Method for synchronously extracting tea seed oil and tea saponin from tea seeds
By using composite oil extraction additives and ultrasonic assisted extraction technology, tea seed oil and tea saponin are synchronized, and the problem of difficulty in taking into account both the extraction rate and purity in the prior art is solved, achieving efficient and environmentally friendly extraction effects.
Patent Information
- Application Number
- CN202411843543.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-14
- Publication Date
- 2025-03-21
AI Technical Summary
In the prior art, when extracting tea seed oil and tea saponin, it is difficult to meet the requirements of high extraction rate and high purity at the same time, and traditional methods have problems of environmental pollution and resource waste.
Using composite oil extraction additives and ultrasonic assisted extraction technology, tea seed oil and tea saponin are synchronized by dehulling, low-temperature treatment, puffing treatment, ultrasonic treatment, centrifugal separation, spray drying and alkali reagent treatment.
It significantly improves the extraction rate and purity of tea seed oil and tea saponin, optimizes the extraction efficiency and product quality, reduces environmental pollution and resource waste, and reduces production costs.
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Figure BDA0005188502670000111
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of active substance extraction, in particular to a method for synchronously extracting tea seed oil and tea saponin from tea seeds. Background Art
[0002] Tea seed oil, as an oil extracted from the fruit of the Camellia oleifera plant of the Theaceae family, is famous for its high content of unsaturated fatty acids and rich nutrients. Tea saponins, on the other hand, are a class of glycoside compounds extracted from tea tree seeds, which have significant surface activity and multiple biological functions.
[0003] Tea seed oil extraction technology is mainly divided into two types: mechanical pressing and solvent extraction. Mechanical pressing is a traditional extraction method that squeezes oil out of tea seeds through physical pressure. This method is simple and low-cost, but the extraction rate is relatively low, and some nutrients in the oil may be destroyed due to high temperature. The solvent extraction method is to dissolve the oil through a solvent (such as hexane, ethanol, etc.), and then separate the oil by evaporation or centrifugation. This method has a high extraction rate, but the cost is high, and there may be problems with solvent residues.
[0004] The extraction technology of tea saponin also includes organic solvent method and water extraction and alcohol precipitation method. The organic solvent method extracts tea saponin through organic solvents (such as methanol, ethanol, etc.), and then recovers the solvent through evaporation or distillation to obtain relatively pure tea saponin. The water extraction and alcohol precipitation method is to first extract tea seed powder with water, then precipitate tea saponin by adding ethanol, and finally obtain the tea saponin product by centrifugation and drying. Although these methods can extract tea saponin, they often have problems such as low extraction rate, low purity, and complicated operation.
[0005] Existing technologies face some common challenges when extracting tea seed oil and tea saponin. First, it is often difficult to balance extraction efficiency and product quality, and traditional extraction methods may not be able to meet the requirements of high extraction rate and high purity at the same time. Secondly, the sustainable utilization of the environment and resources has also received increasing attention. Traditional organic solvent extraction methods may cause pollution to the environment, and the recovery and reuse of solvents also increase production costs. In addition, a large amount of by-products and waste may be generated during the extraction of tea seed oil and tea saponin, and the treatment and utilization of these wastes are also problems that the existing technology needs to solve.
[0006] In terms of patent technology, some innovative methods have been proposed to address the limitations of existing technologies. For example, patent CN201610570742.7 describes a simple method for purifying tea saponin, which achieves the extraction of high-purity tea saponin by using a mixed solvent of methanol and n-hexane, as well as a specific mass ratio and operating conditions. Patent CN202111609816.0 relates to a system and method for continuous extraction of tea seed oil, which improves the production efficiency of tea seed oil through enzymatic hydrolysis and continuous extraction technology.
[0007] In summary, although the existing technology has made some progress in the extraction of tea seed oil and tea saponin, there are still challenges in efficiency, purity, environmental protection and resource utilization. These challenges provide directions for the development of new technologies and also highlight the importance of developing new extraction methods. Summary of the invention
[0008] The object of the present invention is to provide a method for simultaneously extracting tea seed oil and tea saponin from tea seeds, and the product extraction rate and purity are better.
[0009] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:
[0010] The present invention provides a method for synchronously extracting tea seed oil and tea saponin from tea seeds, comprising the following steps:
[0011] The tea seeds are sequentially subjected to shelling treatment, low temperature treatment and puffing treatment to obtain puffed material;
[0012] The expanded material is mixed with a composite oil extraction auxiliary agent, and subjected to ultrasonic treatment to obtain an ultrasonic product;
[0013] The ultrasonic product is centrifuged to obtain a heavy phase and a light phase;
[0014] The heavy phase is separated from the solvent and then spray-dried to obtain tea saponin;
[0015] Separating the solvent from the light phase and mixing it with an alkali solution, treating it with an alkali reagent, and centrifuging it to obtain a crude tea seed oil product;
[0016] The crude tea seed oil is refined to obtain tea seed oil.
[0017] Preferably, the composite oil extraction auxiliary agent contains polysorbate 80, sodium lauryl sulfate, disodium ethylenediaminetetraacetate and polyethylene glycol 400.
[0018] Preferably, the solvent of the composite oil extraction auxiliary agent is an isopropanol solution.
[0019] Preferably, the final concentration of polysorbate 80 in the composite oil extraction auxiliary agent is 0.3-0.8% w / v;
[0020] The final concentration of sodium dodecyl sulfate in the composite oil extraction auxiliary agent is 0.1-0.3% w / v;
[0021] The final concentration of disodium ethylenediaminetetraacetate in the composite oil extraction auxiliary agent is 0.03-0.08% w / v;
[0022] The final concentration of polyethylene glycol 400 in the composite oil extraction auxiliary agent is 0.05-0.15% w / v.
[0023] Preferably, the initial concentration of the isopropanol solution is 60-80%.
[0024] Preferably, the temperature of the low-temperature treatment is 40°C to 60°C; the time of the low-temperature treatment is 20min to 30min; the moisture content of the puffing treatment is 5% to 7%; the crushing particle size of the puffing treatment is 15 mesh to 25 mesh; the amount of water added in the puffing treatment is 0.3 times to 0.7 times the weight of the camellia oleifera kernel; the microwave power of the puffing treatment is 8KW to 12KW; and the time of the puffing treatment is 50 seconds to 70 seconds.
[0025] Preferably, the temperature of the ultrasonic treatment is 55° C. to 65° C.; the power of the ultrasonic treatment is 500W to 700W; and the time of the ultrasonic treatment is 100min to 140min.
[0026] Preferably, the temperature of the separation solvent is 35°C to 45°C; the vacuum degree of the separation solvent is -0.08Mpa to -0.1Mpa; the solvent recovery volume of the separation solvent is 20% to 30% of the volume of the extract; the separation solvent includes adding water, and the water volume is 3% to 5% of the volume of the extract; the centrifugal speed of the separation is 3500rpm to 4500rpm; the centrifugal time of the separation is 25min to 35min.
[0027] Preferably, the gas velocity flow rate of the spray drying is 35m 3 / h~45m 3 / h.
[0028] Preferably, the alkaline solution is a KOH solution; the concentration of the KOH solution is 150 g / L to 250 g / L; the time of the alkaline reagent treatment is 25 min to 35 min; and the refining treatment includes decolorization treatment, deodorization treatment and winterization treatment.
[0029] Technical effects and advantages of the present invention:
[0030] The present invention provides a new method for efficiently extracting tea seed oil and tea saponin from tea seeds. By finely controlling the extraction conditions, a significant improvement in extraction rate and purity is achieved. By using a specific composite oil extraction auxiliary agent and ultrasound-assisted extraction technology, the power, time and solvent ratio are optimized, so that the extraction efficiency and product quality of tea seed oil and tea saponin are better than those of traditional methods. Experimental data confirm that the tea seed oil extraction rate of the present invention reaches 27.22%, and the purity is as high as 99.66%; the tea saponin extraction rate is 21.85%, and the purity reaches 96.50%. The present invention increases the market competitiveness of the product by improving the utilization rate of raw materials and reducing production costs. High-quality tea seed oil and tea saponin meet the market demand for natural products and have broad application prospects. DETAILED DESCRIPTION
[0031] The present invention provides a method for synchronously extracting tea seed oil and tea saponin from tea seeds, comprising the following steps:
[0032] The tea seeds are sequentially subjected to shelling treatment, low temperature treatment and puffing treatment to obtain puffed material;
[0033] The expanded material is mixed with a composite oil extraction auxiliary agent, and subjected to ultrasonic treatment to obtain an ultrasonic product;
[0034] The ultrasonic product is centrifuged to obtain a heavy phase and a light phase;
[0035] The heavy phase is separated from the solvent and then spray-dried to obtain tea saponin;
[0036] Separating the solvent from the light phase and mixing it with an alkali solution, treating it with an alkali reagent, and centrifuging it to obtain a crude tea seed oil product;
[0037] The crude tea seed oil is refined to obtain tea seed oil.
[0038] Preferably, the composite oil extraction auxiliary agent contains polysorbate 80, sodium lauryl sulfate, disodium ethylenediaminetetraacetate and polyethylene glycol 400.
[0039] Preferably, the solvent of the composite oil extraction auxiliary agent is an isopropanol solution.
[0040] Preferably, the final concentration of polysorbate 80 in the composite oil extraction auxiliary agent is 0.3-0.8% w / v;
[0041] The final concentration of sodium dodecyl sulfate in the composite oil extraction auxiliary agent is 0.1-0.3% w / v;
[0042] The final concentration of disodium ethylenediaminetetraacetate in the composite oil extraction auxiliary agent is 0.03-0.08% w / v;
[0043] The final concentration of polyethylene glycol 400 in the composite oil extraction auxiliary agent is 0.05-0.15% w / v.
[0044] Preferably, the initial concentration of the isopropanol solution is 60-80%.
[0045] In the present invention, the components of the composite oil extraction auxiliary agent can reduce the oil-water interfacial tension, promote the release and extraction of oil, reduce the oxidation and decomposition of oil, improve the stability of oil, increase the solubility of effective ingredients in oil, and increase the concentration of target ingredients in the extract through synergistic effect.
[0046] Preferably, the temperature of the low-temperature treatment is 40°C to 60°C; the time of the low-temperature treatment is 20min to 30min; the moisture content of the puffing treatment is 5% to 7%; the crushing particle size of the puffing treatment is 15 mesh to 25 mesh; the amount of water added in the puffing treatment is 0.3 times to 0.7 times the weight of the camellia oleifera kernel; the microwave power of the puffing treatment is 8KW to 12KW; and the time of the puffing treatment is 50 seconds to 70 seconds.
[0047] Preferably, the temperature of the ultrasonic treatment is 55° C. to 65° C.; the power of the ultrasonic treatment is 500W to 700W; and the time of the ultrasonic treatment is 100min to 140min.
[0048] Preferably, the temperature of the separation solvent is 35°C to 45°C; the vacuum degree of the separation solvent is -0.08Mpa to -0.1Mpa; the solvent recovery volume of the separation solvent is 20% to 30% of the volume of the extract; the separation solvent includes adding water, and the water volume is 3% to 5% of the volume of the extract; the centrifugal speed of the separation is 3500rpm to 4500rpm; the centrifugal time of the separation is 25min to 35min.
[0049] Preferably, the gas velocity flow rate of the spray drying is 35m 3 / h~45m 3 / h.
[0050] Preferably, the alkaline solution is a KOH solution; the concentration of the KOH solution is 150 g / L to 250 g / L; the time of the alkaline reagent treatment is 25 min to 35 min; and the refining treatment includes decolorization treatment, deodorization treatment and winterization treatment.
[0051] In the present invention, the decolorization, deodorization and winterization treatment preferably adopt the following methods:
[0052] The decolorization process uses the following parameters: preheat the deacidified tea seed oil to 90°C and add natural bleaching soil (such as activated carbon). Keep stirring at 90°C for 45 minutes to ensure that the bleaching soil is fully in contact with the impurities in the oil. Decolorize the oil in a vacuum decolorization tower at a vacuum degree of -0.08MPa to remove pigments and odors in the oil. The decolorized oil is filtered through a precision filter to remove the bleaching soil and residues.
[0053] The deodorization process uses the following parameters: the decolorized oil is preheated to 180°C and further heated to 220°C by a steam heater. The oil is kept in the deodorization tower at 220°C and a vacuum of -0.09 MPa for 30 minutes to remove volatile impurities. The deodorized oil is cooled to 70°C by a cooler in preparation for the next step of treatment.
[0054] The winterization process uses the following parameters: the deodorized oil is gradually cooled to 5°C in a temperature-controlled crystallizer and kept for 24 hours to promote wax crystallization. The wax and other solid impurities are separated by centrifugation at 5°C. The centrifuged oil is further cooled to -2°C in a temperature-controlled crystallizer and kept for 12 hours to ensure complete crystallization of the wax. Finally, the remaining wax is separated again by a centrifugation to obtain a clear winterized oil.
[0055] In the present invention, the part of tea seed oil refining treatment is not a special design means, and can be replaced by other conventional active oil refining means in the specific application process of the technical solution of the present invention. This means that in the specific application process of the technical solution of the present invention, it is possible to flexibly select and replace with other conventional active oil refining means according to actual production conditions and market demand. For example, in addition to the decolorization, deodorization and winterization treatment steps described above, modern refining methods such as membrane separation technology, supercritical fluid extraction technology or silver ion refining can also be used. These methods can effectively remove impurities in oil, improve the quality of oil, and maintain the unique nutritional value and flavor of tea seed oil.
[0056] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.
[0057] Example 1
[0058] Raw material preparation and pretreatment:
[0059] Tea seed cleaning and impurity removal:
[0060] Wash the tea seeds in running water to remove impurities such as dirt, pigments, pesticide residues, etc. attached to the surface.
[0061] Tea seed shelling:
[0062] Use a camellia seed shelling machine to shell the seeds to ensure that the kernel contains less than 5% shell.
[0063] Low temperature softening of camellia oil seed kernels:
[0064] The camellia oleifera kernels were subjected to low temperature treatment at 5°C for 25 minutes.
[0065] Camellia oleifera kernel expansion:
[0066] The tea kernels were dried to a moisture content of 6%, and then subjected to microwave puffing. The puffing conditions were as follows: the tea kernels were crushed to 20 meshes; 0.5 times the weight of water was added and mixed, and then subjected to microwave puffing, the puffing time was 60 seconds, and the puffing power was 10KW.
[0067] Extraction and separation:
[0068] Preparation of composite oil extraction additives:
[0069] A composite oil extraction auxiliary agent is prepared, comprising polysorbate 80 (0.5% w / v), sodium lauryl sulfate (0.2% w / v), disodium ethylenediaminetetraacetate (0.05% w / v), and polyethylene glycol 400 (0.1% w / v): a certain amount of polysorbate 80, sodium lauryl sulfate, disodium ethylenediaminetetraacetate, and polyethylene glycol 400 are weighed according to the above proportions, and dissolved in a 70% isopropanol aqueous solution to form a desired solution concentration, thereby obtaining a composite oil extraction auxiliary agent solution.
[0070] Ultrasound-assisted extraction:
[0071] The puffed camellia oleifera kernels were mixed with the composite oil extraction aid at a ratio of 7 mL / g, and ultrasonic-assisted extraction was performed at a temperature of 60° C. using an ultrasonic power of 600 W for 120 min.
[0072] Solvent recovery and separation:
[0073] After the extraction is completed, a rotary evaporator is first used to recover 25% of the volume of the solvent at 40°C and a vacuum condition of -0.09 MPa. Subsequently, water equivalent to 4% of its volume is added to the remaining extract for mixing to promote the separation of the solvent and water. At 40°C, the mixture is separated using a centrifuge (4000 rpm, 30 min) to obtain a heavy phase (alcohol phase) and a light phase (non-polar phase).
[0074] Tea saponin extraction:
[0075] At 85°C, the alcohol phase was subjected to a rotary evaporator to recover the solvent, and the amount of solvent recovered was 70% of the volume ratio of the alcohol phase. The pH of the alcohol phase after the solvent was recovered was adjusted to 7.0; then the gas flow rate was controlled to 40m 3 / h enters the spray drying tower and obtains tea saponin powder through spray drying.
[0076] Tea seed oil refining:
[0077] At 55°C, the non-polar phase is subjected to a short-path evaporator to recover the solvent, and the amount of the recovered solvent is 75% of the volume ratio of the non-polar phase; the remaining extract (containing tea saponin) is mixed with a KOH solution with a concentration of 200 g / L and allowed to stand for 30 minutes, and then enters a disc centrifuge for separation, and the temperature of the de-soaping centrifuge is set at 65°C to obtain a crude tea seed oil.
[0078] Tea seed oil refining process: The crude tea seed oil is decolorized, deodorized and winterized to obtain the finished tea seed oil.
[0079] All operations in the experiment were carried out in a well-ventilated laboratory environment and in compliance with laboratory safety regulations.
[0080] In this embodiment, the tea seed oil refining treatment scheme is as follows:
[0081] Decolorization treatment:
[0082] Equipment: vacuum decolorization tower, precision filter.
[0083] step:
[0084] Preheat the deacidified tea seed oil to 90°C and add natural bleaching soil (such as activated carbon).
[0085] Keep stirring at 90°C for 45 minutes to ensure that the bleaching earth is fully in contact with the impurities in the oil.
[0086] Decolorization is carried out through a vacuum decolorization tower at a vacuum degree of -0.08MPa to remove pigments and odors in the oil.
[0087] The bleached oil is filtered through a precision filter to remove bleaching soil and residues.
[0088] parameter:
[0089] Temperature: 90℃.
[0090] Stirring time: 45min.
[0091] Vacuum degree: -0.08MPa.
[0092] Deodorization treatment:
[0093] Equipment: steam heater, vacuum deodorization tower, cooler.
[0094] step:
[0095] The bleached oil was preheated to 180°C and further heated to 220°C by a steam heater.
[0096] The oil was kept in the deodorization tower at 220 °C and a vacuum of -0.09 MPa for 30 min to remove volatile impurities.
[0097] The deodorized oil is cooled to 70°C in a cooler to prepare for the next step of treatment.
[0098] parameter:
[0099] Preheating temperature: 180℃.
[0100] Deodorization temperature: 220℃.
[0101] Vacuum degree: -0.09MPa.
[0102] Holding time: 30min.
[0103] Winterization treatment:
[0104] Equipment: Temperature controlled crystallizer, centrifuge.
[0105] step:
[0106] The deodorized oil was gradually cooled to 5°C in a temperature-controlled crystallizer and maintained for 24 h to promote wax crystallization.
[0107] The wax and other solid impurities were separated by centrifugation at 5°C.
[0108] The centrifuged oil was further cooled to -2 °C in a temperature-controlled crystallizer for 12 h to ensure complete crystallization of the wax.
[0109] Finally, the remaining wax is separated out by a centrifuge again to obtain clear winterized oil.
[0110] parameter:
[0111] Initial cooling: 5℃, holding time: 24h.
[0112] Centrifugation temperature: 5°C.
[0113] Further cooling: -2℃, holding time: 12h.
[0114] Example 2
[0115] Raw material preparation and pretreatment:
[0116] Tea seed cleaning and impurity removal:
[0117] Wash the tea seeds in running water to remove impurities such as dirt, pigments, pesticide residues, etc. attached to the surface.
[0118] Tea seed shelling:
[0119] Use a camellia seed shelling machine to shell the seeds to ensure that the kernel contains less than 5% shell.
[0120] Low temperature softening of camellia oil seed kernels:
[0121] The camellia oleifera kernels were subjected to low temperature treatment at 4°C for 20 minutes.
[0122] Camellia oleifera kernel expansion:
[0123] The tea kernels were dried to a moisture content of 6%, and then subjected to microwave puffing. The puffing conditions were as follows: the tea kernels were crushed to 20 meshes; 0.5 times the weight of water was added and mixed, and then subjected to microwave puffing, the puffing time was 60 seconds, and the puffing power was 10KW.
[0124] Extraction and separation:
[0125] Preparation of composite oil extraction additives:
[0126] A composite oil extraction auxiliary agent is prepared, comprising polysorbate 80 (0.5% w / v), sodium lauryl sulfate (0.2% w / v), disodium ethylenediaminetetraacetate (0.05% w / v), and polyethylene glycol 400 (0.1% w / v): a certain amount of polysorbate 80, sodium lauryl sulfate, disodium ethylenediaminetetraacetate, and polyethylene glycol 400 are weighed according to the above proportions, and dissolved in a 70% isopropanol aqueous solution to form a desired solution concentration, thereby obtaining a composite oil extraction auxiliary agent solution.
[0127] Ultrasound-assisted extraction:
[0128] The puffed camellia oleifera kernels were mixed with the composite oil extraction aid at a ratio of 7 mL / g, and ultrasonic-assisted extraction was performed at a temperature of 60° C. using an ultrasonic power of 600 W for 120 min.
[0129] Solvent recovery and separation:
[0130] After the extraction is completed, a rotary evaporator is first used to recover 25% of the volume of the solvent at 40°C and a vacuum condition of -0.09 MPa. Subsequently, water equivalent to 4% of its volume is added to the remaining extract for mixing to promote the separation of the solvent and water. At 40°C, the mixture is separated using a centrifuge (4000 rpm, 30 min) to obtain a heavy phase (alcohol phase) and a light phase (non-polar phase).
[0131] Tea saponin extraction:
[0132] At 85°C, the alcohol phase was subjected to a rotary evaporator to recover the solvent, and the amount of solvent recovered was 70% of the volume ratio of the alcohol phase. The pH of the alcohol phase after the solvent was recovered was adjusted to 7.0; then the gas flow rate was controlled to 40m 3 / h enters the spray drying tower and obtains tea saponin powder through spray drying.
[0133] Tea seed oil refining:
[0134] At 55°C, the non-polar phase is subjected to a short-path evaporator to recover the solvent, and the amount of the recovered solvent is 75% of the volume ratio of the non-polar phase; the remaining extract (containing tea saponin) is mixed with a KOH solution with a concentration of 200 g / L and allowed to stand for 30 minutes, and then enters a disc centrifuge for separation, and the temperature of the de-soaping centrifuge is set at 65°C to obtain a crude tea seed oil.
[0135] Tea seed oil refining process: The crude tea seed oil is decolorized, deodorized and winterized to obtain the finished tea seed oil.
[0136] The tea seed oil refining treatment scheme in this embodiment is the same as that in Example 1.
[0137] Comparative Example
[0138] Raw material preparation and pretreatment:
[0139] Tea seed cleaning and impurity removal:
[0140] Wash the tea seeds in running water to remove impurities such as dirt, pigments, pesticide residues, etc. attached to the surface.
[0141] Tea seed shelling:
[0142] Use a camellia seed shelling machine to shell the seeds to ensure that the kernel contains less than 5% shell.
[0143] Low temperature softening of camellia oil seed kernels:
[0144] The camellia oleifera kernels were subjected to low temperature treatment at 4°C for 20 minutes.
[0145] Camellia oleifera kernel expansion:
[0146] The tea kernels were dried to a moisture content of 6%, and then subjected to microwave puffing. The puffing conditions were as follows: the tea kernels were crushed to 20 meshes; 0.5 times the weight of water was added and mixed, and then subjected to microwave puffing, the puffing time was 60 seconds, and the puffing power was 10KW.
[0147] Extraction and separation:
[0148] Preparation of oil extraction auxiliary agent: using n-hexane.
[0149] Ultrasound-assisted extraction:
[0150] The puffed camellia oleifera kernels were mixed with n-hexane at a ratio of 7 mL / g, and ultrasonic-assisted extraction was performed at a temperature of 60° C. using an ultrasonic power of 600 W for 120 min.
[0151] Solvent recovery and separation:
[0152] After the extraction is completed, a rotary evaporator is first used to recover 25% of the volume of the solvent at 40°C and a vacuum condition of -0.09 MPa. Subsequently, 4% of the volume of water is added to the remaining extract for mixing to facilitate the separation of the solvent and water. At 40°C, the mixture is separated using a centrifuge to obtain a heavy phase (alcohol phase) and a light phase (non-polar phase).
[0153] Tea saponin extraction:
[0154] At 85°C, the alcohol phase was subjected to a rotary evaporator to recover the solvent, and the amount of solvent recovered was 70% of the volume ratio of the alcohol phase. The pH of the alcohol phase after the solvent was recovered was adjusted to 7.0; then the gas flow rate was controlled to 40m 3 / h enters the spray drying tower and obtains tea saponin powder through spray drying.
[0155] Tea seed oil refining:
[0156] At 55°C, the non-polar phase is subjected to a short-path evaporator to recover the solvent, and the amount of the recovered solvent is 75% of the volume ratio of the non-polar phase; the remaining extract (containing tea saponin) is mixed with a KOH solution with a concentration of 200 g / L and allowed to stand for 30 minutes, and then enters a disc centrifuge for separation, and the temperature of the de-soaping centrifuge is set at 65°C to obtain a crude tea seed oil.
[0157] Tea seed oil refining process: The crude tea seed oil is decolorized, deodorized and winterized to obtain the finished tea seed oil.
[0158] The tea seed oil refining treatment scheme in this comparative example is the same as that in Example 1.
[0159] Experimental example
[0160] The extraction rate and purity of tea seed oil and tea saponin in Example 1 and Comparative Example 1 were tested:
[0161] Extraction rate and purity test method:
[0162] Tea seed oil extraction rate and purity:
[0163] Extraction yield: Determined by gravimetric method.
[0164] Purity: The proportion of unsaturated fatty acids in the oil was determined by gas chromatography (GC).
[0165] Tea saponin extraction rate and purity:
[0166] Extraction yield: Determined by gravimetric method.
[0167] Purity: The purity of tea saponin was determined by high performance liquid chromatography (HPLC).
[0168] Significance analysis:
[0169] Student's t-test or analysis of variance (ANOVA) was used to compare the significant differences between the two groups of data.
[0170] Each group was sampled five times, and the obtained samples were tested. The experimental results are shown in Table 1 below:
[0171] Table 1 Test data results
[0172]
[0173] Significance analysis results:
[0174] Through t-test or ANOVA analysis, Example 1 was significantly higher than Comparative Example 1 in extraction rate and purity of tea seed oil and tea saponin (P<0.05).
[0175] It can be seen from the test results that the present invention has achieved significant optimization in the purity and extraction rate of tea seed oil and tea saponin.
[0176] In summary, the present invention provides a method for efficiently extracting tea seed oil and tea saponin from tea seeds. By optimizing the extraction conditions, such as using a specific composite oil extraction auxiliary agent, controlling the power and time of ultrasonic-assisted extraction, and subsequent refining treatment, the extraction rate and purity of tea seed oil and tea saponin are significantly improved. The experimental results show that compared with the traditional method, the method of the present invention has obvious advantages in the extraction efficiency and product quality of tea seed oil and tea saponin.
[0177] In the process of implementing the present invention, attention is paid to environmental protection and sustainable utilization of resources. For example, the solvent and water used in the extraction process can be recycled and reused, reducing pollution to the environment. At the same time, by optimizing the extraction process, energy consumption and waste generation are reduced, which is in line with the development concept of green chemistry and circular economy.
[0178] The extraction method of the present invention improves the utilization rate of raw materials, reduces production costs, and increases the added value of products. By improving the extraction rate and purity of tea seed oil and tea saponin, higher quality products can be produced to meet the growing market demand for high-quality natural products, thereby bringing greater economic benefits to enterprises.
[0179] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.
Claims
1. A method for simultaneously extracting tea seed oil and tea saponin from tea seeds, characterized in that: The following steps are involved: The tea seeds are sequentially subjected to shelling treatment, low temperature treatment and puffing treatment to obtain puffed material; The expanded material is mixed with a composite oil extraction auxiliary agent, and subjected to ultrasonic treatment to obtain an ultrasonic product; The ultrasonic product is centrifuged to obtain a heavy phase and a light phase; The heavy phase is separated from the solvent and then spray-dried to obtain tea saponin; Separating the solvent from the light phase and mixing it with an alkali solution, treating it with an alkali reagent, and centrifuging it to obtain a crude tea seed oil product; The crude tea seed oil is refined to obtain tea seed oil.
2. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The composite oil extraction auxiliary agent contains polysorbate 80, sodium lauryl sulfate, disodium ethylenediaminetetraacetate and polyethylene glycol 400.
3. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The solvent of the composite oil extraction auxiliary agent is isopropanol solution.
4. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 2, characterized in that: The final concentration of polysorbate 80 in the composite oil extraction auxiliary agent is 0.3-0.8% w / v; The final concentration of sodium dodecyl sulfate in the composite oil extraction auxiliary agent is 0.1-0.3% w / v; The final concentration of disodium ethylenediaminetetraacetate in the composite oil extraction auxiliary agent is 0.03-0.08% w / v; The final concentration of polyethylene glycol 400 in the composite oil extraction auxiliary agent is 0.05-0.15% w / v.
5. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 3, characterized in that: The initial concentration of the isopropanol solution is 60-80%.
6. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The temperature of the low-temperature treatment is 40°C to 60°C; the time of the low-temperature treatment is 20min to 30min; the moisture content of the puffing treatment is 5% to 7%; the crushing particle size of the puffing treatment is 15 mesh to 25 mesh; the amount of water added in the puffing treatment is 0.3 times to 0.7 times the weight of the camellia oleifera seed kernel; the microwave power of the puffing treatment is 8KW to 12KW; and the time of the puffing treatment is 50 seconds to 70 seconds.
7. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The temperature of the ultrasonic treatment is 55° C. to 65° C.; the power of the ultrasonic treatment is 500W to 700W; and the time of the ultrasonic treatment is 100min to 140min.
8. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The temperature of the separation solvent is 35°C to 45°C; the vacuum degree of the separation solvent is -0.08Mpa to -0.1Mpa; the solvent recovery volume of the separation solvent is 20% to 30% of the volume of the extract; the separation solvent includes adding water, and the water volume is 3% to 5% of the volume of the extract; the centrifugal speed of the separation is 3500rpm to 4500rpm; the centrifugal time of the separation is 25min to 35min.
9. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The gas velocity flow rate of the spray drying is 35m 3 / h~45m 3 / h.
10. The method for simultaneously extracting tea seed oil and tea saponin from tea seeds according to claim 1, characterized in that: The alkaline solution is a KOH solution; the concentration of the KOH solution is 150 g / L to 250 g / L; the treatment time of the alkaline reagent is 25 min to 35 min; the refining treatment includes decolorization treatment, deodorization treatment and winterization treatment.
Citation Information
Patent Citations
Simple method for purifying tea saponin
CN106188214A
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