com 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.
[0053] Preferably, the volatile compounds may include, but may not be limited to, hexanal, heptanal, 2-heptanone, 2-pentyl-furan, benzaldehyde, heptenal, l-octen-3-ol, octanal, 2-octanone, 2-butyl-furan, 2-ethyl-l-hexanol, thiophene, 2-hexanol, 2-hexanone, 2-methyl-pentanal, 2- methyl-thiophene, 2-nonanone, 2-propyl-furan, 4-ethyl-benzaledhyde, 2-ethyl-pyrazine, o- tolualdehyde, or any combinations thereof.
[0054] In one aspect, the corn 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 corn protein product. Preferably, the com protein product has content of one or more volatile compounds reduced by 100% as compared to an equivalent untreated com protein product.
[0055] Preferably, the content of one or more volatile compounds in the com protein product can be reduced by a range from 20 to 95%, preferably from 55 to 95%, more preferably from 70 to 95%, as compared to an equivalent untreated corn protein product.
[0056] Preferably, the corn protein product of the present invention may be prepared by any process described in the present disclosure.
[0057] In one aspect, attributes other than the volatile compound content of the corn protein product prepared by any process of the instant invention described in the present disclosure may be improved as compared to an equivalent untreated corn protein product.
Examples
[0058] 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 1 1.1. Materials and Method
[0059] Approximately 5g samples of corn protein isolate (CPI) (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.
[0060] Initial moisture content was estimated using quadruplicate measurements with a moisture balance
Table 1
[0061] For sensory analysis, single samples of about 40g CPI 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.
[0062] 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.
[0063] 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 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 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 Discussion
1.2,1 Moisture Gain
[0064] 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 0%. In high temperatures and dry conditions, the samples lost weight.
Table 2
[0065] 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 0.95. Subsequent analyses were adjusted to a moisture-free basis using the observed moistures for individual samples.
1.2,2 Sensory Analysis
[0066] 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 CPI. 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, 3, and 8 had lower intensities. As suggested by Table 3, intermediate humidity (e.g., 75%) and temperature (e.g., 60°C) appear to be most effective in reducing flavor intensity.
Table 3
1.2.3 Untargeted GC/MS Analysis
[0067] 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.
[0068] 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.
[0069] 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.
[0070] 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 the largest number of compounds.
[0071] Figure 3 shows the comparable information for those samples that were humidified and then dried. While about 1,350 compounds were identified in the samples that were humidified but not dried, about 850 compounds were identified in the samples that were humidified and then dried.
[0072] 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.
Table 4
1.2,4 Targeted GC/FID Analysis
[0073] Treated and untreated samples collected before and after drying were analyzed for about 25 analytes using a calibrated GC/FID method. Not all compounds in the calibration set appear in the samples.
[0074] A study on the distribution of calibrated compounds in the untreated samples shows that about 85% of the mass of these compounds are associated with hexanal, 2-pentyl furan, benzaldehyde, and 2-m ethylbutanol. 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.
[0075] 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.
[0076] 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% for samples undergoing only humidification (humidified-only samples) and samples undergoing both humidification and drying (humidified and dried samples). Some treatments decreased concentrations of some compounds by more than 95%. Drying clearly had a benefit for decreasing volatile compounds such as benzaldehyde, l-octen-3-ol, and 2-octanone. Except for o-tolualdehyde, high humidity tends to decrease concentrations of volatile compounds. [0077] Table 5 summarizes the effect of different treatment conditions on the number of compounds that have changed significantly in concentration. Columns 1 to 3 represent number of compounds having significant changes in concentration between untreated samples and humidified-only samples, between untreated samples and humidified and dried samples, and between humidified-only samples and humidified and dried samples, respectively. Except for treatment condition 1 (30°C, 100% relative humidity, and 30 min), half or more of the compounds measured showed a significant change as compared to the untreated (which was assumed to be invariant) before drying (column 1) and after (column 2) drying. Many compounds changed significantly in concentration with drying (column 3) as compared to those before drying.
Table 5
1.2.5 Conclusion
[0078] The following observations can be drawn from the above studies:
[0079] - Exposure of corn protein to high humidifying temperature and relative humidity can significantly decrease the overall flavor intensity.
[0080] - The decline in flavor intensity may not be readily related to a change in any single volatile compound but a combination of volatile compounds.
[0081] - A large number of volatile compounds decreased in concentration as indicated by untargeted GC/MS. A relatively small number of compounds increased in concentration.
[0082] - The concentration of the most quantitated compounds (from GC/FID analysis using quantitative standards) were negatively correlated with the amount of moisture adsorbed during the humidification.
[0083] - Most compounds tracked in quantitative analysis showed sensitivity to conditions during humidification Generally, high relative humidity favored decreased concentrations, before and after drying.
Example 2
2.1 Materials and Method
[0084] Samples of corn protein isolate (CPI) (Cargill Incorporated) were weighed out. Duplicate samples of about 70g were prepared for ultimate sensory analysis. Triplicate samples of about 5g were prepared for chemical analysis. Samples were weighed into pre-weighed aluminum pans suitable for the sample weight.
[0085] For a treatment, the five samples were placed into the Unox Combi oven for both humidification and drying. One cycle consisted of a humidifying step of 60 minutes at 70°C and 100% relative humidity, followed by a drying step of 20 minutes at 80°C and 0% relative humidity. The oven was programmed for 1, 2, 4, or 6 repetitions of this cycle. Samples were reweighed at the end of the final cycle.
[0086] A preliminary experiment was conducted in which triplicate samples of about 5g were taken through one cycle at a time but were reweighed at each condition change. Only the weight change associated with water gain or loss was recorded. This was used to establish the response of sample weight to humidity cycling at a more granular level. [0087] For sensory analysis, single samples of about 40g CPI were placed in larger aluminum pans and exposed to the same humidification and drying treatment conditions in each cycle as described above.
[0088] 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.
[0089] The panel was then given three blind samples (concentrations of 0.5%, 2.5%, and 4%) as a validation testing to ensure the panel was aligned and could reproduce their data, they 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 is an overall flavor intensity value. The response curve can be used to compute an apparent 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.
2.2 Results and Discussion
2,2,1 Moisture Change
[0090] Rapid moisture uptake was observed in the first 60 minutes followed by a slower absorption in subsequent cycles. The estimated maximum moisture fraction was near 0.23.
[0091] Repeated humidification-drying steps under the treatment conditions used here resulted in a small but significant decrease (p<0.05) in maximum moisture content across cycles. During drying, the first and second cycles of drying do not seem to have an impact, but lower moistures are observed after 3 or 4 cycles.
[0092] The mean moisture values at the end of each step in each cycle were shown in Table 6.
Table 6
2,2.2 Sensory Analysis
[0093] The panel successfully placed blind references at the appropriate intensity relative to the established scale. 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.
[0094] Humidification and drying decreased the overall flavor intensity of the samples as shown in Table 7, which includes the measured specific flavor intensities and their computed equivalent concentrations. There was about an 83% decrease in the equivalent concentration after the first two cycles.
Table 7
[0095] Figure 4 shows that two cycles of humidification-drying lead to a lower overall intensity than one cycle, but that additional cycles beyond the second cycle either have minimal benefit or a detrimental effect on the overall intensity as measured by intensity scores.
2,2,3 Volatile Concentration [0096] The quantitative method assesses the concentrations of twenty-eight compounds, but many more are detected without identification. As an indicator of overall change, the total peak area can be summed for each sample. The results are shown in Figure 5. The first cycle of humidificationdrying causes a 40 to 60% decline and the second cycle causes a smaller decline. Subsequent cycles seem to have little effect. This pattern generally matched the changes in sensory intensity observed in Figure 4
[0097] Nineteen of the twenty-eight identified compounds were detected in the untreated samples. While the overall trend showed a smooth exponential decay, individual compounds showed a range of responses to repeated exposure to drying at high relative humidity. Treatment of humidification and drying generally decreased the concentrations of the identified volatile compounds (Figures 6A to 6D). 2,4-decadienal (Figure 6D) showed increases in concentrations.
[0098] Because the detected compounds have different starting concentrations, it is clearer to demonstrate the effect of treatment conditions when the data is expressed as a percentage of the initial concentrations of the respective compounds (Figures 7A to 7E). Some compounds show almost no decline after the first cycle (e g., 2-pentylfuran), while some compounds show decreases with each additional cycle (e.g., l-octene-3-ol). It may be suggested that additional cycles of humidification-drying could continue to decrease the overall concentrations of volatile compounds; however, the overall sensory response may not be changed.
[0099] In general, it is observed that the following volatile compounds showed decreases in concentration after the first cycle of humidification-drying: hexanal, heptanal, 2-heptanone, 2- pentyl-furan, benzaldehyde, heptenal, l-octen-3-ol, octanal, 2-octanone, 2-butyl-furan, 2-ethyl-l- hexanol, thiophene, 2-hexanol, 2-hexanone, 2-methyl-pentanal, 2-methyl-thiophene, 2-nonanone, 2-propyl-furan, 4-ethyl-benzaledhyde, 2-ethyl-pyrazine, and o-tolualdehyde. Table 8 summaries the percentage reduction of these volatile compounds after the different treatment cycles.
Table 8
[0100] Concentrations of many of the detected compounds measured in the samples can be correlated with the observed flavor intensity. As shown in Table 9, a “+” sign indicates a positive correlation between the compound and the flavor intensity of the protein material, while a sign indicates a negative correlation. A “n/a” sign indicates that the corresponding compound has neither a positive nor negative correlation.
Table 9
[0101] In short, concentrations of certain volatile compounds can be reduced by humidificationdrying treatment as observed in Figures 7A to 7E, while Table 8 provides a linkage between concentration changes of such volatile compounds and changes in flavor intensity of the treated samples. For example, decreases in concentrations of some volatile compound concentration may correlate to decreases in overall flavor intensity.
2,2.4 Untargeted Volatile Analysis
[0102] As shown in Table 10, many of the volatile compounds detected were not influenced by the treatment at all, though subsequent treatments decreased the number of compounds unaffected. As indicated in Figure 4, the overall sensory intensity plateaus after two cycles of humidificationdrying. One of the possible explanations is that the changes in concentration seen with more than two cycles of humidification-drying occur in compounds that do not contribute to the sensory experience. These data may also suggest that some of the compounds that increase in the early cycles of treatment are transient; they disappear on further treatment.
Table 10
[0103] The first cycle of humidification-drying influenced the total volatiles as shown in Figure 8. The number of compounds influenced increased with subsequent cycles of treatment. Most of the change in apparent concentration after two cycles of treatment occurred in those compounds that were at “medium” initial concentration. 2,2,5 Conclusion
[0104] The following observations can be drawn from the above studies:
[0105] - Repeated cycles of humidification- drying decreased overall flavor intensity, but the effect of additional treatment cycles decreased after two cycles.
[0106] - Most of the detected compounds decreased through multiple cycles of treatment.
[0107] - Untargeted analysis showed strongly that the greatest declines in concentration occurred in the most prevalent compounds. Overall, repeated treatment increased the number of compounds affected and the degree of effect The compounds that increase in concentration were prominent among those compounds initially in low concentration and repeated treatments seemed to decrease the concentration of some of these compounds.
[0108] - Though multiple cycles of humidification- drying seemed to decrease the concentrations of an increasing number of compounds, some compounds remained near their original concentrations than change at least two-fold. In contrast, after the second cycle of humidificationdrying, 50% more compounds decreased in concentration at least two-fold as have remained unchanged or increased.
Clauses describing the invention
[0109] Clause 1. A process for preparing a corn protein product, comprising the steps of: a. providing a corn protein containing material; b. humidifying the corn 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 com protein product; wherein the com protein product has a reduced volatile compound content as compared to an equivalent untreated corn protein product.
[0110] Clause 2. The process of clause 1, wherein the com protein containing material is selected from the group consisting of textured corn flour, textured corn protein concentrate, com protein isolate, com protein concentrate, and any combinations thereof.
[oni] Clause 3. The process of any of the preceding clauses, wherein the relative humidity in the humidifying step is in a range from 50 to 100%.
[0112] Clause 4. The process of any of the preceding clauses, wherein the humidifying temperature is in a range from 55 to 95°C.
[0113] Clause 5. The process of any of the preceding clauses, wherein the humidifying temperature is less than 100°C. [0114] Clause 6. The process of any of the preceding clauses, wherein the corn 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
[0115] Clause 7. 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.
[0116] Clause 8. The process of any of the preceding clauses, wherein water is uniformly delivered and distributed over the com protein containing material in the humidifying step.
[0117] Clause 9. 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.
[0118] Clause 10. The process of any of the preceding clauses, water delivered in the humidifying step is not in a form of steam.
[0119] Clause 11. 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.
[0120] Clause 12. 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.
[0121] Clause 13. 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.
[0122] Clause 14. A process for reducing volatile compound content of a corn protein product, comprising the steps of: a. humidifying a com 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 corn protein product; wherein the com protein product has a reduced volatile compound content as compared to an equivalent untreated corn protein product.
[0123] Clause 15. A process for reducing volatile compound content of a corn protein product, consisting of the steps of: a. humidifying a com 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 corn protein product; wherein the com protein product has a reduced volatile compound content as compared to an equivalent untreated corn protein product.
[0124] Clause 16 The process of any of clauses 14 to 15, wherein the com protein containing material is selected from the group consisting of textured corn flour, textured corn protein concentrate, com protein isolate, com protein concentrate, and any combinations thereof.
[0125] Clause 17. The process of any of clauses 14 to 16, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.
[0126] Clause 18. The process of any of the clauses 14 to 17, wherein the com 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.
[0127] Clause 19. The process of any of the clauses 14 to 18, 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.
[0128] Clause 20. The process of any of clauses 14 to 19, wherein water is uniformly delivered and distributed over the corn protein containing material in the humidifying step.
[0129] Clause 21. The process of any of clauses 14 to 20, water delivered in the humidifying step is in a form of a liquid water or a vapor.
[0130] Clause 22. The process of any of clauses 14 to 21, water delivered in the humidifying step is not in a form of steam.
[0131] Clause 23. The process of any of clauses 14 to 22, wherein the humidified material is dried at a drying temperature in a range from 50 to 90°C.
[0132] Clause 24. The process of any of clauses 14 to 23, 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. [0133] Clause 25. The process of any of clauses 14 to 24, 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.
[0134] Clause 26. The process of any of the preceding clauses, wherein the com 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 soy protein product.
[0135] Clause 27. A corn protein product prepared by the process of any of the preceding clauses. [0136] Clause 28. A com protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated com protein product. [0137] Clause 29. The corn protein product of any of clauses 27 to 28, 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 corn protein product.
[0138] Clause 30. The corn protein product of any of clauses 27 to 29, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, ketone, furan, alcohol, and pyrazine.
[0139] Clause 31. The corn protein product of any of clauses 27 to 30, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, 2-heptanone, 2- pentyl-furan, benzaldehyde, heptenal, l-octen-3-ol, octanal, 2-octanone, 2-butyl-furan, 2-ethyl-l- hexanol, thiophene, 2-hexanol, 2-hexanone, 2-methyl-pentanal, 2-methyl-thiophene, 2-nonanone, 2-propyl-furan, 4-ethyl-benzaledhyde, 2-ethyl-pyrazine, o-tolualdehyde, and any combinations thereof.
[0140] Clause 32. The corn protein product of any of clauses 27 to 31, having content of hexanal reduced by a range from 30 to 99%, from 40 to 98%, or from 50 to 95% as compared to an equivalent untreated corn protein product.
[0141] Clause 33. The corn protein product of any of clauses 27 to 32, having content of hexanal reduced by at least 50%, at least 80%, at least 85%, or at least 90% as compared to an equivalent untreated com protein product.
[0142] Clause 34. The corn protein product of any of clauses 27 to 33, having content of hexanal reduced by at least 50% after one cycle of humidifying step and the drying step, at least 80% after two cycles of humidifying step and the drying step, at least 85% after four cycles of humidifying step and the drying step, or at least 90% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.
[0143] Clause 35. The corn protein product of any of clauses 27 to 34, having content of heptanal reduced by a range from 40 to 99%, from 50 to 95%, or from 60 to 90% as compared to an equivalent untreated corn protein product.
[0144] Clause 36. The corn protein product of any of clauses 27 to 35, having content of heptanal reduced by at least 60%, at least 75%, at least 80%, or at least 85% as compared to an equivalent untreated com protein product.
[0145] Clause 37. The corn protein product of any of clauses 27 to 36, having content of heptanal reduced by at least 60% after one cycle of humidifying step and the drying step, at least 75% after two cycles of humidifying step and the drying step, at least 80% after four cycles of humidifying step and the drying step, or at least 85% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product. [0146] Clause 38. The corn protein product of any of clauses 27 to 37, having content of 2- heptanone reduced by a range from 60 to 99%, from 70 to 98%, or from 80 to 95% as compared to an equivalent untreated corn protein product.
[0147] Clause 39. The corn protein product of any of clauses 27 to 38, having content of 2- heptanone reduced by at least 80%, at least 85%, or at least 90% as compared to an equivalent untreated com protein product.
[0148] Clause 40. The corn protein product of any of clauses 27 to 39, having content of 2- heptanone reduced by at least 80% after one cycle of humidifying step and the drying step, at least 90% after two cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.
[0149] Clause 41. The com protein product of any of clauses 27 to 40, having content of 2-pentyl- furan reduced by a range from 80 to 99%, from 85 to 98%, or from 90 to 97% as compared to an equivalent untreated corn protein product.
[0150] Clause 42. The com protein product of any of clauses 27 to 41, having content of 2-pentyl- furan reduced by at least 90%, at least 95%, or at least 96% as compared to an equivalent untreated corn protein product.
[0151] Clause 43. The com protein product of any of clauses 27 to 42, having content of 2-pentyl- furan reduced by at least 90% after one cycle of humidifying step and the drying step, at least 95% after two cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.
[0152] Clause 44. The corn protein product of any of clauses 27 to 43, having content of benzaldehyde reduced by a range from 15 to 90%, from 25 to 80%, or from 35 to 70% as compared to an equivalent untreated corn protein product.
[0153] Clause 45. The corn protein product of any of clauses 27 to 44, having content of benzaldehyde reduced by at least 35%, at least 50%, at least 60%, or at least 65% as compared to an equivalent untreated corn protein product.
[0154] Clause 46. The corn protein product of any of clauses 27 to 45, having content of benzaldehyde reduced by at least 35% after one cycle of humidifying step and the drying step, at least 50% after two cycles of humidifying step and the drying step, at least 60% after four cycles of humidifying step and the drying step, or at least 65% after six cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.
[0155] Clause 47. The corn protein product of any of clauses 27 to 46, having content of heptenal reduced by a range from 25 to 75%, from 35 to 65%, or from 45 to 55% as compared to an equivalent untreated corn protein product. [0156] Clause 48. The corn protein product of any of clauses 27 to 47, having content of heptenal reduced by at least 35%, at least 40%, at least 50%, or at least 55% as compared to an equivalent untreated com protein product.
[0157] Clause 49. The corn protein product of any of clauses 27 to 48, having content of heptenal reduced by at least 35% after one cycle of humidifying step and the drying step, at least 40% after two cycles of humidifying step and the drying step, at least 50% after four cycles of humidifying step and the drying step, or at least 55% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.
[0158] Clause 50. The corn protein product of any of clauses 27 to 49, having content of 1-octen- 3-ol reduced by a range from 15 to 99% or from 20 to 98% as compared to an equivalent untreated corn protein product.
[0159] Clause 51. The corn protein product of any of clauses 27 to 50, having content of 1-octen- 3-ol reduced by at least 20%, at least 70%, at least 90%, or at least 95% as compared to an equivalent untreated corn protein product.
[0160] Clause 52. The corn protein product of any of clauses 27 to 51, having content of 1-octen- 3-ol reduced by at least 20% after one cycle of humidifying step and the drying step, at least 70% after two cycles of humidifying step and the drying step, at least 90% after four cycles of humidifying step and the drying step, or at least 95% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.
[0161] Clause 53. The corn protein product of any of clauses 27 to 52, having content of octanal reduced by a range from 15 to 85%, from 20 to 80%, or from 25 to 75% as compared to an equivalent untreated corn protein product.
[0162] Clause 54. The corn protein product of any of clauses 27 to 53, having content of octanal reduced by at least 25%, at least 50%, at least 70%, or at least 75% as compared to an equivalent untreated com protein product.
[0163] Clause 55. The corn protein product of any of clauses 27 to 54, having content of octanal reduced by at least 25% after one cycle of humidifying step and the drying step, at least 50% after two cycles of humidifying step and the drying step, at least 70% after four cycles of humidifying step and the drying step, or at least 75% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.
[0164] Clause 56. The corn protein product of any of clauses 27 to 55, having content of 2- octanone reduced by a range from 60 to 99%, from 70 to 95%, or from 80 to 90% as compared to an equivalent untreated corn protein product. [0165] Clause 57. The corn protein product of any of clauses 27 to 56, having content of 2- octanone reduced by at least 70%, at least 75%, at least 80%, or at least 85% as compared to an equivalent untreated corn protein product.
[0166] Clause 58. The corn protein product of any of clauses 27 to 57, having content of 2- octanone reduced by at least 80% after one cycle of humidifying step and the drying step or at least 85% after two cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.
[0167] Clause 59. The corn protein product of any of clauses 27 to 58, having content of thiophene reduced by a range from 80 to 99%, from 90 to 99%, or from 95 to 99% as compared to an equivalent untreated corn protein product.
[0168] Clause 60. The corn protein product of any of clauses 27 to 59, having content of thiophene reduced by at least 85%, at least 90%, at least 95%, or at least 99% as compared to an equivalent untreated com protein product.
[0169] Clause 61. The corn protein product of any of clauses 27 to 60, having content of thiophene reduced by at least 95% after one cycle of humidifying step and the drying step, at least 98% after two cycles of humidifying step and the drying step, or at least 99% after six cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.
[0170] Clause 62. The com protein product of any of clauses 27 to 61, having content of 2-hexanol reduced by a range from 45 to 99%, from 55 to 90%, or from 65 to 80% as compared to an equivalent untreated corn protein product.
[0171] Clause 63. The com protein product of any of clauses 27 to 62, having content of 2-hexanol reduced by at least 60%, at least 65%, at least 70%, or at least 75% as compared to an equivalent untreated com protein product.
[0172] Clause 64. The com protein product of any of clauses 27 to 63, having content of 2-hexanol reduced by at least 60% after one cycle of humidifying step and the drying step, at least 65% after two cycles of humidifying step and the drying step, or at least 75% after six cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.
[0173] Clause 65. The corn protein product of any of clauses 27 to 64, having content of 2- nonanone reduced by a range from 50 to 99%, from 55 to 95%, or from 60 to 90% as compared to an equivalent untreated corn protein product.
[0174] Clause 66. The corn protein product of any of clauses 27 to 65, having content of 2- nonanone reduced by at least 50%, at least 60%, at least 80%, or at least 85% as compared to an equivalent untreated corn protein product.
[0175] Clause 67. The corn protein product of any of clauses 27 to 66, having content of 2- nonanone reduced by at least 60% after two cycles of humidifying step and the drying step, at least 80% after four cycles of humidifying step and the drying step, or at least 85% after six cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product
[0176] Clause 68. The corn protein product of any of clauses 27 to 67, having content of o- tolualdehyde reduced by a range from 15 to 99%, from 20 to 95%, or from 25 to 90% as compared to an equivalent untreated corn protein product.
[0177] Clause 69. The corn protein product of any of clauses 27 to 68, having content of o- tolualdehyde reduced by at least 25%, at least 50%, at least 70%, or at least 80% as compared to an equivalent untreated corn protein product.
[0178] Clause 70. The corn protein product of any of clauses 27 to 69, having content of o- tolualdehyde reduced by at least 25% after one cycle of humidifying step and the drying step, at least 50% after two cycles of humidifying step and the drying step, at least 70% after four cycles of humidifying step and the drying step, or at least 80% after six cycles of humidifying step and the drying step as compared to an equivalent untreated com protein product.
[0179] Clause 71. The corn protein product of any of clauses 27 to 70, having content of 2-ethyl- 1 -hexanol reduced by a range from 20 to 99%, from 25 to 95%, or from 30 to 90% as compared to an equivalent untreated corn protein product.
[0180] Clause 72. The corn protein product of any of clauses 27 to 71, having content of 2-ethyl- 1-hexanol reduced by at least 30%, at least 75%, at least 80%, or at least 85% as compared to an equivalent untreated corn protein product.
[0181] Clause 73. The corn protein product of any of clauses 27 to 72, having content of 2-ethyl- 1 -hexanol reduced by at least 30% after one cycle of humidifying step and the drying step, at least 80% after two cycles of humidifying step and the drying step, or at least 85% after four cycles of humidifying step and the drying step as compared to an equivalent untreated corn protein product.

Claims

CLAIMS What is claimed is:
1. A process for preparing a corn protein product, comprising the steps of: a. providing a com protein containing material; b. humidifying the com protein containing material at an elevated 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 com protein product; wherein the corn protein product has a reduced volatile compound content as compared to an equivalent untreated com protein product.
2. The process of claim 1, wherein the com protein containing material is selected from the group consisting of textured corn flour, textured corn protein concentrate, corn protein isolate, com protein concentrate, and any combinations thereof.
3. The process of any of the preceding claims, wherein the relative humidity in the humidifying step is in a range from 50 to 100%.
4. The process of any of the preceding claims, wherein the humidifying temperature is in a range from 55 to 95°C.
5. The process of any of the preceding claims, wherein the com 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.
6. 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.
7. 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.
8. 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.
9. A process for reducing volatile compound content of a corn protein product, comprising the steps of: a. humidifying a com 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 corn protein product; wherein the corn protein product has a reduced volatile compound content as compared to an equivalent untreated com protein product.
10. The process of claim 9, wherein the com protein containing material is selected from the group consisting of textured corn flour, textured corn protein concentrate, corn protein isolate, com protein concentrate, and any combinations thereof.
11. The process of any of claims 9 to 10, wherein the humidifying step is performed at a humidifying temperature in a range from 55 to 95°C.
12. The process of any of claims 9 to 11, wherein the com 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 com protein product.
13. The process of any of claims 9 to 12, 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.
14. A com protein product prepared by the process of any of the preceding claims.
15. A com protein product having content of one or more volatile compounds reduced as compared to an equivalent untreated com protein product.
16. The corn protein product of any of claims 14 to 15, 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 com protein product.
17. The corn protein product of any of claims 14 to 16, wherein the one or more volatile compounds are selected from the group consisting of aldehyde, ketone, furan, alcohol, and pyrazine.
18. The corn protein product of any of claims 14 to 17, wherein the one or more volatile compounds are selected from the group consisting of hexanal, heptanal, 2-heptanone, 2- pentyl-furan, benzaldehyde, heptenal, l-octen-3-ol, octanal, 2-octanone, 2 -butyl -furan, 2- ethyl-1 -hexanol, thiophene, 2-hexanol, 2-hexanone, 2-methyl-pentanal, 2-m ethyl -thiophene, 2-nonanone, 2-propyl -furan, 4-ethyl-benzaledhyde, 2-ethyl-pyrazine, o-tolualdehyde, and any combinations thereof.
PCT/US2025/022530 2024-04-02 2025-04-01 Corn protein product and process of preparing the same Pending WO2025212640A1 (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007149089A1 (en) * 2006-06-21 2007-12-27 Solae, Llc Bland tasting soy protein isolate
CN101390564B (en) * 2007-09-18 2011-01-26 中国食品发酵工业研究院 A kind of production method of corn protein isolate
WO2019006286A1 (en) * 2017-06-30 2019-01-03 Kellogg Company Deflavored pea composition
CN114732079A (en) * 2020-12-24 2022-07-12 丰益(上海)生物技术研发中心有限公司 A kind of preparation method of vegetable protein powder with clean flavor
WO2023062035A1 (en) * 2021-10-11 2023-04-20 Nub Technologies Ltd Process for treating plant and/or raw food material
CN116669572A (en) * 2020-10-20 2023-08-29 皆食得公司 heat-treated soy flour

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2007149089A1 (en) * 2006-06-21 2007-12-27 Solae, Llc Bland tasting soy protein isolate
CN101390564B (en) * 2007-09-18 2011-01-26 中国食品发酵工业研究院 A kind of production method of corn protein isolate
WO2019006286A1 (en) * 2017-06-30 2019-01-03 Kellogg Company Deflavored pea composition
CN116669572A (en) * 2020-10-20 2023-08-29 皆食得公司 heat-treated soy flour
CN114732079A (en) * 2020-12-24 2022-07-12 丰益(上海)生物技术研发中心有限公司 A kind of preparation method of vegetable protein powder with clean flavor
WO2023062035A1 (en) * 2021-10-11 2023-04-20 Nub Technologies Ltd Process for treating plant and/or raw food material

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