CN112316484A - Method for extracting camellia oleifera polyphenol from tea oil - Google Patents
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- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
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- B01D11/02—Solvent extraction of solids
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- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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Abstract
The invention relates to the technical field of oil tea fruit extraction, in particular to a method for extracting oil tea polyphenol from oil tea, which adopts supercritical removal of the oil tea from oil tea seeds and then further extraction of the oil tea polyphenol, thereby improving the extraction rate of the oil tea polyphenol. In addition, the process adopts the deoiled tea seeds and the oil tea shells as raw materials to extract the oil tea polyphenol, the utilization rate of the raw materials is fully improved, in addition, the oil tea polyphenol is extracted by taking the shells as one of the raw materials in the process, so that the utilization rate of resources is improved, the whole process is simple, the solvent pollution is avoided, the use amount is small, and the green and environment-friendly effects are realized.
Description
Technical Field
The invention relates to the technical field of oil tea fruit extraction, in particular to a method for extracting oil tea polyphenol from tea oil.
Background
Camellia oleifera is a plant of the Theaceae family, and is called four woody oil plants in the world together with olive oil, coconut and oil palm. The unsaturated fatty acid content of the tea oil extracted from the camellia seeds reaches over 90 percent, and the tea oil has the reputation of the oriental olive oil. The oil-tea camellia cake after oil extraction contains various active substances such as saponin, polyphenol, squalene, polysaccharide, protein and the like, so that the oil-tea camellia has high comprehensive utilization value.
The camellia oleifera shells and the camellia seeds contain camellia oleifera polyphenols, and the content of the camellia oleifera shells is relatively high. Research shows that the oil tea polyphenol can eliminate active oxygen free radicals, block lipid peroxidation process, improve activity of enzyme in human body, and has the effects of resisting mutation, cancer and aging. Secondly, the tea-oil polyphenol can eliminate the accumulation of cholesterol on the arterial vessel wall by increasing the content of high-density lipoprotein cholesterol, thereby playing the roles of reducing blood pressure, reducing blood fat, preventing diseases such as atherosclerosis, myocardial infarction and the like. In addition, the oil tea polyphenol also has the effect of improving the comprehensive immunity of human bodies, and is widely applied to the industries of medical health care products, cosmetics and foods. Therefore, the camellia oleifera polyphenol has potential development and utilization values.
At present, the methods for extracting the oil tea polyphenol mainly comprise a solvent method, a precipitation method and an adsorption method. Although the solvent method has simple process and is suitable for large-scale production, the production period is long, the temperature is high, the tea polyphenol is easy to oxidize and inactivate, and meanwhile, a large amount of organic solvent is used in the production process, so that the operation is not safe enough, the environment is polluted, and the development direction of green chemistry is not met; the precipitation method mainly utilizes metal ions and polyphenol to form a complex, the complex is precipitated from a solution and then dissolved by acid, so that the polyphenol is dissociated from the precipitate, and the method has larger amount of organic solvent and is doped with metal ions; the adsorption method mainly comprises the steps of extracting tea polyphenol by using an organic solvent, and then adsorbing and separating the tea polyphenol by using resin, wherein the subsequent separation is relatively complicated, and the extraction method of the tea polyphenol mainly comprises solvent extraction, and can also be used for extracting the tea polyphenol by using ultrasonic waves or microwaves. Substances such as oil tea saponin, polyphenol and the like can be obtained while the solvent is used for extracting the oil tea polyphenol, so that the separation and purification of the extracting solution and the obtaining of the purer oil tea polyphenol have important significance.
Disclosure of Invention
The invention aims to solve the problem of providing a method for extracting the camellia oleifera polyphenol from the camellia oleifera oil, which has the advantages of simple process, no solvent pollution, small usage amount, environmental protection and environmental protection.
In order to solve the technical problems, the invention adopts the technical scheme that: a method for extracting camellia oleifera polyphenol from camellia oil comprises the following steps:
the method comprises the following steps: respectively drying camellia seeds and camellia shells obtained by removing the shells of camellia fruits to ensure that the water content is lower than 4 percent;
step two: respectively crushing the dried camellia seeds and the dried camellia shells to 20 meshes for later use;
step three: adding the camellia seed powder into an extraction kettle, removing the tea oil for 1.5-4h, feeding the CO discharged from the extraction kettle into a separation tank at a flow rate, separating, and obtaining the tea oil in the separation tank;
step four: after the camellia seed subjected to tea oil removal in the third step or the crushed fruit shell obtained in the second step is mixed with 20% -80% ethanol water solution according to the proportion that l-30ml of ethanol water solution is added into each gram of raw material, stirring and extracting are carried out for 30-180min at the temperature of 30-80 ℃ T, so as to obtain a camellia polyphenol extracting solution, and then the camellia polyphenol crude extract is obtained through rotary evaporation, wherein the mass content of camellia polyphenol is 5-8%;
step five: dissolving the crude extract of the oil tea polyphenol obtained in the step four in water to prepare an aqueous solution of the crude extract of the oil tea polyphenol with the concentration of the crude extract of the oil tea polyphenol of 0.1-lmg/mL, and adjusting the pH to 1-7 by adopting a 0.Imol/LHC1 solution for later use;
step six: adding the aqueous solution of the camellia oleifera polyphenol crude extract from the upper end of an adsorption column at the speed of 1.0-5.OBV/h, wherein the addition amount of the aqueous solution of the camellia oleifera polyphenol crude extract is 2-6 times of the column volume, when the concentration of effluent flowing through the adsorption column is not changed, the resin adsorption is saturated, rinsing the resin subjected to adsorption saturation for 1-2 times at the flow rate of 600mL/h by using deionized water to remove impurities, collecting washing liquid, performing gradient elution by using ethanol solution respectively, collecting the eluent, and performing reduced pressure rotary evaporation on the eluent at 45 ℃ to obtain a purified camellia oleifera polyphenol product with the mass content of 43-75%;
step seven: and (3) carrying out reduced pressure evaporation on the oil-containing tea polyphenol product to obtain a light yellow powdery solid.
Further, the extraction conditions of the extraction kettle are as follows: the pressure is 15-45MPa, the temperature is 35-65 ℃, and the flow rate of C0 is 30-150L/h.
Further, in the third step, the separation includes a first stage separation and a second stage separation.
Further, the first-stage separation is carried out at a temperature of 35-65 ℃ and a pressure of 10-20 MPa.
Further, the secondary separation is carried out at a temperature of 20-40 ℃ and a pressure of 4-7 MPa.
Further, the pretreatment step of the macroporous resin is as follows: soaking in ethanol for 24h to remove residual organic solvent including pore-forming agent in the resin, soaking in NaOH aqueous solution, and washing with water to neutrality; then soaking the mixture in HC1 water solution, washing the mixture with deionized water to neutrality, drying the mixture at 100 deg.c, and loading the dried macroporous adsorption resin into adsorption column.
Furthermore, the adsorption time is 1-4h at the adsorption temperature of 25-45 ℃.
Further, the elution conditions are as follows: desorbing with 0-80% ethanol solution at flow rate of 0.5-5.0BV/h from top to bottom at 25-45 deg.C for 1-4h, and collecting the eluate with a collector.
Compared with the prior art, the invention has the advantages and positive effects that:
according to the method, the tea oil in the camellia seeds is removed through supercritical extraction, and then the camellia polyphenol is further extracted, so that the extraction rate of the camellia polyphenol is improved, the crude extract solution of the camellia polyphenol is separated and purified through macroporous adsorption resin, the process is simple compared with a liquid-liquid solvent purification method, no solvent pollution is caused, the method is more environment-friendly, the purity of the obtained camellia polyphenol is high, the mass content of the obtained camellia polyphenol can reach more than 78%, and the method is higher than the liquid-liquid solvent purification method. In addition, the process adopts the deoiled tea seeds and the oil tea shells as raw materials to extract the oil tea polyphenol, the utilization rate of the raw materials is fully improved, in addition, the oil tea polyphenol is extracted by taking the shells as one of the raw materials in the process, so that the utilization rate of resources is improved, the whole process is simple, the solvent pollution is avoided, the use amount is small, and the green and environment-friendly effects are realized.
Detailed Description
For a better understanding of the present invention, the present invention is further described below in conjunction with specific embodiments.
Pre-treating the macroporous resin: soaking in ethanol for 24h to remove residual organic solvent including pore-forming agent in the resin, soaking in NaOH aqueous solution, and washing with water to neutrality; then soaking the mixture in HC1 water solution, washing the mixture with deionized water to neutrality, drying the mixture at 100 deg.c, and loading the dried macroporous adsorption resin into adsorption column.
Example 1:
the method comprises the following steps: respectively drying camellia seeds and camellia shells obtained by removing the shells of camellia fruits to ensure that the water content is lower than 4 percent;
step two: respectively crushing the dried camellia seeds and the dried camellia shells to 20 meshes for later use;
step three: adding the camellia seed powder into an extraction kettle, extracting under the conditions that the pressure is 15MPa, the temperature is 35 ℃ and the flow rate of C0 is 30L/h, removing the tea oil for 1.5h, feeding the flow rate of CO discharged from the extraction kettle into a separation tank, and separating, wherein the separation comprises primary separation and secondary separation, the primary separation is carried out at the temperature of 35 ℃ and the pressure of 10MPa, the secondary separation is carried out at the temperature of 20 ℃ and the pressure of 4MPa, and the tea oil is obtained in the separation tank;
step four: mixing the camellia seed subjected to tea oil removal in the third step or the crushed fruit shell obtained in the second step with 20% ethanol aqueous solution according to the proportion that 30ml of ethanol aqueous solution is added into each gram of raw material, stirring and extracting at the temperature of 30 ℃ T for 30min to obtain a camellia polyphenol extracting solution, and performing rotary evaporation to obtain a camellia polyphenol crude extract, wherein the mass content of camellia polyphenol is 5%;
step five: dissolving the crude extract of the camellia oleifera polyphenol obtained in the step four in water to prepare an aqueous solution of the crude extract of the camellia oleifera polyphenol with the concentration of the crude extract of the camellia oleifera polyphenol of 0.1mg/mL, and adjusting the pH to 7 by adopting a 0.Imol/LHC1 solution for later use;
step six: pretreating, adding the water solution of the oil tea polyphenol crude extract from the upper end of an adsorption column at the speed of 1BV/h, adsorbing at the temperature of 25 ℃ for 1-4h, wherein the water solution adding amount of the crude oil tea polyphenols extract is 2 times of the column volume, when the concentration of effluent flowing through the adsorption column is not changed, the resin adsorption is saturated, rinsing the resin saturated by adsorption for 1 time at the flow rate of 600mL/h by using deionized water to remove impurities, collecting washing liquid, performing gradient elution by using ethanol solution respectively, desorbing by using 0%, 20%, 40%, 60% and 80% ethanol solution at the flow rate of 0.5BV/h from top to bottom at the desorption temperature of 25 ℃ for 1h, collecting the eluent by a collector, and performing reduced pressure rotary evaporation on the eluent at 45 ℃ to obtain a purified oil tea polyphenol product with the mass content of 43%;
step seven: and (3) carrying out reduced pressure evaporation on the oil-containing tea polyphenol product to obtain a light yellow powdery solid serving as an experimental group A.
Example 2:
the first step and the second step are the same as the example 1;
step three: adding the camellia seed powder into an extraction kettle, extracting under the conditions that the pressure is 45MPa, the temperature is 65 ℃ and the flow rate of C0 is 150L/h, removing the camellia oil for 4h, feeding the flow rate of CO discharged from the extraction kettle into a separation tank, and separating, wherein the separation comprises primary separation and secondary separation, the primary separation is carried out at the temperature of 65 ℃ and the pressure of 20MPa, the secondary separation is carried out at the temperature of 40 ℃ and the pressure of 7MPa, and the camellia oil is obtained in the separation tank;
step four: mixing the camellia seed subjected to tea oil removal in the third step or the crushed fruit shell obtained in the second step with 80% ethanol aqueous solution according to the proportion of 30ml of ethanol aqueous solution added into each gram of raw material, stirring and extracting at the temperature of 80 ℃ T for 180min to obtain a camellia polyphenol extracting solution, and performing rotary evaporation to obtain a camellia polyphenol crude extract, wherein the mass content of camellia polyphenol is 8%;
step five: dissolving the crude oil tea polyphenol extract obtained in the step four in water to prepare an aqueous solution of the crude oil tea polyphenol extract containing oil tea polyphenol with the concentration of lmg/mL, and adjusting the pH to 5 by adopting a 0.Imol/LHC1 solution for later use;
step six: pretreating, adding the water solution of the camellia polyphenol crude extract from the upper end of an adsorption column at the speed of 5BV/h, wherein the adsorption temperature is 45 ℃, the adsorption time is 4h, wherein the water solution adding amount of the crude oil tea polyphenols extract is 6 times of the column volume, and the resin adsorption is saturated when the concentration of the effluent flowing through the adsorption column is not changed, rinsing the resin saturated by adsorption for 2 times at the flow rate of 600mL/h by using deionized water to remove impurities, collecting washing liquid, performing gradient elution by using ethanol solution respectively, desorbing by using 0%, 20%, 40%, 60% and 80% ethanol solution at the flow rate of 5BV/h, the desorption temperature of 45 ℃ and the desorption time of 4h from top to bottom, collecting the eluent by a collector, and performing reduced pressure rotary evaporation on the eluent at 45 ℃ to obtain a purified oil tea polyphenol product with the mass content of 47%;
the procedure is as in example 1 to give a pale yellow powdery solid as test group B.
Example 3:
the first step and the second step are the same as the example 1;
step three: adding the camellia seed powder into an extraction kettle, extracting under the conditions that the pressure is 30MPa, the temperature is 45 ℃ and the flow rate of C0 is 120L/h, removing the camellia oil for 3h, feeding the flow rate of CO discharged from the extraction kettle into a separation tank, and separating, wherein the separation comprises primary separation and secondary separation, the primary separation is carried out at the temperature of 45 ℃ and the pressure of 15MPa, the secondary separation is carried out at the temperature of 30 ℃ and the pressure of 5MPa, and the camellia oil is obtained in the separation tank;
step four: mixing the camellia seed subjected to tea oil removal in the third step or the crushed fruit shell obtained in the second step with 50% ethanol aqueous solution according to the proportion that 15ml of ethanol aqueous solution is added into each gram of raw material, stirring and extracting at 50 ℃ T for 120min to obtain a camellia polyphenol extracting solution, and performing rotary evaporation to obtain a camellia polyphenol crude extract, wherein the mass content of camellia polyphenol is 7%;
step five: dissolving the crude extract of the camellia oleifera polyphenol obtained in the step four in water to prepare an aqueous solution of the crude extract of the camellia oleifera polyphenol with the concentration of the crude extract of the camellia oleifera polyphenol of 0.6mg/mL, and adjusting the pH to 5 by adopting a 0.Imol/LHC1 solution for later use;
step six: pretreating, adding the water solution of the oil tea polyphenol crude extract from the upper end of an adsorption column at the speed of 1.0-5.OBV/h, adsorbing at 35 deg.C for 2h, wherein the water solution adding amount of the crude oil tea polyphenols extract is 3 times of the column volume, and the resin adsorption is saturated when the concentration of the effluent flowing through the adsorption column is not changed, rinsing the resin saturated by adsorption for 1-2 times at a flow rate of 600mL/h by using deionized water to remove impurities, collecting a washing solution, performing gradient elution by using an ethanol solution, desorbing and desorbing by using 0%, 20%, 40%, 60% and 80% ethanol solution at a flow rate of 3BV/h at a desorption temperature of 35 ℃ for 3h from top to bottom, collecting the eluent by a collector, and performing reduced pressure rotary evaporation on the eluent at 45 ℃ to obtain a purified oil tea polyphenol product with the mass content of 75%;
the procedure is as in example 1 to give a pale yellow powdery solid as test group C.
Example 4:
the first step and the second step are the same as the example 1;
mixing oil tea seeds and crushed fruit shells with 20% ethanol aqueous solution according to the proportion that 30ml ethanol aqueous solution is added into each gram of raw material, stirring and extracting for 30min at the temperature of 30 ℃ T to obtain oil tea polyphenol extracting solution, performing rotary evaporation to obtain oil tea polyphenol crude extract, and performing reduced pressure evaporation on the oil tea polyphenol-containing product to obtain light yellow powdery solid serving as a control group.
Example 5:
the oil tea fruit raw material extraction with the same quality is measured, the obtained oil tea polyphenol crude extract is detected and analyzed by adopting an ultraviolet spectrophotometer according to GB/T8313-2008, and the result is shown in Table 1.
Table 1: content of polyphenol of oil tea
| Experimental group A | Experimental group B | Experimental group C | Control group | |
| Content (wt.) | 48.3％ | 52.1％ | 26.7％ | 76.2％ |
As can be seen from table 1, according to the method, the tea oil in the camellia seeds is removed through supercritical extraction, and then the camellia polyphenol is further extracted, so that the extraction rate of the camellia polyphenol is improved, the crude extract solution of the camellia polyphenol is separated and purified through macroporous adsorption resin, the process is simple, no solvent pollution is caused, the method is more environment-friendly, and the obtained camellia polyphenol has high purity, the mass content of the camellia polyphenol can reach more than 78%, and the method is higher than the liquid-liquid solvent purification method. In addition, the process adopts the deoiled tea seeds and the oil tea shells as raw materials to extract the oil tea polyphenol, the utilization rate of the raw materials is fully improved, in addition, the oil tea polyphenol is extracted by taking the shells as one of the raw materials in the process, so that the utilization rate of resources is improved, the whole process is simple, the solvent pollution is avoided, the use amount is small, and the green and environment-friendly effects are realized.
The embodiments of the present invention have been described in detail, but the description is only for the preferred embodiments of the present invention and should not be construed as limiting the scope of the present invention. All equivalent changes and modifications made within the scope of the present invention should be covered by the present patent.
Claims (8)
1. A method for extracting tea-oil polyphenol from tea oil is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: respectively drying camellia seeds and camellia shells obtained by removing the shells of camellia fruits to ensure that the water content is lower than 4 percent;
step two: respectively crushing the dried camellia seeds and the dried camellia shells to 20 meshes for later use;
step three: adding the camellia seed powder into an extraction kettle, removing the tea oil for 1.5-4h, feeding the CO discharged from the extraction kettle into a separation tank at a flow rate, separating, and obtaining the tea oil in the separation tank;
step four: after the camellia seed subjected to tea oil removal in the third step or the crushed fruit shell obtained in the second step is mixed with 20% -80% ethanol water solution according to the proportion that l-30ml of ethanol water solution is added into each gram of raw material, stirring and extracting are carried out for 30-180min at the temperature of 30-80 DEG CT, a camellia polyphenol extracting solution is obtained, and then the camellia polyphenol crude extract is obtained through rotary evaporation, wherein the mass content of camellia polyphenol is 5-8%;
step five: dissolving the crude extract of the oil tea polyphenol obtained in the step four in water to prepare an aqueous solution of the crude extract of the oil tea polyphenol with the concentration of the crude extract of the oil tea polyphenol of 0.1-lmg/mL, and adjusting the pH to 1-7 by adopting a 0.Imol/LHC1 solution for later use;
step six: adding the aqueous solution of the camellia oleifera polyphenol crude extract from the upper end of an adsorption column at the speed of 1.0-5.OBV/h, wherein the addition amount of the aqueous solution of the camellia oleifera polyphenol crude extract is 2-6 times of the column volume, when the concentration of effluent flowing through the adsorption column is not changed, the resin adsorption is saturated, rinsing the resin subjected to adsorption saturation for 1-2 times at the flow rate of 600mL/h by using deionized water to remove impurities, collecting washing liquid, performing gradient elution by using ethanol solution respectively, collecting the eluent, and performing reduced pressure rotary evaporation on the eluent at 45 ℃ to obtain a purified camellia oleifera polyphenol product with the mass content of 43-75%;
step seven: and (3) carrying out reduced pressure evaporation on the oil-containing tea polyphenol product to obtain a light yellow powdery solid.
2. The method for extracting camellia polyphenol from camellia oil according to claim 1, wherein the method comprises the following steps: the extraction conditions of the extraction kettle are as follows: the pressure is 15-45MPa, the temperature is 35-65 ℃, and the flow rate of C0 is 30-150L/h.
3. The method for extracting camellia polyphenol from camellia oil according to claim 1, wherein the method comprises the following steps: in the third step, the separation comprises primary separation and secondary separation.
4. The method for extracting camellia polyphenol from camellia oil as claimed in claim 3, wherein: the first-stage separation is carried out at a temperature of 35-65 ℃ and a pressure of 10-20 MPa.
5. The method for extracting camellia polyphenol from camellia oil as claimed in claim 3, wherein: the second stage separation is carried out at a temperature of 20-40 ℃ and a pressure of 4-7 MPa.
6. The method for extracting camellia polyphenol from camellia oil according to claim 1, wherein the method comprises the following steps: the pretreatment steps of the macroporous resin are as follows: soaking in ethanol for 24 hr to remove residual organic solvent containing pore-forming agent, soaking in NaOH aqueous solution, washing with water to neutrality, soaking in HC1 aqueous solution, washing with deionized water to neutrality, drying at 100 deg.C, and loading the dried macroporous adsorbent resin into adsorption column.
7. The method for extracting camellia polyphenol from camellia oil according to claim 1, wherein the method comprises the following steps: the adsorption temperature is 25-45 ℃ and the adsorption time is 1-4 h.
8. The method for extracting camellia polyphenol from camellia oil according to claim 1, wherein the method comprises the following steps: the elution conditions were: desorbing with 0-80% ethanol solution at flow rate of 0.5-5.0BV/h from top to bottom at 25-45 deg.C for 1-4h, and collecting the eluate with a collector.
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