CN108434182B - Supercritical CO2Method for extracting seabuckthorn leaf polyphenol by fluid extraction technology - Google Patents
Supercritical CO2Method for extracting seabuckthorn leaf polyphenol by fluid extraction technology Download PDFInfo
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- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 40
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 40
- 235000003145 Hippophae rhamnoides Nutrition 0.000 title claims abstract description 34
- 238000000605 extraction Methods 0.000 title claims description 74
- 239000012530 fluid Substances 0.000 title claims description 17
- 240000000950 Hippophae rhamnoides Species 0.000 title description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 63
- 241000229143 Hippophae Species 0.000 claims abstract description 46
- 239000000284 extract Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims description 32
- 238000002791 soaking Methods 0.000 claims description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 18
- 235000003935 Hippophae Nutrition 0.000 claims description 16
- 238000011084 recovery Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 abstract description 6
- 239000003963 antioxidant agent Substances 0.000 abstract description 4
- 230000003078 antioxidant effect Effects 0.000 abstract description 4
- 238000002360 preparation method Methods 0.000 abstract description 4
- 230000002378 acidificating effect Effects 0.000 abstract description 2
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 abstract description 2
- 230000007760 free radical scavenging Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 8
- 239000000126 substance Substances 0.000 description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 238000002137 ultrasound extraction Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- -1 shiitake mushroom Chemical class 0.000 description 3
- 241001117772 Elaeagnaceae Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- 240000000599 Lentinula edodes Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 244000248825 Peltandra virginica Species 0.000 description 1
- 235000001188 Peltandra virginica Nutrition 0.000 description 1
- 235000008599 Poria cocos Nutrition 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 230000032677 cell aging Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 201000005577 familial hyperlipidemia Diseases 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 201000001421 hyperglycemia Diseases 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000011550 stock solution Substances 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 238000009777 vacuum freeze-drying Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A61K2236/50—Methods involving additional extraction steps
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Abstract
The invention discloses a preparation method of a sea buckthorn polyphenol extract, which specifically adopts a sea buckthorn leaf raw material soaked in an acidic ethanol solution and CO2By means of supercritical extraction, IC with total antioxidant capacity and DPPH free radical scavenging rate compared with the prior art can be obtained50Higher polyphenol extracts.
Description
Technical Field
The invention relates to a method for extracting chemical components, in particular to a method for extracting seabuckthorn leaf polyphenol, and especially relates to supercritical CO2A method for extracting folium Hippophae polyphenol with fluid is provided.
Background
Hippophae rhamnoides (Hippophae rhamnoides L.) is a shrub or small tree of the genus Hippophae of the family Elaeagnaceae (Elaeagnaceae). The sea-buckthorn is widely planted in China, and roots, stems, leaves, flowers and fruits of the sea-buckthorn contain more than 200 nutrient substances, so that the sea-buckthorn becomes an economic tree species which is greatly developed in the three north areas of China and has excellent water and soil conservation. The folium Hippophae as waste contains abundant polyphenols, is the main active ingredient of folium Hippophae, and has good effects in preventing and treating hyperglycemia, hyperlipemia, cancer, cell aging, etc.
Water extraction, microwave extraction, ultrasonic extraction and the like are adopted by researchers in the past to extract the seabuckthorn leaf polyphenol, and the traditional extraction methods are time-consuming in operation and can cause undesirable results such as reduction of the activity of the seabuckthorn leaf polyphenol extract.
Supercritical fluid extraction is an emerging extraction technology that takes advantage of the specific properties of fluids in the vicinity of the critical point. Supercritical CO2The liquid is the most commonly used fluid which is neither liquid nor gas, but has the properties of high density of liquid and low viscosity of gas, thereby having higher dissolving capacity and higher diffusion performance, and being capable of being fully mixed and contacted with a sample to exert the dissolving capacity to the maximum extent. In order to improve the selectivity of some polar substances, supercritical CO is often adopted2Adding proper entrainer (or modifier) into the extraction system, wherein the common entrainer is methanol, ethanol, acetone, ethyl acetate, water and the like, and improving CO by using the entrainer2Fluid solubility properties such that supercritical CO2It is possible to extract substances with strong polarity such as polyphenol.
Although using supercritical CO2The research of extracting some plant polysaccharides (such as shiitake mushroom, tuckahoe, etc.) by fluid extraction technology has been reported, but supercritical CO is adopted2The research of extracting the seabuckthorn leaf polyphenol by the fluid extraction technology has not been reported.
Therefore, the research aims at preparing the high-activity seabuckthorn leaf polyphenol by adopting supercritical CO added with the entrainer2The extraction method for extracting the seabuckthorn leaf polyphenol provides guidance for reasonably utilizing the seabuckthorn leaf resource with rich biomass and preparing the high-activity seabuckthorn leaf polyphenol.
Disclosure of Invention
The invention aims to provide a high-efficiency supercritical CO by taking seabuckthorn leaves which are abundant in resources in China and not effectively developed and utilized as plant materials2A method for extracting folium Hippophae polyphenol with fluid is provided.
1. Supercritical CO2A method for preparing a seabuckthorn leaf polyphenol extract from a fluid, comprising the steps of:
(1) mixing folium Hippophae powder crushed to 20 meshes with ethanol solution, soaking overnight (10-24h) to obtain soaking material, filling the soaking material in an extraction kettle of 300 ml, wherein the volume ratio of the folium Hippophae powder to the ethanol solution is 1:1, the ethanol solution is ethanol water solution with volume fraction of 60%, the volume unit of the ethanol solution is ml, and the mass unit of the folium Hippophae powder sample is g; the pH of the 60% ethanol water solution is 3-4.
(2) Fixing the filled extraction kettle in a heating box, connecting interfaces at two ends of the extraction kettle when all air valves in the system are in a closed state, and closing a door of the heating box, wherein all the air valves comprise an air inlet switch, an air outlet valve and a fine adjustment valve;
(3) opening supercritical CO2The fluid extraction equipment power supply is used for setting the temperature of the extraction kettle and the temperature of the fine adjustment valve, when the temperature reaches a set value, the air inlet switch is opened to adjust the pressure of the extraction kettle, and when the pressure of the extraction kettle reaches a set condition, the pressure is kept for 5min under the condition, wherein the temperature of the extraction kettle is 40 ℃, the temperature of the fine adjustment valve is 90 ℃, and the pressure of the extraction kettle is 30 MPa;
(4) opening the gas outlet valve, controlling the gas flow in the recovery bottle by using a fine-tuning valve, enabling the tail-connected flow meter to display the flow to be 2L/min, balancing the pressure of the extraction kettle by using a carbon dioxide pneumatic pump, keeping the pressure of the extraction kettle constant, opening an entrainer pump, controlling the flow velocity of the entrainer, closing a gas inlet switch after the extraction time is up, and enabling CO in the extraction kettle to be discharged2Discharging, recovering the extract in a recovery bottle until CO is discharged2Emptying, and taking down a recovery bottle, wherein the entrainer is an ethanol solution with the volume fraction of 60%, the flow rate of the entrainer is 1.5ml/min, and the extraction time is 1.5 hours;
(5) transferring the extract in the recovery bottle to a concentration bottle, concentrating on a rotary evaporator with the vacuum degree of 0.09Mpa and the water bath temperature controlled at 50 ℃, pouring the solution in the concentration bottle into a watch glass, and freeze-drying in a vacuum freeze-dryer to obtain the seabuckthorn leaf polyphenol extract.
The technical scheme of the invention is different from the prior art mainly in three points:
1. soaking folium Hippophae powder in ethanol solution overnight;
2. the solution is 60% ethanol water solution, and the pH value is 3-4;
3. the static extraction and the dynamic extraction are carried out in steps in the extraction process, but not synchronously carried out conventionally.
The technical effects of the above three different points are as follows:
1. due to CO2Is nonpolar substance, and folium Hippophae polyphenol is treated with supercritical CO2The solubility in fluid is low, the direct extraction yield is low, and the seabuckthorn leaf powder soaked overnight by ethanol can dissolve a small part of polyphenol in the ethanol and promote other polyphenol components to be in an activated state to be dissolved out, thereby being beneficial to CO2Extracting in supercritical extraction;
2. the inventor simultaneously finds that the pH value of the ethanol water solution is adjusted to be in a slightly acidic range, the dissolution of the organic phase of the polyphenol component phase is facilitated, the effect of ethanol soaking overnight is facilitated, the effect of an entrainer is exerted during supercritical extraction, and CO is enabled to be generated2The efficiency of supercritical extraction is integrally improved;
3. during supercritical extraction, the process of static extraction is firstly adopted, certain temperature and pressure are utilized, the efficiency of extraction in the early stage and the extraction of effective components are improved, the process of dynamic extraction is adopted in the later stage, the further extraction of polyphenol components is realized, the two processes are organically combined, and the extraction efficiency is improved as much as possible.
The inventor points out that the three invention points are three key steps which complement each other, the effective extraction of the sea buckthorn polyphenol components is realized together in a front-back manner, and the inventor also carries out optimization selection on parameter setting in each step.
The seabuckthorn leaf polyphenol extract obtained by the invention is characterized in that: the product yield is about 3.7%, wherein the seabuckthorn fruit is morePhenol accounts for about 5.9% of the extract, total antioxidant capacity (expressed by Vc equivalent) of the polyphenol extract is 8.44mgVc/g extract, DPPH free radical clearance rate IC5010.05. mu.g/mL; meanwhile, the total antioxidant capacity of the seabuckthorn leaf polyphenol extract prepared by adopting the traditional ultrasonic extraction technology is 6.15mg Vc/g extract, and the DPPH free radical clearance rate IC50The total antioxidant capacity of the seabuckthorn leaf polyphenol extract prepared by the supercritical carbon dioxide extraction technology is 1.37 times that of an ultrasonic extraction preparation, and the DPPH scavenging capacity is 2.01 times that of the ultrasonic extraction preparation.
The extraction yield without soaking is 1.66 times of the extraction yield with soaking.
The pH of the ethanol solution is adjusted by adding acid, and the yield is 2.10 times of the unadjusted pH.
One specific scheme may be:
supercritical CO2The method for preparing seabuckthorn leaf polyphenol by using fluid comprises the following steps:
(1) mixing folium Hippophae powder crushed to 20 meshes with an ethanol solution, soaking overnight to obtain a soaking material, filling the soaking material in a 300 ml extraction kettle, wherein the volume ratio of the folium Hippophae powder to the ethanol solution is 1:1, the ethanol solution is an ethanol aqueous solution with the volume fraction of 60%, the volume unit of the ethanol solution is ml, and the mass unit of a folium Hippophae powder sample is g;
(2) fixing the filled extraction kettle in a heating box, connecting interfaces at two ends of the extraction kettle when all air valves in the system are in a closed state, and closing a door of the heating box, wherein all the air valves comprise an air inlet switch, an air outlet valve and a fine adjustment valve;
(3) opening supercritical CO2The fluid extraction equipment power supply is used for setting the temperature of the extraction kettle and the temperature of the fine adjustment valve, when the temperature reaches a set value, the air inlet switch is opened to adjust the pressure of the extraction kettle, and when the pressure of the extraction kettle reaches a set condition, the pressure is kept for 5min under the condition, wherein the temperature of the extraction kettle is 40 ℃, the temperature of the fine adjustment valve is 90 ℃, and the pressure of the extraction kettle is 30 MPa;
(4) opening the gas outlet valve, controlling the gas flow in the recovery bottle by using a fine-tuning valve, enabling the tail-connected flow meter to display the flow to be 2L/min, balancing the pressure of the extraction kettle by using a carbon dioxide pneumatic pump, keeping the pressure of the extraction kettle constant, opening an entrainer pump, controlling the flow velocity of the entrainer, closing a gas inlet switch after the extraction time is up, and enabling CO in the extraction kettle to be discharged2Discharging, recovering the extract in a recovery bottle until CO is discharged2Emptying, and taking down a recovery bottle, wherein the entrainer is an ethanol solution with the volume fraction of 60%, the flow rate of the entrainer is 1.5ml/min, and the extraction time is 1.5 hours;
(5) transferring the extract in the recovery bottle to a concentration bottle, concentrating on a rotary evaporator with the vacuum degree of 0.09Mpa and the water bath temperature controlled at 50 ℃, pouring the solution in the concentration bottle into a watch glass, and freeze-drying in a vacuum freeze-dryer to obtain the seabuckthorn leaf polyphenol extract.
Detailed Description
Example 1 preparation of Hippophae rhamnoides leaf Polyphenol extract
Mixing 100g of 20-mesh sea buckthorn leaf powder with 100ml of 60% ethanol solution (pH is 4), soaking overnight, filling the soaked material into a 300 ml extraction kettle, fixing the filled extraction kettle in a heating box, connecting interfaces at two ends of the extraction kettle, closing an air inlet switch, an air outlet valve and a fine adjustment valve, and closing the heating box door; opening supercritical CO2A power supply of the fluid extraction equipment sets the temperature of the extraction kettle to be 40 ℃ and the temperature of the fine adjustment valve to be 90 ℃, when the temperature reaches a set value, an air inlet switch is opened, the pressure of the extraction kettle is adjusted to be 30MPa, and the extraction kettle is kept for 10min under the pressure condition; opening an air outlet valve, controlling the gas flow in the recovery bottle by using a fine adjustment valve to ensure that the tail-connected flow meter displays the flow of 2L/min, balancing the pressure of the extraction kettle by using a carbon dioxide pneumatic pump, keeping the pressure of the extraction kettle constant, opening an entrainer pump, controlling the flow rate of the ethanol solution with the volume fraction of 60% to be 1.5ml/min, extracting for 1.5 hours, closing an air inlet switch, and allowing CO in the extraction kettle to flow2Discharging, recovering the extract in a recovery bottle until CO is discharged2Emptying and taking down the recovery bottle; transferring the extractive solution in the recovery bottle to a concentration bottle, and concentrating on a rotary evaporatorAnd (3) pouring the solution in the concentration bottle into a watch glass after the vacuum degree of a rotary evaporator is 0.09Mpa and the water bath temperature is controlled at 50 ℃, and freeze-drying in a vacuum freeze-drying machine to obtain 3.7g of the dried seabuckthorn leaf polyphenol extract, wherein the polyphenol accounts for 5.9 percent of the extract.
Example 2
Effect of ethanol soaking
The comparison test is carried out by adopting a soaking mode and a non-soaking mode, the yield and the polyphenol content are compared for three times respectively, and the obtained results are as follows:
| (yield/Polyphenol content) | 1 | 2 | 3 | Average |
| Soaking | 3.69/5.91 | 3.71/5.88 | 3.69/5.90 | 3.70/5.90 |
| Without soaking | 2.22/4.55 | 2.24/4.55 | 2.23/4.51 | 2.23/4.54 |
As can be seen from the above table, there is a significant improvement in the way of extraction after soaking, both in terms of the yield of the final product and in terms of the polyphenol content extracted.
Example 3
Influence of the pH of the ethanol solution
The inventors carried out a comparative experiment using a gradient method, and carried out the test at pH values of ethanolic stock solution (pH approximately about 6.9), 6.5, 6.0, 5.5, 5.0, 4.5, 4.0, 3.5, 3.0, 2.5, 2.0, and 1.5, and obtained the following results:
from the experimental results, it can be seen that, initially, when the pH gradient of the ethanol solution is decreased, both the yield and the polyphenol content are greatly increased, and when the pH is between 3 and 4, the ethanol solution is basically in a stable state, and when the pH is decreased again and gradually enters a strong acid zone, the yield and the polyphenol content are in a rapidly decreased state.
Claims (2)
1. Supercritical CO2A method for preparing a seabuckthorn leaf polyphenol extract from a fluid, comprising the steps of:
(1) mixing folium Hippophae powder crushed to 20 meshes with an ethanol solution, soaking for 10-24h to obtain a soaking material, filling the soaking material in a 300 ml extraction kettle, wherein the volume ratio of the folium Hippophae powder to the ethanol solution is 1:1, the ethanol solution is an ethanol aqueous solution with the volume fraction of 60%, the volume unit of the ethanol solution is ml, and the mass unit of a folium Hippophae powder sample is g; wherein the pH of the 60% ethanol aqueous solution is 3-4;
(2) fixing the filled extraction kettle in a heating box, connecting interfaces at two ends of the extraction kettle when all air valves in the system are in a closed state, and closing a door of the heating box, wherein all the air valves comprise an air inlet switch, an air outlet valve and a fine adjustment valve;
(3) opening supercritical CO2The fluid extraction equipment power supply is used for setting the temperature of the extraction kettle and the temperature of the fine adjustment valve, when the temperature reaches a set value, the air inlet switch is opened to adjust the pressure of the extraction kettle, and when the pressure of the extraction kettle reaches a set condition, the pressure is kept for 5min under the condition, wherein the temperature of the extraction kettle is 40 ℃, the temperature of the fine adjustment valve is 90 ℃, and the pressure of the extraction kettle is 30 MPa;
(4) opening the gas outlet valve, controlling the gas flow in the recovery bottle by using a fine-tuning valve, enabling the tail-connected flow meter to display the flow to be 2L/min, balancing the pressure of the extraction kettle by using a carbon dioxide pneumatic pump, keeping the pressure of the extraction kettle constant, opening an entrainer pump, controlling the flow velocity of the entrainer, closing a gas inlet switch after the extraction time is up, and enabling CO in the extraction kettle to be discharged2Discharging, recovering the extract in a recovery bottle until CO is discharged2Emptying, and taking down a recovery bottle, wherein the entrainer is an ethanol solution with the volume fraction of 60%, the flow rate of the entrainer is 1.5ml/min, and the extraction time is 1.5 hours;
(5) transferring the extract in the recovery bottle to a concentration bottle, concentrating on a rotary evaporator with the vacuum degree of 0.09Mpa and the water bath temperature controlled at 50 ℃, pouring the solution in the concentration bottle into a watch glass, and freeze-drying in a vacuum freeze-dryer to obtain the seabuckthorn leaf polyphenol extract.
2. The polyphenol extract of seabuckthorn leaves produced according to the method of claim 1.
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