CN112704904A - Supercritical CO2Method for extracting plant active ingredients by technology - Google Patents
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Abstract
The invention relates to the technical field of plant extraction, in particular to supercritical CO2A method for extracting plant active ingredients by a technology; the method comprises the steps of firstly carrying out polarity change, shock wave and tearing treatment on plant powder to be extracted through a high-frequency high-voltage electromagnetic field to form nano-scale small-molecule active particles, then soaking the nano-scale small-molecule active particles in a mixed solution containing complex enzyme and calcium ions, and carrying out microwave radiation treatment on the mixed solution; the damage to effective components in plant raw material cells during temperature rise can be effectively controlled by adopting a radiation wall breaking technology, so that the extract is easier to refine, the purity of the extracted plant active component extract is improved, and the extraction difficulty is reduced; the obtained material is subjected to freeze drying treatment, so that the quality and the use value of the extracted plant active ingredient extract are ensured; and finally, the plant active ingredient extract with higher purity and higher yield is prepared by matching the supercritical extraction process and the multi-stage extraction and separation process.
Description
Technical Field
The invention relates to the technical field of plant extractionIn particular to supercritical CO2A method for extracting plant active ingredients by a technique.
Background
The Chinese medicine is mainly composed of plant medicine (root, stem, leaf and fruit), animal medicine (internal organs, skin, bone and organ, etc.) and mineral medicine. Since the plant herbs account for the majority of the Chinese herbs, the Chinese herbs are also called Chinese herbs. Because the effective components in the plants can play a good role in treating diseases and conditioning the body, the plants can be directly used as medicines.
At present, the effective components in the plants are mostly obtained by a plant extraction method, namely, the plant extraction is a product formed by taking the plants as raw materials, directionally obtaining and concentrating one or more effective components in the plants through a physical and chemical extraction and separation process according to the requirement on the extraction site, and not changing the structures of the effective components. According to different components of the extracted plants, glycoside, acid, polyphenol, polysaccharide, terpenoid, flavone, alkaloid and the like are formed; according to different properties, the plant oil can be divided into vegetable oil, extract, powder, crystalline lens and the like.
Chinese patent application No. CN201510544843.2 discloses a plant extraction technology and patent application No. CN201510377480.8 discloses a peony seed essential oil supercritical extraction method, and although the two patent documents can extract effective components in plants to a certain extent, the obtained plant active component extract has low yield and relatively low purity, and simultaneously, the waste of plant raw materials is increased, and the cost input is increased.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, a first object of the present invention is to provide a supercritical CO2The method for extracting the plant active ingredients technically has the advantages that the extracted plant active ingredients have high purity and high yield; the yield of the plant active ingredient extract can be effectively improved, the waste of plant raw materials can be reduced, and the cost is saved.
In order to achieve the purpose, the invention provides the following technical scheme:
supercritical CO2The method for extracting the active ingredients of the plants comprises the following steps:
s1, carrying out magnetic separation on the plant raw materials by using an electronic screening machine, finely screening the plant raw materials to be extracted without deterioration, insect damage and mildew, and then storing the plant raw materials in a dry environment for later use;
s2, slicing the plant raw materials to be extracted screened in the step S1, rinsing the obtained plant slices, drying the plant slices in drying equipment, and then sending the dried plant slices into a grinder to be ground into plant powder to be extracted of 80-150 meshes;
s3, sending the plant powder to be extracted obtained in the step into a condenser equipped with a high-frequency high-voltage electromagnetic field, and carrying out polarity change, shock wave and tearing treatment at the speed of 1.6-2.0 hundred million times/second; then transferring the treated plant powder to be extracted into a soaking tank equipped with a microwave device, and adding a calcium ion solution with the mass of 10-15 of the plant powder to be extracted and a proper amount of complex enzyme into the soaking tank; adjusting the pH value of the mixed liquid in the soaking tank to 3.2-4.5 by using a proper amount of hydrochloric acid solution, then raising the temperature in the soaking tank to 40-50 ℃, and simultaneously starting a microwave device to perform radiation treatment on the plant powder to be extracted in the extraction kettle for 3-5 min; then stirring and carrying out enzymolysis for 5-8 h at the temperature; after the enzymolysis is finished, carrying out freeze drying treatment on the materials in the soaking tank, sieving the obtained solid materials with a 200-300-mesh sieve, and then storing the obtained plant extract powder for later use;
s4, accurately weighing an entrainer with the weight of 0.6-18% of the plant extract powder obtained in the step S3, mixing and stirring the entrainer and the plant extract powder uniformly, granulating, feeding granules obtained through granulation into a supercritical extraction kettle, and conveying CO into the extraction kettle at the flow rate of 2.3-2.8L/h2Performing primary extraction on the fluid under the conditions that the extraction pressure is 18-25 MPa and the extraction temperature is 35-55 ℃, wherein the extraction time is 50-90 min;
s5, introducing the obtained extract into a primary separator, and separating paste and extract at the pressure of 20-40 MPa and the temperature of 30-40 DEG CWaste residues, the paste is introduced into a secondary extraction kettle, secondary extraction is carried out for 1-2 h under the conditions that the pressure is 15-45 MPa and the temperature is 30-40 ℃, then a secondary extract is introduced into a secondary separator, and the paste, an entrainer and CO are separated from the secondary separator under the conditions that the pressure is 5-15 MPa and the temperature is 30-50 DEG C2；
S6, adding superfine silica gel powder directly into the paste obtained in the secondary separator, stirring uniformly, extruding through a 300-400-mesh screen, and performing supercritical gradient extraction crystallization at 30-35 ℃, 38-45 ℃, 50-55 ℃ and under the pressure of 13-16 MPa, 15-20 MPa and 18-23 MPa by using ethyl acetate, ethanol and petroleum ether as entrainers respectively to obtain a solid material, namely a finished product of the plant active ingredient extract.
By adopting the technical scheme: the method comprises the steps of firstly, carrying out polarity change, shock wave and tearing treatment on plant powder to be extracted through a high-frequency high-voltage electromagnetic field, so that chemical bonds of active ingredients in cells of the plant powder to be extracted are vibrated and torn, and particles are promoted to rub and collide with each other, so that nanoscale micromolecule active particles are formed, then, soaking the particles in a mixed solution containing complex enzyme and calcium ions, and carrying out microwave radiation treatment on the mixed solution; the damage to effective components in plant raw material cells during temperature rise can be effectively controlled by adopting a radiation wall breaking technology, so that the extract is easier to refine, the purity of the extracted plant active component extract is improved, and the extraction difficulty is reduced; the obtained material is subjected to freeze drying treatment, so that the quality and the use value of the extracted plant active ingredient extract are ensured. And finally, the plant active ingredient extract with higher purity and higher yield is prepared by matching the supercritical extraction process and the multi-stage extraction and separation process.
The invention is further configured to: and in the step S3, the frequency of the electromagnetic wave is 10000-30000 MHz.
By adopting the technical scheme: the method has the advantages that the high-frequency high-voltage electromagnetic field is adopted to carry out polarity change, shock wave and tearing treatment on the plant powder to be extracted, so that chemical bonds of effective components in cells of the plant powder to be extracted are vibrated and torn, mutual friction and collision among particles are promoted, nano-scale small molecular active particles are formed, the yield of the plant active component extract can be effectively improved, waste of plant raw materials can be reduced, and the cost is saved.
The invention is further configured to: the calcium ion solution used in the step S3 is a calcium nitrate solution, and the concentration of the calcium nitrate solution is 1.2-1.8 mol/L.
By adopting the technical scheme: the plant powder to be extracted is soaked in calcium nitrate solution, and the complex enzyme is used to effectively increase the permeability of plant cell membranes to be extracted, so that the dissolved substances in the plant cells to be extracted can flow out sufficiently, the purity and content of the obtained plant active ingredient extract are increased, and the utilization rate of plant raw materials is also increased.
The invention is further configured to: the complex enzyme used in the step S3 is prepared from cellulase, pectinase and lipase according to the mass ratio of 1: 0.3-1.5: 0.12-1.8, and mixing; and the dosage of the complex enzyme is 0.8-4.5% of the mass of the plant powder to be extracted.
By adopting the technical scheme: the use of the complex enzyme can effectively carry out enzymolysis on the cell walls of the plant raw material cells fully, and the extraction efficiency and the extraction purity of the plant raw material extract can be effectively improved by matching with the use of other subsequent processes.
The invention is further configured to: the concentration of the hydrochloric acid solution used in the step S3 is 1.5-2.0 mol/L.
By adopting the technical scheme: the use of the hydrochloric acid solution can adjust the pH of the mixed solution in the soaking tank to 3.2-4.5, so that the activity of the complex enzyme is exerted to the maximum, the enzymolysis efficiency of plant raw material cell walls is effectively improved, and the subsequent extraction or extraction of plant active ingredient extracts is facilitated.
The invention is further configured to: in the step S3, when the plant powder to be extracted is subjected to radiation treatment, the radiation frequency is set to 2000-2500 MHz, and the radiation power is set to 3500-5500W.
By adopting the technical scheme: the radiation wall breaking technology can effectively control the damage to the effective components in the plant raw material cells during temperature rise, and simultaneously, the excessive dissolution of the ineffective components such as mucoid, colloid and the like due to too small powder of the medicinal materials is avoided, so that the extract is easier to refine, the purity of the extracted plant active component extract is improved, and the extraction difficulty is reduced.
The invention is further configured to: the temperature of the freeze drying in the step S3 is-50 to-40 ℃, and the freeze drying time is 15 to 20 hours.
By adopting the technical scheme: the loss of volatile substances in the effective components of the plant raw materials can be effectively reduced by using the freeze drying process, the probability of oxidation of some effective substances which are easily oxidized in the effective components can be effectively reduced, and the quality and the use value of the extracted plant active component extract are ensured. In addition, the water content in the prepared plant extract powder can be kept between 1 and 5 percent by using the freeze drying process, so that the plant extract powder after freeze drying can be stored for a long time without deterioration.
The invention is further configured to: the entrainer used in the step S4 is selected from one of ethyl acetate, emu oil and absolute ethyl alcohol.
By adopting the technical scheme: the solubility of solute near the critical point of the solvent is most sensitive to the change of temperature and pressure, and after the entrainer is added, the critical point of the mixed solvent can be correspondingly changed and is closer to the extraction temperature; the sensitivity of solute solubility to temperature and pressure is enhanced, so that the separated components are separated from the circulating gas through temperature and pressure, the high energy consumption of gas recompression is avoided, and the extraction efficiency and purity of the plant raw material extract are improved.
Advantageous effects
Compared with the known public technology, the technical scheme provided by the invention has the following beneficial effects:
the method comprises the steps of firstly, carrying out polarity change, shock wave and tearing treatment on plant powder to be extracted through a high-frequency high-voltage electromagnetic field, so that chemical bonds of active ingredients in cells of the plant powder to be extracted are vibrated and torn, and particles are promoted to rub and collide with each other, so that nanoscale micromolecule active particles are formed, then, soaking the particles in a mixed solution containing complex enzyme and calcium ions, and carrying out microwave radiation treatment on the mixed solution; the damage to effective components in plant raw material cells during temperature rise can be effectively controlled by adopting a radiation wall breaking technology, and meanwhile, the excessive dissolution of ineffective components such as mucilage, colloid and the like due to too small medicinal powder is avoided, so that the extract is easier to refine, the purity of the extracted plant active component extract is improved, and the extraction difficulty is reduced; the obtained material is subjected to freeze drying treatment, so that the loss of volatile substances in the effective components of the plant raw materials can be effectively reduced, the probability of oxidation of some effective substances which are easily oxidized in the effective components can be effectively reduced, and the quality and the use value of the extracted plant active component extract are ensured. And finally, the plant active ingredient extract with higher purity and higher yield is prepared by matching the supercritical extraction process and the multi-stage extraction and separation process.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. It is to be understood that the embodiments described are only a few embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be further described with reference to the following examples.
Example 1
The method for extracting the active ingredient (paeonol) in the tree peony bark by using the tree peony bark as the raw material comprises the following steps:
s1, carrying out magnetic separation on the tree peony bark by using an electronic screening machine, finely selecting the tree peony bark to be extracted without deterioration, insect damage and mildew, and then storing the tree peony bark in a dry environment for later use;
s2, slicing the moutan bark to be extracted which is screened in the step S1, rinsing the obtained moutan bark slices, drying the moutan bark slices in drying equipment, and then sending the dried moutan bark slices into a grinder to be ground into moutan bark powder to be extracted of 80 meshes;
s3, sending the cortex moutan powder to be extracted obtained in the above steps to a condenser equipped with a high-frequency and high-voltage electromagnetic field, and performing polarity change, shock wave and tearing treatment at a rate of 1.6 hundred million times/second; transferring the treated tree peony bark powder to be extracted into a soaking tank equipped with a microwave device, and adding a calcium ion solution with the mass 10 times that of the tree peony bark powder to be extracted and a proper amount of complex enzyme into the soaking tank; adjusting the pH of the mixed solution in the soaking tank to 3.2 with appropriate amount of hydrochloric acid solution, heating the temperature in the soaking tank to 40 deg.C, and simultaneously starting microwave device to perform radiation treatment on the cortex moutan powder to be extracted in the extraction kettle for 3 min; then stirring and carrying out enzymolysis for 5 hours at the temperature; after the enzymolysis is finished, carrying out freeze drying treatment on the materials in the soaking tank, sieving the obtained solid materials with a 200-mesh sieve, and then storing the obtained cortex moutan extract powder for later use;
s4, accurately weighing entrainer with weight of 0.6% of the cortex moutan extract powder obtained in the step S3, mixing and stirring the entrainer and the cortex moutan extract powder uniformly, granulating, feeding granules obtained by granulation into a supercritical extraction kettle, and conveying CO into the extraction kettle at a flow rate of 2.3L/h2Performing primary extraction on the fluid under the conditions that the extraction pressure is 18MPa and the extraction temperature is 35 ℃, wherein the extraction time is 50 min;
s5, introducing the obtained extract into a primary separator, separating paste and waste residue under the conditions of 20MPa of pressure and 30 ℃, introducing the paste into a secondary extraction kettle, performing secondary extraction under the conditions of 15MPa of pressure and 30 ℃ of extraction time of 1h, introducing the secondary extract into a secondary separator, and separating the paste, entrainer and CO from the secondary separator under the conditions of 5MPa of pressure and 30 ℃ of extraction time of 1h2；
S6, directly adding superfine silica gel powder into the paste obtained in the secondary separator, uniformly stirring, extruding through a 300-mesh screen, and performing supercritical gradient extraction crystallization at 30 ℃, 38 ℃, 50 ℃ and 13MPa, 15MPa and 18MPa by respectively using ethyl acetate, ethanol and petroleum ether as entrainers to finally obtain a solid material, namely a finished paeonol product.
The frequency of the electromagnetic wave used in step S3 is 10000 MHz.
The calcium ion solution used in step S3 is a calcium nitrate solution, and the concentration of the calcium nitrate solution is 1.2 mol/L.
The complex enzyme used in the step S3 is prepared from cellulase, pectinase and lipase according to the mass ratio of 1: 0.3: 0.12 is prepared by mixing; and the dosage of the compound enzyme is 0.8 percent of the mass of the tree peony bark powder to be extracted.
The concentration of the hydrochloric acid solution used in step S3 was 1.5 mol/L.
When the cortex moutan powder to be extracted is subjected to radiation treatment again in the step S3, the radiation frequency is set to 2000MHz, and the radiation power is set to 3500W.
The temperature of the freeze drying in the step S3 is-50 ℃, and the freeze drying time is 15 h.
The entrainer used in step S4 is ethyl acetate.
Example 2
The method for extracting the active ingredient of moutan bark (paeonol) provided in this example is substantially the same as that of example 1, and the main differences are as follows: in step S3, performing polarity change, vibration wave and tearing treatment on the tree peony bark powder to be extracted at the speed of 1.8 hundred million times/second;
the frequency of the electromagnetic wave used in step S3 is 20000 MHz.
The concentration of the calcium nitrate solution in step S3 was 1.5 mol/L.
The complex enzyme used in the step S3 is prepared from cellulase, pectinase and lipase according to the mass ratio of 1: 1.0: 0.8, mixing and preparing; the using amount of the compound enzyme is 0.25 percent of the mass of the tree peony bark powder to be extracted; and the pH of the mixed liquid in the soaking tank is 3.8.
In step S3, the radiation frequency was set to 2300MHz, and the radiation power was set to 4500W.
Example 3
The method for extracting the active ingredient of moutan bark (paeonol) provided in this example is substantially the same as that of example 1, and the main differences are as follows: in step S3, polarity change, vibration wave and tearing are carried out on the tree peony bark powder to be extracted at the speed of 2.0 hundred million times/second;
the frequency of the electromagnetic wave used in step S3 is 30000 MHz.
The concentration of the calcium nitrate solution in step S3 was 1.8 mol/L.
The complex enzyme used in the step S3 is prepared from cellulase, pectinase and lipase according to the mass ratio of 1: 1.5: 1.8 mixing and preparing; the using amount of the compound enzyme is 4.5 percent of the mass of the tree peony bark powder to be extracted; and the pH of the mixed solution in the soaking tank is 4.5.
In step S3, the radiation frequency is set to 2500MHz, and the radiation power is set to 5500W.
Comparative example 1
The method for extracting the active ingredient of moutan bark (paeonol) provided in this example is substantially the same as that of example 1, and the main differences are as follows: in the step S3, polarity change, shock wave and tearing treatment are not carried out on the tree peony bark powder to be extracted;
comparative example 2
The method for extracting the active ingredient of moutan bark (paeonol) provided in this example is substantially the same as that of example 1, and the main differences are as follows: in step S3, a calcium nitrate solution is not used;
comparative example 3
The method for extracting the active ingredient of moutan bark (paeonol) provided in this example is substantially the same as that of example 1, and the main differences are as follows: in step S3, no complex enzyme is used;
comparative example 4
The method for extracting the active ingredient of moutan bark (paeonol) provided in this example is substantially the same as that of example 1, and the main differences are as follows: in the step S3, the tree peony bark powder to be extracted is not subjected to radiation treatment;
performance testing
The equivalent amount of the moutan bark active ingredient extract (paeonol) obtained in examples 1 to 3 and comparative examples 1 to 4 was measured by HPLC method for the yield (yield: weight of paeonol/weight of moutan bark x 100%) and purity of the extracted paeonol, and the obtained data are reported in the following table:
| yield of paeonol/% | Purity/% of paeonol | |
| Example 1 | 25.63 | 98.67 |
| Example 2 | 25.39 | 99.58 |
| Example 3 | 26.36 | 99.72 |
| Comparative example 1 | 18.25 | 98.37 |
| Comparative example 2 | 21.28 | 98.53 |
| Comparative example 3 | 16.57 | 98.12 |
| Comparative example 4 | 18.63 | 99.36 |
By analyzing the relevant data in the tables, the extracted plant active ingredients extracted by the method have high purity and high yield; the yield of the plant active ingredient extract can be effectively improved, the waste of plant raw materials can be reduced, and the cost is saved. Thus, the supercritical CO provided by the invention is shown2The method for extracting the plant active ingredients by the technology has wider market prospect and is more suitable for popularization.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.
Claims (8)
1. Supercritical CO2The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps:
s1, carrying out magnetic separation on the plant raw materials by using an electronic screening machine, finely screening the plant raw materials to be extracted without deterioration, insect damage and mildew, and then storing the plant raw materials in a dry environment for later use;
s2, slicing the plant raw materials to be extracted screened in the step S1, rinsing the obtained plant slices, drying the plant slices in drying equipment, and then sending the dried plant slices into a grinder to be ground into plant powder to be extracted of 80-150 meshes;
s3, sending the plant powder to be extracted obtained in the step into a condenser equipped with a high-frequency high-voltage electromagnetic field, and carrying out polarity change, shock wave and tearing treatment at the speed of 1.6-2.0 hundred million times/second; then transferring the treated plant powder to be extracted into a soaking tank equipped with a microwave device, and adding a calcium ion solution with the mass of 10-15 of the plant powder to be extracted and a proper amount of complex enzyme into the soaking tank; adjusting the pH value of the mixed liquid in the soaking tank to 3.2-4.5 by using a proper amount of hydrochloric acid solution, then raising the temperature in the soaking tank to 40-50 ℃, and simultaneously starting a microwave device to perform radiation treatment on the plant powder to be extracted in the extraction kettle for 3-5 min; then stirring and carrying out enzymolysis for 5-8 h at the temperature; after the enzymolysis is finished, carrying out freeze drying treatment on the materials in the soaking tank, sieving the obtained solid materials with a 200-300-mesh sieve, and then storing the obtained plant extract powder for later use;
s4, accurately weighing an entrainer with the weight of 0.6-18% of the plant extract powder obtained in the step S3, mixing and stirring the entrainer and the plant extract powder uniformly, granulating, feeding granules obtained through granulation into a supercritical extraction kettle, and conveying CO into the extraction kettle at the flow rate of 2.3-2.8L/h2Performing primary extraction on the fluid under the conditions that the extraction pressure is 18-25 MPa and the extraction temperature is 35-55 ℃, wherein the extraction time is 50-90 min;
s5, introducing the obtained extract into a primary separator, separating paste and waste residue under the conditions of pressure of 20-40 MPa and temperature of 30-40 ℃, introducing the paste into a secondary extraction kettle, performing secondary extraction under the conditions of pressure of 15-45 MPa and temperature of 30-40 ℃ for 1-2 h, introducing the secondary extract into a secondary separator, and separating the paste, entrainer and CO from the secondary separator under the conditions of pressure of 5-15 MPa and temperature of 30-50 DEG C2；
S6, adding superfine silica gel powder directly into the paste obtained in the secondary separator, stirring uniformly, extruding through a 300-400-mesh screen, and performing supercritical gradient extraction crystallization at 30-35 ℃, 38-45 ℃, 50-55 ℃ and under the pressure of 13-16 MPa, 15-20 MPa and 18-23 MPa by using ethyl acetate, ethanol and petroleum ether as entrainers respectively to obtain a solid material, namely a finished product of the plant active ingredient extract.
2. A supercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: and in the step S3, the frequency of the electromagnetic wave is 10000-30000 MHz.
3. A supercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: the calcium ion solution used in the step S3 is a calcium nitrate solution, and the concentration of the calcium nitrate solution is 1.2-1.8 mol/L.
4. A supercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: the complex enzyme used in the step S3 is prepared from cellulase, pectinase and lipase according to the mass ratio of 1: 0.3-1.5: 0.12-1.8, and mixing; and the dosage of the complex enzyme is 0.8-4.5% of the mass of the plant powder to be extracted.
5. A supercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: the concentration of the hydrochloric acid solution used in the step S3 is 1.5-2.0 mol/L.
6. A supercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: when the plant powder to be extracted is subjected to radiation treatment in the step S3, the radiation frequency is set to 2000-2500 MHz, and the radiation power is set to 3500-5500W.
7. A supercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: the temperature of the freeze drying in the step S3 is-50 to-40 ℃, and the freeze drying time is 15 to 20 hours.
8. According to the rightSupercritical CO according to claim 12The method for extracting the active ingredients of the plants technically is characterized by comprising the following steps: the entrainer used in the step S4 is selected from one of ethyl acetate, emu oil and absolute ethyl alcohol.
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