Extraction method of oat protein, product and application of product in hair care product

Abstract

The invention provides an extraction method of oat protein, and belongs to the technical field of extraction of effective components. The extraction method comprises the following steps: (1) preparing oat powder; and (2) adding oat powder into a solvent, heating, extracting, centrifuging, taking supernate, precipitating, standing, washing and drying to obtain the oat protein. According to the method, a mixture of proline, betaine and glycerol is adopted as a deep eutectic solvent, the molar ratio of proline to betaine to glycerol is controlled to be (1-3): 1: (4-6), organic substances are extracted and separated through interaction of hydrogen bonds and coordination components in a system, and the effects of being high in extraction efficiency, capable of keeping protein activity and environmentally friendly are achieved.

Description

Technical Field

[0001] The invention belongs to the technical field of effective ingredient extraction, and particularly relates to an oat protein extraction method, a product and application of the oat protein in hair care products. Background Art

[0002] Oats are herbaceous crops of the genus Avena in the Poaceae family. 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 proportion, and has excellent physiological functions and activities.

[0003] The required protein can be extracted by enriching or separating it from the raw materials. Currently, the commonly used methods for extracting protein include alkali dissolution and acid precipitation, enzymatic hydrolysis and ultrasonic extraction. Currently, the most common means for extracting oat protein is alkali dissolution and acid precipitation. However, the alkali concentration cannot be too high when extracting protein using this method. Pay attention to the regulation of pH value, otherwise it will cause unfavorable condensation reactions between lysine and cystine or alanine to generate harmful substances, further leading to the loss of protein nutrients. The advantages of enzymatic hydrolysis for protein extraction are that the reaction conditions are relatively mild, the material-liquid ratio is easy to control, the protein is hydrolyzed into short peptide chains with a high extraction rate, and it can effectively reduce the loss of nutritional value of the protein. However, excessive enzymatic hydrolysis can easily lead to a reduction in or permanent loss of some functional properties of the protein. Ultrasonic extraction of protein has a volume-increasing effect, so the concentration of the alkali solution can be appropriately reduced when extracting protein to avoid the damage of the alkali solution to the protein, but the processing process is more cumbersome.

[0004] Chinese patent CN118852322A discloses a method for efficiently extracting oat protein based on a low eutectic system, which includes the following steps: (1) preparing oat powder; (2) mixing a hydrogen bond acceptor, a hydrogen bond donor and the oat powder to form a low 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 to precipitate; (5) centrifuging to remove the lower layer of protein; (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 remove the lower layer of protein; (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 oat protein extraction method, minimize the impact on the environment, and promote the application of low eutectic system in the extraction of biomacromolecules.

[0005] Chinese patent CN119119170A discloses a method for extracting oat bran protein, which comprises mixing HBD and HBA in different molar ratios and magnetically stirring until a clear liquid is formed; washing oats with deionized water, drying at 40°C to a water content of 10%, crushing, passing through a 60-mesh sieve, and taking the oat bran on the 60-mesh sieve; mixing oat bran and n-hexane (g / ml) in a ratio of 1:5, magnetically stirring at 600 rpm for 3 hours at room temperature, centrifuging at 4000 rpm for 10 minutes, repeating defatting three times, allowing to evaporate and air-dry to obtain defatted oat bran; vortex mixing defatted oat bran with DES solution in a solid-to-liquid ratio of 1:10, stirring at 600 rpm for 60 minutes at 50°C, cooling to room temperature, and centrifuging at 3500 rpm for 10 minutes; taking the supernatant, and extracting the precipitate again with fresh DES twice using the same extraction process. The resulting supernatants are combined and placed in a dialysis bag with a molecular weight cut-off of 3500 D. The suspension was dialyzed at 4°C for about 3 days, and the resulting suspension was freeze-dried to obtain crude protein powder.

[0006] The above-mentioned existing technologies all use deep eutectic solvents (DES) to extract and separate organic substances through the interaction between hydrogen bonds and coordination 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 alkali dissolution and acid precipitation methods.

[0007] Therefore, it is also necessary to develop a method for extracting oat protein that has high extraction efficiency, can maintain protein activity, and is green and environmentally friendly. Summary of the Invention

[0008] Based on the deficiencies in the prior art, the present invention aims to provide a method for extracting oat protein that has high extraction efficiency, can maintain 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 strong, improve hair gloss, and have a good repairing effect on scalp hair follicles.

[0009] In order to achieve the above object, the present invention adopts the following technical solutions:

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

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

[0012] (2) The oat powder in step (1) is added to a solvent for heating and extraction, and the supernatant is obtained by centrifugation, precipitated, allowed to stand, washed, and dried to obtain the oat protein.

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

[0014] The preparation method of the solvent is:

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

[0016] The heating extraction is water bath heating extraction, and the temperature of the water bath is 60-80°C, preferably 75°C.

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

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

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

[0020] As a preferred embodiment, the heating extraction is as follows: first extract in a water bath for 20 minutes, then ultrasonicate for 10 minutes, then heat in a water bath for 20 minutes, then ultrasonicate for 10 minutes, and repeat 2-3 times.

[0021] Since the deep eutectic solvent is a solvent with relatively high viscosity, the viscosity of the solvent will affect the extraction efficiency of the target product when the active ingredient is extracted. Therefore, the purpose of improving the extraction efficiency can be achieved by adjusting the viscosity of the deep eutectic solvent. During the implementation of the present invention, the viscosity of the solvent is reduced by adding water to the solvent.

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

[0023] During the implementation of the present invention, it was found that when the amount of water added was less than 3%, the viscosity of the deep eutectic solvent could not be improved significantly, and thus the purpose of improving the extraction efficiency could not be achieved; when the water content was higher than 6%, on the one hand, the hydrogen bond interaction in the deep eutectic solvent would be destroyed, and on the other hand, the solubility of the protein in the solvent would be affected, thereby failing to achieve the purpose of improving the extraction efficiency.

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

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

[0026] The washing is carried out using deionized water, the washing temperature is 50-70° C., and the washing time is 1-2 hours.

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

[0028] In another aspect, the present invention further provides the use of the oat protein prepared by the above preparation method in the preparation of cosmetic raw materials or cosmetics, wherein the cosmetics are hair care products.

[0029] The hair care product 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 conditioner, a preservative and water; the moisturizer is glycerin; the skin conditioner is hydroxypropyl guar hydroxypropyltrimonium chloride, and the preservatives are ethylhexylglycerin and phenoxyethanol.

[0031] Compared with the prior art, the present invention has the following beneficial effects:

[0032] (1) During the implementation of the present invention, a mixture of proline, betaine and glycerol is used as a low eutectic solvent, and the molar ratio of the three is controlled to be 1-3:1:4-6. The extraction and separation of organic matter are achieved through the interaction between hydrogen bonds and coordination components in the system. However, during the extraction process, it is found that the low eutectic solvent is a solvent with relatively high viscosity. When the effective ingredients are extracted, the viscosity of the solvent will affect the extraction efficiency of the target product. Therefore, in order to better improve the extraction efficiency of oat protein, the viscosity of the solvent is reduced by adding water to the solvent during the implementation of the present invention.

[0033] (2) During the implementation of the present invention, 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 found that when the amount of water added is less than 3%, the viscosity of the deep eutectic solvent cannot be well improved, and thus the purpose of improving the extraction efficiency cannot be achieved; when the water content is higher than 6%, on the one hand, the hydrogen bond interaction in the deep eutectic solvent will be destroyed, and on the other hand, the solubility of the protein in the solvent will be affected, thereby failing to achieve the purpose of improving the extraction efficiency.

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

[0035] The following will be combined with the tables in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0036] Hereinafter, examples of the present invention and comparative examples will be shown to explain the composition of the present invention in more detail, but the present invention is not limited thereto.

[0037] The present invention does not limit the sources of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are common commercial products in the technical field.

[0038] Example 1 A method for extracting oat protein

[0039] The steps include:

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

[0041] (2) 10 g of the oat powder in step (1) was added to 50 mL of a mixed solvent containing 5.2% water, proline, betaine, and glycerol in a molar ratio of 2:1:5, and heated for extraction. The supernatant was centrifuged and deionized water was added to the supernatant (the volume ratio of deionized water to supernatant was 5:1). The mixture was allowed to stand for 20 h, washed with deionized water at a temperature of 60° C. for 1.5 h, and freeze-dried to obtain the oat protein.

[0042] The heating extraction is as follows: first extract in a 75°C water bath for 20 minutes, then keep warm and ultrasonicate at 160W for 10 minutes, then heat in a 75°C water bath for 20 minutes, then keep warm and ultrasonicate at 160W for 10 minutes, and repeat twice.

[0043] Example 2 A method for extracting oat protein

[0044] The steps include:

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

[0046] (2) 10 g of the oat powder in step (1) was added to 30 mL of a mixed solvent containing 3% water, proline, betaine, and glycerol in a molar ratio of 1:1:4, and heated for extraction. The supernatant was centrifuged and deionized water was added to the supernatant (the volume ratio of deionized water to supernatant was 4:1). The mixture was allowed to stand for 24 h, washed with deionized water at a temperature of 50° C. for 2 h, and freeze-dried to obtain the oat protein.

[0047] The heating extraction is as follows: first extract in a 60°C water bath for 20 minutes, then keep warm and ultrasonicate at 200W for 10 minutes, then heat in a 60°C water bath for 20 minutes, then keep warm and ultrasonicate at 200W for 10 minutes, and repeat twice.

[0048] Example 3 A method for extracting oat protein

[0049] The steps include:

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

[0051] (2) 10 g of the oat powder in step (1) was added to 80 mL of a mixed solvent containing 6% water, proline, betaine, and glycerol in a molar ratio of 1:1:2, and heated for extraction. The supernatant was centrifuged and deionized water was added to the supernatant (the volume ratio of deionized water to supernatant was 6:1). The mixture was allowed to stand for 20 h, washed with deionized water at a washing temperature of 70° C. for 1 h, and freeze-dried to obtain the oat protein.

[0052] The heating extraction is as follows: first extract in an 80°C water bath for 20 minutes, then keep warm and ultrasonicate at 150W for 10 minutes, then heat in an 80°C water bath for 20 minutes, then keep warm and ultrasonicate at 150W for 10 minutes, and repeat twice.

[0053] Comparative Example 1

[0054] The difference from Example 1 is that no water is added to the solvent, and the other steps are 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%, and the other aspects are the same as Example 1.

[0057] Comparative Example 3

[0058] The difference from Example 1 is that the solvent is only water, and the rest is the same as 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 the solvent. Other aspects are the same as Example 1.

[0061] Comparative Example 5

[0062] The difference from Example 1 is that betaine is replaced by choline chloride, and the rest 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 is the mass of the prepared oat protein; W2 is 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, it can be seen that the oat protein prepared by the methods provided in Examples 1-3 of the present 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 the oat protein and reduce the extraction rate.

[0072] 2. The mass percentage of protein in oat protein

[0073] The results were shown in Table 2 below.

[0074] Table 2

[0075] The mass percentage of protein 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 in the oat protein prepared by the present invention is relatively high, reaching more than 80%. However, changing the type of solvent in the comparative example not only affects the extraction efficiency of the oat protein and reduces 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 are not intended to limit the same. Although the present invention has been described in detail with reference to the above embodiments, a person skilled in the art may still modify or make equivalent substitutions for the specific implementation schemes of the present invention. Any modifications or equivalent substitutions that do not depart from the spirit and scope of the present invention are within the scope of protection of the claims of the present invention.

Claims

1. A method for extracting oat protein, characterized in that: The steps include: (1) Preparation of oat powder: Grind oat flakes into 100-120 mesh to obtain oat powder; (2) adding the oat powder in step (1) into a solvent for heating and extraction, centrifuging to obtain the supernatant, precipitating, standing, washing, and drying to obtain the oat protein. The solvent is a low eutectic solvent composed of proline, betaine and glycerol, and the molar ratio of the three is 1-3:1:4-6.

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

5.

3. The extraction method according to claim 1, wherein: The heating extraction is water bath heating extraction, the water bath temperature is 50-70° C.; the heating extraction time is 2-3 hours.

4. The extraction method according to claim 1, wherein: The material-liquid ratio of the oat powder to the solvent is 1g:3-8mL.

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

6. The extraction method according to claim 1, wherein: The heating extraction is as follows: first extracting in a water bath for 20 minutes, then ultrasonicating for 10 minutes, then heating in a water bath for 20 minutes, then ultrasonicating for 10 minutes, and repeating this 2-3 times.

7. The extraction method according to claim 1, wherein: The solvent also contains 3-6% water.

8. The extraction method according to claim 1, wherein: The precipitation is performed by adding deionized water to the supernatant, and the volume ratio of the deionized water to the supernatant is 4-6:

1.

9. Oat protein prepared by the preparation method according to any one of claims 1 to 8.

10. Use of the oat protein prepared by the preparation method according to any one of claims 1 to 8 in the preparation of cosmetic raw materials or cosmetics, wherein the cosmetics are hair care products.