A method of extracting oat protein, products thereof and use in hair care products

Abstract

This invention provides a method for extracting oat protein, belonging to the field of active ingredient extraction technology. The extraction method includes the following steps: (1) preparing oat powder; (2) adding oat powder to a solvent and heating for extraction, centrifuging to collect the supernatant, precipitating, allowing to stand, washing, and drying to obtain the oat protein. This invention uses a mixture of proline, betaine, and glycerol as a eutectic solvent, and controls the molar ratio of the three to be 1-3:1:4-6. Through the interaction of hydrogen bonds and coordinating components in the system, the extraction and separation of organic matter are achieved, resulting in high extraction efficiency, preservation of protein activity, and a green and environmentally friendly effect.

Description

Technical Field

[0001] This invention belongs to the field of active ingredient extraction technology, specifically relating to a method for extracting oat protein, a product thereof, and its application in hair care products. Background Technology

[0002] Oats are herbaceous crops belonging to the genus Avena of the family Poaceae. They are rich in nutrients such as protein, fat, and β-glucan. Oat protein is a high-quality plant-based protein with a reasonable amino acid composition and ratio, and it has excellent physiological functions and activities.

[0003] Proteins can be extracted by enriching or separating them from raw materials. Commonly used methods include alkali-soluble acid precipitation, enzymatic hydrolysis, and ultrasonic extraction. For oat protein extraction, alkali-soluble acid precipitation is the most common method. However, the alkali concentration cannot be too high during extraction; pH control is crucial. Otherwise, lysine and cysteine ​​or alanine may undergo unfavorable condensation reactions, generating harmful substances and further leading to protein nutrient loss. Enzymatic hydrolysis offers advantages such as milder reaction conditions, easier control of the solid-liquid ratio, and a high extraction rate of short peptide chains. It also effectively reduces the loss of nutritional value. However, excessive enzymatic hydrolysis can lead to a reduction or permanent loss of some functional properties of the protein. Ultrasonic extraction, due to its volume-enhancing effect, allows for a reduction in alkali concentration to avoid protein degradation. However, the process is more complex.

[0004] Chinese patent CN118852322A discloses a method for efficient extraction of oat protein based on a eutectic system. The method includes the following steps: (1) preparing oat powder; (2) mixing hydrogen bond acceptors and hydrogen bond donors with oat powder to form a eutectic system (DESys) for extraction; (3) centrifuging to obtain a supernatant; (4) adding 50.0 mL of deionized water and storing at 2.0-6.0 °C for 15-20 hours to allow protein precipitation; (5) centrifuging to obtain the lower protein layer; (6) adding 50.0 mL of water to the protein and washing at 50.0-80.0 °C for 1-3 hours to remove residual hydrogen bond acceptors and hydrogen bond donors; (7) centrifuging to obtain the lower protein layer; (8) titrating the washed solution with silver nitrate until no precipitate is produced; (9) freeze-drying the oat protein (OP). This invention aims to develop a green and efficient method for extracting oat protein, minimizing the impact on the environment, and promoting the application of eutectic systems in the extraction of biomacromolecules.

[0005] Chinese patent CN119119170A discloses a method for extracting oat bran protein. The method involves mixing HBD and HBA in different molar ratios and magnetically stirring until a clear, transparent liquid is formed. Oatmeal is washed with deionized water, dried at 40°C to a moisture content of 10%, pulverized, and passed through a 60-mesh sieve. The residue passing through the 60-mesh sieve is taken as oat bran. Oat bran is mixed with n-hexane (g / ml) at a 1:5 ratio and magnetically stirred at 600 rpm for 3 hours at room temperature. The mixture is then centrifuged at 4000 rpm for 10 minutes, defatted, and repeated three times. The mixture is then allowed to evaporate naturally and air-dried to obtain defatted oat bran. The defatted oat bran is vortexed with a DES solution at a solid-liquid ratio of 1:10 and stirred at 600 rpm for 60 minutes at 50°C. After cooling to room temperature, the mixture is centrifuged at 3500 rpm for 10 minutes. The supernatant is collected, and the precipitate is extracted twice more with fresh DES using the same extraction process. The resulting supernatants are combined and placed in a dialysis bag. The molecular weight cutoff is 3500D. Dialyze at 4°C for about 3 days, then freeze-dry the resulting suspension to obtain crude protein powder.

[0006] The aforementioned existing technologies all use deep eutectic solvents (DES) to extract and separate organic substances through the interaction of hydrogen bonds and coordinating components in the system. Although deep eutectic solvents have the advantages of being green and environmentally friendly and maintaining protein activity, the extraction rate is significantly lower than that of the alkali dissolution and acid precipitation method.

[0007] Therefore, it is necessary to develop an oat protein extraction method that is highly efficient, can maintain protein activity, and is environmentally friendly. Summary of the Invention

[0008] Based on the shortcomings of existing technologies, this invention aims to provide a method for extracting oat protein that is highly efficient, maintains protein activity, and is environmentally friendly. The oat protein obtained by this method can be used to prepare hair care products, which can make hair stronger, improve hair shine, and have a good repairing effect on scalp hair follicles.

[0009] To achieve the above objectives, the present invention adopts the following technical solution:

[0010] On one hand, the present invention provides a method for extracting oat protein, comprising the following steps:

[0011] (1) Preparation of oat powder: Grind oat flakes to 100-120 mesh to obtain oat powder;

[0012] (2) Take the oat powder from step (1) and add it to the solvent for heating and extraction. Centrifuge to obtain the supernatant, precipitate, stand, wash and dry to obtain the oat protein.

[0013] The solvent is a eutectic solvent composed of proline, betaine and glycerol, with a molar ratio of 1-3:1:4-6; preferably 2:1:5.

[0014] The solvent is prepared by:

[0015] Weigh proline, glycerol, and betaine, mix them in proportion, and rotary evaporate them at 80°C to obtain a stable and transparent liquid, which is the desired solvent.

[0016] The heating extraction is a water bath extraction, with the water bath temperature being 60-80℃; preferably 75℃.

[0017] The heating extraction time is 2-3 hours; preferably 2 hours.

[0018] The ratio of oat powder to solvent is 1g:3-8mL; preferably 1g:5mL.

[0019] The above-mentioned heating extraction operation also includes ultrasonic extraction; the power of the ultrasound is 150-200W; preferably 160-180W; and even more preferably 160W.

[0020] As a preferred embodiment, the heating extraction is performed as follows: first, water bath extraction for 20 minutes, then sonication for 10 minutes, then water bath heating for 20 minutes, then sonication for 10 minutes, repeating 2-3 times.

[0021] Since eutectic solvents are solvents with relatively high viscosity, the viscosity of the solvent will affect the extraction efficiency of the target product when extracting active ingredients. Therefore, the extraction efficiency can be improved by adjusting the viscosity of the eutectic solvent. In the implementation of this invention, water is added to the solvent to reduce the viscosity of the solvent.

[0022] In some preferred embodiments, the solvent further contains 3-6% water; preferably 5.2%.

[0023] During the implementation of this invention, it was found that when the water content is less than 3%, the viscosity of the eutectic solvent cannot be improved well, thus failing to achieve the goal of improving extraction efficiency; when the water content is higher than 6%, on the one hand, it will destroy the hydrogen bond interaction in the eutectic solvent, and on the other hand, it will affect the solubility of proteins in the solvent, thus failing to achieve the goal of improving extraction efficiency.

[0024] The precipitation is achieved by adding deionized water to the supernatant, wherein the volume ratio of deionized water to supernatant is 4-5:1; preferably 5:1.

[0025] The settling temperature is room temperature, and the time is 20-24 hours.

[0026] The washing process involves using deionized water at a temperature of 50-70℃ for 1-2 hours.

[0027] On the other hand, the present invention also provides an oat protein prepared by the above preparation method.

[0028] Furthermore, the present invention also provides the application of oat protein prepared by the above preparation method in the preparation of cosmetic raw materials or cosmetics, wherein the cosmetic is a hair care product.

[0029] The hair care product mentioned is shampoo or conditioner.

[0030] In another aspect, the present invention also provides a hair care product comprising oat protein prepared by the above method, a moisturizer, a skin conditioning agent, a preservative, and water; wherein the moisturizer is glycerin; the skin conditioning agent is hydroxypropyl guar gum hydroxypropyltrimethylammonium chloride; and the preservative is ethylhexylglycerin and phenoxyethanol.

[0031] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0032] (1) In the implementation of this invention, a mixture of proline, betaine and glycerol is used as a eutectic solvent and the molar ratio of the three is controlled to be 1-3:1:4-6. Through the interaction of hydrogen bonds and coordinating components in the system, the extraction and separation of organic substances are realized. However, it was found that the eutectic solvent is a solvent with relatively high viscosity during the extraction process. When extracting the effective components, the viscosity of the solvent will affect the extraction efficiency of the target product. Therefore, in order to improve the extraction efficiency of oat protein, this invention reduces the viscosity of the solvent by adding water during the implementation process.

[0033] (2) In the process of implementation, it was found that adding a certain amount of water to the solvent can improve the extraction efficiency of oat protein. The water content is 3-6%. It was also found that when the water content is less than 3%, the viscosity of the eutectic solvent cannot be improved well, so the purpose of improving the extraction efficiency cannot be achieved. When the water content is higher than 6%, on the one hand, it will destroy the interaction of hydrogen bonds in the eutectic solvent, and on the other hand, it will affect the dissolution of protein in the solvent, so the purpose of improving the extraction efficiency cannot be achieved.

[0034] (3) The present invention uses a process of eutectic solvent + ultrasonic extraction, which not only maintains the activity of protein, but also increases the extraction efficiency of protein, so that the obtained oat protein can be used to prepare hair care products, which can make hair strong, improve the luster of hair, and have a good repair effect on scalp hair follicles. Detailed Implementation

[0035] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the tables in the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0036] The following examples and comparative examples of the present invention are shown to provide a more detailed description of the compositions of the present invention, but the present invention is not limited thereto.

[0037] The present invention does not limit the source of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are all commercially available products in this technical field.

[0038] Example 1: A method for extracting oat protein

[0039] Includes the following steps:

[0040] (1) Preparation of oat powder: Grind oat flakes to 100-120 mesh to obtain oat powder;

[0041] (2) Take 10g of oat powder from step (1) and add it to 50mL of a mixed solvent containing 5.2% water and a molar ratio of 2:1:5 of proline, betaine and glycerol. Heat and extract, centrifuge and take the supernatant. Add deionized water to the supernatant (the volume ratio of deionized water to supernatant is 5:1), let stand for 20h, wash with deionized water at a temperature of 60℃ for 1.5h, freeze dry to obtain the oat protein.

[0042] The heating extraction process is as follows: first, extract in a 75°C water bath for 20 minutes, then maintain the temperature at 160W and sonicate for 10 minutes, then heat in a 75°C water bath for 20 minutes, then maintain the temperature at 160W and sonicate for 10 minutes, repeating this process twice.

[0043] Example 2: A method for extracting oat protein

[0044] Includes the following steps:

[0045] (1) Preparation of oat powder: Grind oat flakes to 100-120 mesh to obtain oat powder;

[0046] (2) Take 10g of oat powder from step (1) and add it to 30mL of a mixed solvent containing 3% water and a molar ratio of 1:1:4 of proline, betaine and glycerol. Heat and extract, centrifuge and take the supernatant. Add deionized water to the supernatant (the volume ratio of deionized water to supernatant is 4:1), let stand for 24h, wash with deionized water at a temperature of 50℃ for 2h, freeze dry to obtain the oat protein.

[0047] The heating extraction process is as follows: first, extract in a 60°C water bath for 20 minutes, then maintain the temperature at 200W and sonicate for 10 minutes, then heat in a 60°C water bath for 20 minutes, then maintain the temperature at 200W and sonicate for 10 minutes, repeating this process twice.

[0048] Example 3: A method for extracting oat protein

[0049] Includes the following steps:

[0050] (1) Preparation of oat powder: Grind oat flakes to 100-120 mesh to obtain oat powder;

[0051] (2) Take 10g of oat powder from step (1) and add it to 80mL of a mixed solvent containing 6% water and a molar ratio of 1:1:2 of proline, betaine and glycerol. Heat and extract, centrifuge and take the supernatant. Add deionized water to the supernatant (the volume ratio of deionized water to supernatant is 6:1), let stand for 20h, wash with deionized water at a temperature of 70℃ for 1h, freeze dry to obtain the oat protein.

[0052] The heating extraction process is as follows: first, extract in an 80°C water bath for 20 minutes, then maintain the temperature at 150W and sonicate for 10 minutes, then heat in an 80°C water bath for 20 minutes, then maintain the temperature at 150W and sonicate for 10 minutes, repeating this process twice.

[0053] Comparative Example 1

[0054] The difference from Example 1 is that no water is added to the solvent; otherwise, it is the same as Example 1.

[0055] Comparative Example 2

[0056] The difference from Example 1 is that the water content in the solvent is 8%, while the rest is the same as in Example 1.

[0057] Comparative Example 3

[0058] The difference from Example 1 is that the solvent is only water, while everything else is the same as in Example 1.

[0059] Comparative Example 4

[0060] The difference from Example 1 is that betaine is omitted, and only proline and glycerol containing 5.2% water in a molar ratio of 2:5 are used as solvents. Otherwise, it is the same as Example 1.

[0061] Comparative Example 5

[0062] The difference from Example 1 is that betaine is replaced with choline chloride, otherwise it is the same as Example 1.

[0063] Effect detection:

[0064] 1. Oat protein extraction rate detection:

[0065] The calculation formula is: Extraction rate % = (W1 / W2) * 100%

[0066] in:

[0067] W1 represents the mass of the prepared oat protein; W2 represents the mass of the original oat powder.

[0068] The calculation results are shown in Table 1 below.

[0069] Table 1

[0070] Extraction rate % Example 1 18.58 Example 2 17.26 Example 3 19.25 Comparative Example 1 10.82 Comparative Example 2 12.43 Comparative Example 3 8.24 Comparative Example 4 13.80 Comparative Example 5 15.92

[0071] According to the test results in Table 1 above, the oat protein prepared by the method provided in Examples 1-3 of this invention has a high extraction rate, which can reach more than 17%. However, changing the type of solvent in the comparative examples will affect the extraction efficiency of oat protein and reduce the extraction rate.

[0072] 2. Percentage of protein by mass in oat protein

[0073] The Dumas combustion method was used for detection. The results are shown in Table 2 below.

[0074] Table 2

[0075] % of protein by mass in oat protein Example 1 82.6 Example 2 83.7 Example 3 85.2 Comparative Example 1 75.5 Comparative Example 2 78.8 Comparative Example 3 65.4 Comparative Example 4 78.2 Comparative Example 5 68.7

[0076] According to the test results in Table 2 above, the protein content of the oat protein prepared by this invention is relatively high, reaching over 80%. However, changing the type of solvent in the comparative example not only affects the extraction efficiency of oat protein, reducing the extraction rate, but also reduces the protein content in the obtained oat protein, thereby affecting the purity of the oat protein and user satisfaction.

[0077] The above embodiments are only used to illustrate the technical solutions of the present invention and not to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still make modifications or equivalent substitutions to the specific implementation schemes of the present invention, and these modifications or equivalent substitutions do not depart from the spirit and scope of the present invention, and are all within the protection scope of the claims of the present invention.

Claims

1. A method of extracting oat protein, characterized by: Includes the following steps: (1) Preparation of oat powder: Oat flakes are crushed to 100-120 mesh to obtain oat powder; (2) Add the oat powder from step (1) to a solvent and heat to extract. Centrifuge to collect the supernatant, precipitate, stand, wash and dry to obtain the oat protein. The solvent is a eutectic solvent composed of proline, betaine and glycerol, with a molar ratio of 1-3:1:4-6; the solvent also contains 3-6% water; the ratio of oat powder to solvent is 1g:3-8mL. The heating extraction process described is as follows: first, extract in a water bath for 20 minutes, then sonicate for 10 minutes, then heat in a water bath for 20 minutes, then sonicate for 10 minutes, repeating this process 2-3 times.

2. The extraction method of claim 1, wherein: The molar ratio of proline, betaine, and glycerol is 2:1:

5.

3. The extraction method of claim 1, wherein: The heating extraction is a water bath extraction, with the water bath temperature being 50-70℃; the heating extraction time is 2-3 hours.

4. The extraction method of claim 1, wherein: The heating extraction operation also includes ultrasound; the power of the ultrasound is 150-200W.

5. The extraction method of claim 1, wherein: The precipitation is achieved by adding deionized water to the supernatant, with the volume ratio of deionized water to supernatant being 4-6:1.