Method for extracting tea saponin from camellia seed meal
Through crushing, drying, ultrasonic impregnation, high-pressure pressing, microwave ultrasonic extraction and dopamine treatment, the problems of too dark color and too many impurities caused by traditional water extraction are solved, and efficient and high-purity tea saponin extraction is achieved.
Patent Information
- Application Number
- CN202510158392.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-13
- Publication Date
- 2025-05-06
AI Technical Summary
Traditional water extraction method of tea saponin extracting from oil tea seed meal can easily lead to too dark color and too many impurities in the extract, affecting product quality.
The fine powder of tea seed meal was treated by crushing and drying, followed by ultrasonic impregnation using saturated sodium chloride solution, followed by high-pressure pressing and microwave ultrasonic extraction, and finally dopamine solution was added for concentration and drying to extract high-purity tea saponin.
This method significantly improves the extraction efficiency and purity of tea saponin, reduces the content of protein impurities, and improves the quality of the product.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of biomass extraction, and more specifically, relates to a method for extracting tea saponin from camellia oleifera seed meal. Background Art
[0002] Tea saponin, also known as camellia saponin, is a mixture of saponins found in tea seeds and tea leaves. At the same time, tea saponin is also a small molecule substance with excellent performance and a green natural surfactant. The waste after tea oil is squeezed out of camellia seeds is camellia meal. Camellia meal contains rich nutrients, such as protein, crude fiber, fat, polysaccharides, etc. At the same time, camellia meal also contains some substances with antioxidant activity, among which the content of tea saponin is relatively high in camellia meal. However, a large amount of camellia meal has not been effectively utilized.
[0003] There are more than a dozen methods for extracting tea saponin from camellia oleifera seed cake. From the initial hot water extraction method to the current ultra-high pressure method, supercritical extraction method and other new technologies, the yield and purity of tea saponin have been continuously improved. According to the literature review, organic solvent extraction, microwave-assisted extraction and ultrasound-assisted extraction are the most widely used in the extraction of tea saponin; water extraction has not been widely used because the extract is too dark in color and has too many impurities; and other new technologies, such as irradiation extraction, supercritical extraction, and flash extraction have not been widely popularized due to equipment and cost reasons.
[0004] Based on this, developing a tea saponin extraction method with high extraction efficiency and high product purity is still a technical problem that technicians in this field need to overcome. Summary of the invention
[0005] The technical problem to be solved by the present invention is that when extracting tea saponin from camellia oleifera seed cake, the single water extraction method easily leads to the problem that the color of the extract is too dark and there are too many impurities after extraction, which affects the product quality. Based on the above problems, the present invention provides a method for extracting tea saponin from camellia oleifera seed cake.
[0006] The purpose of the invention is to provide a method for extracting tea saponin from camellia oleifera seed meal.
[0007] The above-mentioned purpose of the present invention is achieved through the following technical solutions: A method for extracting tea saponin from camellia oleifera seed meal, the specific extraction steps comprising: After the camellia oleifera seed meal is crushed, it is passed through a 40-80 mesh sieve to obtain a fine powder of the camellia oleifera seed meal; Drying the camellia seed meal powder at a temperature of 60-100° C. to a constant weight to obtain a dry camellia seed meal powder; By weight, 100-120 parts of dried camellia dregs powder, 200-220 parts of saturated sodium chloride solution at a temperature of 40-50°C, and 300-340 parts of ethanol solution with a mass fraction of 20-60% are taken, and the dried camellia dregs powder and the saturated sodium chloride solution at a temperature of 40-50°C are first mixed, and then ultrasonically immersed at a temperature of 40-50°C for 10-20 minutes, and then cooled to a temperature below 10°C, centrifuged, and a filter cake is collected; The filter cake is pressed for 5-10 minutes at a pressure of 10-15 MPa to obtain a pressed material; The squeezed material and the ethanol solution are mixed, heated to 40-50°C, subjected to microwave ultrasonic extraction for 10-15 minutes, and filtered to obtain a filtrate; The filtrate is concentrated and dried to obtain tea saponin.
[0008] Beneficial technical effects of the above technical solution: First, the oil-tea camellia seed meal is refined by pulverizing, and then, continuous drying is performed at a certain temperature to remove the residual moisture in the refined oil-tea camellia seed meal. When a saturated sodium chloride solution is subsequently used for ultrasonic impregnation under a certain temperature condition, the plant cells as a whole are dehydrated due to the sufficient drying mentioned above, which facilitates the saturated sodium chloride solution to smoothly enter the interior of the oil-tea camellia seed meal under the cavitation effect of the ultrasonic wave. The so-called saturated sodium chloride solution at a certain temperature refers to a heat-insulating sodium chloride solution under the temperature condition. When the temperature is subsequently lowered, the dissolution equilibrium of sodium chloride is broken, thereby causing sodium chloride to precipitate in the form of crystals. Since the saturated sodium chloride solution has been fully impregnated in the oil-tea camellia seed meal under the action of ultrasound, when the crystals precipitate, part of them will remain in the plant cells, and part of them will remain in the internal pores. Combined with the subsequent high-pressure squeezing effect, the sodium chloride crystals will be broken, causing the plant cells to rupture, or the pores to be effectively widened. Therefore, it will provide great convenience for the subsequent microwave ultrasonic extraction of the ethanol solution and significantly improve the extraction effect. In addition, it is particularly important to note that the reason for using sodium chloride salt solution for treatment and the treatment process before using ethanol solution for extraction is that, under the action of high concentration of sodium chloride salt solution, the water-soluble protein inside the plant cells of the camellia oleifera meal will be denatured due to salting out and converted into precipitates. In the subsequent extraction process using ethanol solution, this part of the water-soluble protein will not be extracted together with the tea saponin, thereby significantly reducing the introduction of this part of impurities.
[0009] Further, the ultrasonic impregnation includes: Ultrasonic immersion was performed at an ultrasonic frequency of 80-120 kHz.
[0010] Furthermore, the microwave ultrasonic extraction comprises: Microwave ultrasonic extraction is performed under the conditions of microwave power of 280-450W and ultrasonic frequency of 150-180kHz.
[0011] Further, the pH value of the saturated sodium chloride solution is 7.5-8.0; The pH value of the saturated sodium chloride solution is adjusted using an alkaline solution; The alkaline solution is selected from any one of a sodium hydroxide solution and a potassium hydroxide solution.
[0012] The above technical solution further brings about the following beneficial effects: Camellia oleifera meal is treated with a weakly alkaline saturated sodium chloride solution. Furthermore, since the main components of the cell wall of plant cells are cellulose, pectin, hemicellulose, lignin and protein, the structure of the plant cell wall can be destroyed in an alkaline environment, especially the components such as pectin and hemicellulose therein, making it easier for tea saponin to dissolve from the cell wall; more importantly, the alkaline environment can change the polarity of the solvent, thereby enhancing the solvent's ability to dissolve tea saponin, thereby increasing the extraction rate of tea saponin; however, it should be noted that if the alkalinity is too strong, that is, if the pH value is too high, it will cause the tea saponin to hydrolyze faster during the extraction process, thereby affecting the extraction of the product. Therefore, the pH value needs to be controlled below a certain value to achieve a balance between multiple functions.
[0013] Furthermore, the specific extraction step also includes: After the camellia oleifera seed meal is crushed, it is passed through a 40-80 mesh sieve to obtain a fine powder of the camellia oleifera seed meal; Drying the camellia seed meal powder at a temperature of 60-100° C. to a constant weight to obtain a dry camellia seed meal powder; By weight, 100-120 parts of dried camellia dregs powder, 200-220 parts of saturated sodium chloride solution at a temperature of 40-50°C, and 300-340 parts of ethanol solution with a mass fraction of 20-60% are taken, and the dried camellia dregs powder and the saturated sodium chloride solution at a temperature of 40-50°C are first mixed, and then ultrasonically immersed at a temperature of 40-50°C for 10-20 minutes, and then cooled to a temperature below 10°C, centrifuged, and a filter cake is collected; The filter cake is pressed for 5-10 minutes at a pressure of 10-15 MPa to obtain a pressed material; The squeezed material and the ethanol solution are mixed, heated to 40-50°C, subjected to microwave ultrasonic extraction for 10-15 minutes, and filtered to obtain a filtrate; and a dopamine solution in an amount of 10-12% of the mass of the filtrate is added to the filtrate to obtain a mixed solution; Wherein, the concentration of the dopamine solution is 2-3g / L; The mixed solution is concentrated and spray-dried to obtain tea saponin.
[0014] In the above technical scheme, a dopamine solution of appropriate concentration is further added to the filtrate after the extraction is completed. Mainly, during the concentration and drying process, the hydrolysis of tea saponin also needs to be considered. The introduction of dopamine can cause a certain degree of oxidative self-polymerization during the concentration and drying process. During the self-polymerization process, the tea saponin molecules are firmly adsorbed, the free tea saponin is reduced, and the hydrolysis reaction of the tea saponin is limited.
[0015] Further, the concentration includes: The mixed solution is concentrated to 0.2-0.25 times the original volume.
[0016] Further, the spray drying comprises: Under the conditions of feed rate of 25-30 g / min, air inlet temperature of 120-130° C., air outlet temperature of 100-105° C., main disk speed of 8000-8500 r / min, spray drying is carried out, and the dried powder is collected to obtain tea saponin. DETAILED DESCRIPTION
[0017] The present invention is further described below with reference to specific examples, but the examples do not limit the present invention in any form. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art.
[0018] Unless otherwise specified, the reagents and materials used in the following examples are commercially available.
[0019] In the monodisperse hollow nanoparticles mentioned below, the specific meaning of hollow is that bubbles are introduced by using emulsifiers or the like during the preparation process, so that the inside of the particles is in a hollow state, as distinguished from a completely solid state. Example 1
[0020] Pour the camellia seed meal into a universal grinder, grind it, and pass it through a 40-mesh sieve to obtain fine camellia seed meal powder; The camellia oleifera seed meal powder is transferred into an oven and dried at 60°C to a constant weight to obtain a dry camellia oleifera seed meal powder; According to weight, 100 parts of dried camellia dregs powder, 200 parts of saturated sodium chloride solution at 40°C, and 300 parts of ethanol solution with a mass fraction of 20% are taken, and the dried camellia dregs powder and the saturated sodium chloride solution at 40°C are first mixed, and then ultrasonically immersed for 10 minutes at a temperature of 40°C and an ultrasonic frequency of 80kHz, and then cooled to a temperature of 8°C, and after standing for 3 hours, poured into a centrifuge, centrifuged at a speed of 8000r / min for 25 minutes, and the filter cake is collected; The pH value of the saturated sodium chloride solution is 7.5; The pH value of the saturated sodium chloride solution is adjusted using an alkaline solution; The alkaline solution is selected from sodium hydroxide solution; The filter cake was pressed for 5 min at a pressure of 10 MPa to obtain a pressed material; The squeezed material and the ethanol solution are mixed, heated to 40°C, and subjected to microwave ultrasonic extraction for 10 minutes, and then filtered to obtain a filtrate; a dopamine solution with a mass percentage of 10% of the filtrate is added to the filtrate to obtain a mixed solution; The microwave ultrasonic extraction was carried out under the conditions of microwave power of 280W and ultrasonic frequency of 150kHz; Wherein, the concentration of the dopamine solution is 2g / L; After the mixed solution is concentrated to 0.2 times of the original volume, it is spray-dried at a feed rate of 25 g / min, an inlet air temperature of 120°C, an outlet air temperature of 100°C, and a main disk speed of 8000 r / min, and the dried powder is collected to obtain tea saponin. Example 2
[0021] Pour the camellia seed meal into a universal grinder, grind it, and then pass it through a 60-mesh sieve to obtain fine camellia seed meal powder; The camellia oleifera seed meal powder is transferred into an oven and dried at 80°C to a constant weight to obtain a dry camellia oleifera seed meal powder; By weight, 110 parts of dried camellia dregs powder, 210 parts of saturated sodium chloride solution at 45°C, and 320 parts of 40% ethanol solution are taken. The dried camellia dregs powder and the saturated sodium chloride solution at 45°C are first mixed, and then ultrasonically immersed for 15 minutes at a temperature of 45°C and an ultrasonic frequency of 100kHz. Then, the mixture is cooled to a temperature of 9°C, allowed to stand for 3.8 hours, poured into a centrifuge, and centrifuged at a speed of 9000r / min for 30 minutes to collect the filter cake. The pH value of the saturated sodium chloride solution is 7.8; The pH value of the saturated sodium chloride solution is adjusted using an alkaline solution; The alkaline solution is selected from sodium hydroxide solution; The filter cake was pressed for 8 min at a pressure of 12 MPa to obtain a pressed material; The squeezed material and the ethanol solution were mixed, heated to 45°C, and subjected to microwave ultrasonic extraction for 12 minutes, and then filtered to obtain a filtrate; a dopamine solution with a mass percentage of 11% of the filtrate was added to the filtrate to obtain a mixed solution; The microwave ultrasonic extraction was carried out under the conditions of microwave power of 360W and ultrasonic frequency of 160kHz; Wherein, the concentration of the dopamine solution is 2.5g / L; After the mixed solution is concentrated to 0.22 times of the original volume, it is spray-dried at a feed rate of 28 g / min, an inlet air temperature of 125°C, an outlet air temperature of 102°C, and a main disk speed of 8200 r / min, and the dried powder is collected to obtain tea saponin. Example 3
[0022] Pour the camellia seed meal into a universal grinder, grind it, and then pass it through a 480-mesh sieve to obtain fine camellia seed meal powder; The camellia oleifera seed meal powder is transferred into an oven and dried at 100° C. to a constant weight to obtain a dry camellia oleifera seed meal powder; According to weight, 120 parts of dried camellia dregs powder, 220 parts of saturated sodium chloride solution at 50°C, and 340 parts of 60% ethanol solution are taken, and the dried camellia dregs powder and the saturated sodium chloride solution at 50°C are first mixed, and then ultrasonically immersed for 20 minutes at a temperature of 50°C and an ultrasonic frequency of 120kHz, and then cooled to a temperature of 6°C, and after standing for 5 hours, poured into a centrifuge, centrifuged at a speed of 10000r / min for 50 minutes, and the filter cake is collected; The pH value of the saturated sodium chloride solution is 8.0; The pH value of the saturated sodium chloride solution is adjusted using an alkaline solution; The alkaline solution is selected from potassium hydroxide solution; The filter cake was pressed for 10 min at a pressure of 15 MPa to obtain a pressed material; The squeezed material and the ethanol solution were mixed, heated to 50°C, and subjected to microwave ultrasonic extraction for 15 minutes, and then filtered to obtain a filtrate; a dopamine solution with a mass percentage of 12% of the filtrate was added to the filtrate to obtain a mixed solution; The microwave ultrasonic extraction is carried out under the conditions of microwave power of 450W and ultrasonic frequency of 180kHz; Wherein, the concentration of the dopamine solution is 3g / L; After the mixed solution is concentrated to 0.25 times of the original volume, it is spray-dried at a feed rate of 30 g / min, an inlet air temperature of 130°C, an outlet air temperature of 105°C, and a main disk speed of 8500 r / min, and the dried powder is collected to obtain tea saponin. Example 4
[0023] The present embodiment differs from embodiment 1 in that no dopamine solution is added, and other conditions remain unchanged. Example 5
[0024] Compared with Example 1, the present embodiment differs in that the pH value of the saturated sodium chloride solution is 7.0, and the other conditions remain unchanged.
[0025] Comparative Example 1 Pour the camellia seed meal into a universal grinder, grind it, and pass it through a 40-mesh sieve to obtain fine camellia seed meal powder; The camellia oleifera seed meal powder is transferred into an oven and dried at 60°C to a constant weight to obtain a dry camellia oleifera seed meal powder; According to weight, 100 parts of dry camellia dregs powder and 300 parts of 20% ethanol solution are taken, the dry camellia dregs powder and the ethanol solution are mixed, heated to 40°C, and subjected to microwave ultrasonic extraction for 10 minutes, and then filtered to obtain a filtrate; then a dopamine solution with a mass fraction of 10% of the filtrate is added to the filtrate to obtain a mixed solution; The microwave ultrasonic extraction was carried out under the conditions of microwave power of 280W and ultrasonic frequency of 150kHz; Wherein, the concentration of the dopamine solution is 2g / L; After the mixed solution is concentrated to 0.2 times of the original volume, it is spray-dried at a feed rate of 25 g / min, an inlet air temperature of 120°C, an outlet air temperature of 100°C, and a main disk speed of 8000 r / min, and the dried powder is collected to obtain tea saponin.
[0026] Comparative Example 2 Pour the camellia seed meal into a universal grinder, grind it, and pass it through a 40-mesh sieve to obtain fine camellia seed meal powder; The camellia oleifera seed meal powder is transferred into an oven and dried at 60°C to a constant weight to obtain a dry camellia oleifera seed meal powder; According to weight, 100 parts of dry camellia dregs powder, 200 parts of 10% sodium chloride solution, and 300 parts of 20% ethanol solution are taken. The dry camellia dregs powder and the 10% sodium chloride solution are first mixed, and then ultrasonically immersed for 10 minutes at a temperature of 40°C and an ultrasonic frequency of 80kHz, and then cooled to a temperature of 8°C, and allowed to stand for 3 hours, and then poured into a centrifuge, and centrifuged at a speed of 8000r / min for 25 minutes to collect the filter cake; The pH value of the 10% sodium chloride solution is 7.5; The pH value of the sodium chloride solution with a mass fraction of 10% is adjusted by using an alkaline solution; The alkaline solution is selected from sodium hydroxide solution; The filter cake was pressed for 5 min at a pressure of 10 MPa to obtain a pressed material; The squeezed material and the ethanol solution are mixed, heated to 40°C, and subjected to microwave ultrasonic extraction for 10 minutes, and then filtered to obtain a filtrate; a dopamine solution with a mass percentage of 10% of the filtrate is added to the filtrate to obtain a mixed solution; The microwave ultrasonic extraction was carried out under the conditions of microwave power of 280W and ultrasonic frequency of 150kHz; Wherein, the concentration of the dopamine solution is 2g / L; After the mixed solution is concentrated to 0.2 times of the original volume, it is spray-dried at a feed rate of 25 g / min, an inlet air temperature of 120°C, an outlet air temperature of 100°C, and a main disk speed of 8000 r / min, and the dried powder is collected to obtain tea saponin.
[0027] The content of protein impurities in the tea saponin products obtained in the examples and comparative examples was measured. The specific test method was to use the Kjeldahl nitrogen determination method for testing. The detailed test results are shown in Table 1. ; It can be seen from the above test results that the extraction method adopted by the present invention can effectively reduce the content of protein impurities in the product and improve the purity of the product.
[0028] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.
Claims
1. A method for extracting tea saponin from camellia oleifera seed meal, characterized in that: The specific extraction steps include: After the camellia oleifera seed meal is crushed, it is passed through a 40-80 mesh sieve to obtain a fine powder of the camellia oleifera seed meal; Drying the camellia oleifera seed meal powder at a temperature of 60-100° C. to a constant weight to obtain a dry camellia oleifera seed meal powder; By weight, 100-120 parts of dried camellia dregs powder, 200-220 parts of saturated sodium chloride solution at a temperature of 40-50°C, and 300-340 parts of ethanol solution with a mass fraction of 20-60% are taken, and the dried camellia dregs powder and the saturated sodium chloride solution at a temperature of 40-50°C are first mixed, and then ultrasonically immersed at a temperature of 40-50°C for 10-20 minutes, and then cooled to a temperature below 10°C, centrifuged, and a filter cake is collected; The filter cake is pressed for 5-10 minutes at a pressure of 10-15 MPa to obtain a pressed material; The squeezed material and the ethanol solution are mixed, heated to 40-50°C, subjected to microwave ultrasonic extraction for 10-15 minutes, and filtered to obtain a filtrate; The filtrate is concentrated and dried to obtain tea saponin.
2. The method for extracting tea saponin from camellia oleifera seed meal according to claim 1, characterized in that: The ultrasonic impregnation comprises: Ultrasonic immersion was performed at an ultrasonic frequency of 80-120 kHz.
3. The method for extracting tea saponin from camellia oleifera seed meal according to claim 1, characterized in that: The microwave ultrasonic extraction comprises: Microwave ultrasonic extraction is performed under the conditions of microwave power of 280-450W and ultrasonic frequency of 150-180kHz.
4. The method for extracting tea saponin from camellia oleifera seed meal according to claim 1, characterized in that: The pH value of the saturated sodium chloride solution is 7.5-8.0; The pH value of the saturated sodium chloride solution is adjusted using an alkaline solution; The alkaline solution is selected from any one of a sodium hydroxide solution and a potassium hydroxide solution.
5. The method for extracting tea saponin from camellia oleifera seed meal according to claim 1, characterized in that: The specific extraction step also includes: After the camellia oleifera seed meal is crushed, it is passed through a 40-80 mesh sieve to obtain a fine powder of the camellia oleifera seed meal; Drying the camellia oleifera seed meal powder at a temperature of 60-100° C. to a constant weight to obtain a dry camellia oleifera seed meal powder; By weight, 100-120 parts of dried camellia dregs powder, 200-220 parts of saturated sodium chloride solution at a temperature of 40-50°C, and 300-340 parts of ethanol solution with a mass fraction of 20-60% are taken, and the dried camellia dregs powder and the saturated sodium chloride solution at a temperature of 40-50°C are first mixed, and then ultrasonically immersed at a temperature of 40-50°C for 10-20 minutes, and then cooled to a temperature below 10°C, centrifuged, and a filter cake is collected; The filter cake is pressed for 5-10 minutes at a pressure of 10-15 MPa to obtain a pressed material; The squeezed material and the ethanol solution are mixed, heated to 40-50°C, subjected to microwave ultrasonic extraction for 10-15 minutes, and filtered to obtain a filtrate; and a dopamine solution in an amount of 10-12% of the mass of the filtrate is added to the filtrate to obtain a mixed solution; Wherein, the concentration of the dopamine solution is 2-3g / L; The mixed solution is concentrated and spray-dried to obtain tea saponin.
6. The method for extracting tea saponin from camellia oleifera seed meal according to claim 5, characterized in that: The concentration includes: The mixed solution is concentrated to 0.2-0.25 times the original volume.
7. The method for extracting tea saponin from camellia oleifera seed meal according to claim 5, characterized in that: The spray drying comprises: Under the conditions of feed rate of 25-30 g / min, air inlet temperature of 120-130° C., air outlet temperature of 100-105° C., main disk speed of 8000-8500 r / min, spray drying is carried out, and the dried powder is collected to obtain tea saponin.