CN111228852A - Preparation method of aster keemun extract - Google Patents
Preparation method of aster keemun extract Download PDFInfo
- Publication number
- CN111228852A CN111228852A CN202010057873.1A CN202010057873A CN111228852A CN 111228852 A CN111228852 A CN 111228852A CN 202010057873 A CN202010057873 A CN 202010057873A CN 111228852 A CN111228852 A CN 111228852A
- Authority
- CN
- China
- Prior art keywords
- aster
- mixed solvent
- keemun
- extraction
- qishiwan
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/028—Flow sheets
- B01D11/0284—Multistage extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention belongs to the technical field of plant extraction, and provides a preparation method of a Keemun aster extract, which comprises the following steps: s1, cleaning the root of a Qiquan, adding the cleaned root of the Qiquan into a first mixed solvent, and homogenizing at 20-30 ℃ to obtain a Qiquan homogenate liquid; s2, freeze-drying the homogenate to obtain Qiquan powder; s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material; s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38-42 ℃, the extraction pressure is 25-30 MPa, the flow rate is 22-25 kg/h, and the extraction time is 1-1.5 h; s5, analyzing the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 5-13 kg/h, the analyzing pressure is 6-8 MPa, the temperature is 40-45 ℃, the analyzing time is 1.5-2.5 h, and discharging is carried out to obtain the Qizi extract. Through the technical scheme, the problems that the extraction period of the extraction method of the Qishiwan aster extract is long and the yield of the active ingredient shionone is low in the prior art are solved.
Description
Technical Field
The invention belongs to the technical field of plant extraction, and relates to a preparation method of a keemun aster extract.
Background
Qiziyuan is a special product in Anguo city of Baoding city in Hebei province and is a geographical sign of agricultural products in China. Qishiwan is a genuine variety in Anguo, and is used as a medicine by root, and has the color similar to coral, silky hair (also called braid), soft texture similar to cotton, and sweet smell and fragrance. Qiziyuan is long in length, thick and red in color, and evaluated as the same kind of crown throughout the country. The Qishiwan aster has the efficacies of moistening lung and descending qi, relieving cough and eliminating phlegm, is mainly used for treating symptoms such as cough due to adverse rising of qi, phlegm vomiting difficulty, lung deficiency and chronic cough, phlegm with blood and the like, and has large dosage in the traditional Chinese medicine clinical prescription and the Chinese patent medicine. The asterone is one of main effective components of the keemun aster for relieving cough and eliminating phlegm, and the conventional extraction method mainly adopts alcohol extraction or petroleum ether extraction, but the extraction period is long, and the yield of the effective component, namely the asterone, is low.
Disclosure of Invention
The invention provides a preparation method of a Keemun aster extract, and solves the problems that the extraction period of an extraction method of the Keemun aster extract is long and the yield of active ingredient shionone is low in the prior art.
The technical scheme of the invention is realized as follows:
a preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qiquan, adding the cleaned root of the Qiquan into a first mixed solvent, and homogenizing at 20-30 ℃ to obtain a Qiquan homogenate liquid;
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution;
s2, freeze-drying the homogenate to obtain Qiquan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
the second mixed solvent comprises the following components in parts by weight:
0.2-0.5 part of ethyl acetate, 2.7-5.2 parts of polydimethylsiloxane and 5.6-8.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38-42 ℃, the extraction pressure is 25-30 MPa, the flow rate is 22-25 kg/h, and the extraction time is 1-1.5 h;
s5, analyzing the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 5-13 kg/h, the analyzing pressure is 6-8 MPa, the temperature is 40-45 ℃, the analyzing time is 1.5-2.5 h, and discharging is carried out to obtain the Qizi extract.
As a further technical feature, the mass ratio of tert-butanol to water in the tert-butanol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0%.
As a further technical feature, the second mixed solvent is composed of the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol.
The technical characteristics are that the mass ratio of the first mixed solvent to the radix asterias keemuni is 2.2-5: 1.
as a further technical feature, the mass ratio of the first mixed solvent to the aster keemun root is 3.7: 1.
as a further technical feature, the mass ratio of the second mixed solvent to the keemun aster powder is 1.2-3.5: 10.
as a further technical feature, the mass ratio of the second mixed solvent to the keemun aster powder is 2.3: 10.
as a further technical characteristic, the freeze-drying temperature in the step S2 is-10 ℃ to-20 ℃.
As a further technical characteristic, in the step S4, the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h.
As a further technical feature, in the analysis process of step S5, the flow rate of the carbon dioxide fluid is 9kg/h, the analysis pressure is 7MPa, the temperature is 43 ℃, and the analysis time is 2 h.
The working principle and the beneficial effects of the invention are as follows:
1. in the invention, the extraction method of the aster keemun extract by supercritical carbon dioxide is adopted, compared with the existing extraction method of alcohol or petroleum ether, the extraction time is short, and the extraction period is greatly shortened. The preparation method provided by the invention not only improves the extraction rate of the aster keemun extract to 3.52%, but also obviously improves the content of shionone in the aster keemun extract, so that the yield of the shionone in the obtained aster keemun extract is higher and can reach 83.82%, and the problems of long extraction period and low yield of the shionone as an effective component in the extraction method of the aster keemun extract in the prior art are effectively solved.
2. In the invention, the root of the Qiquan is cleaned, then the first mixed solvent is added for homogenate, and then the mixture is freeze-dried, so that the extraction rate of the Qiquan extract is obviously improved compared with the method that the root of the Qiquan is cleaned, directly freeze-dried and then crushed. The tertiary butanol aqueous solution in the first mixed solvent is compatible with the sucrose, so that the extraction rate of the aster keemun extract is further improved.
3. According to the invention, the Qiquan powder is mixed with the second mixed solvent and then subjected to supercritical carbon dioxide extraction, and the second mixed solvent, namely ethyl acetate, polydimethylsiloxane and ethanol, are compatible with each other, so that the extraction rate of the Qiquan extract is improved, the content of asterone in the Qiquan extract is obviously improved, and the yield of asterone in the obtained Qiquan extract is higher.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 20 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 2
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qiquan, adding the cleaned root of the Qiquan into a first mixed solvent, and homogenizing at 30 ℃ to obtain a Qiquan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 3
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 4
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 2.2: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 5
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the Qishiwan aster is 5: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 6
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-10 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 7
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-20 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 8
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 1.2: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 9
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 3.5: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 10
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.2 part of ethyl acetate, 2.7 parts of polydimethylsiloxane and 5.6 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 11
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.5 part of ethyl acetate, 5.2 parts of polydimethylsiloxane and 8.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 12
A preparation method of an Aster keemun extract comprises the following steps:
cleaning radix Asteris Keemum, adding into the first mixed solvent, and homogenizing at 25 deg.C to obtain homogenized slurry of radix Asteris Keemum;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38 ℃, the extraction pressure is 25MPa, the flow rate is 22kg/h, and the extraction time is 1.5 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 13
A preparation method of an Aster keemun extract comprises the following steps:
cleaning radix Asteris Keemum, adding into the first mixed solvent, and homogenizing at 25 deg.C to obtain homogenized slurry of radix Asteris Keemum;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 42 ℃, the extraction pressure is 30MPa, the flow rate is 25kg/h, and the extraction time is 1 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Example 14
A preparation method of an Aster keemun extract comprises the following steps:
cleaning radix Asteris Keemum, adding into the first mixed solvent, and homogenizing at 25 deg.C to obtain homogenized slurry of radix Asteris Keemum;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h; (ii) a
S5, analyzing the extracted carbon dioxide fluid at the flow rate of 13kg/h, the analyzing pressure of 8MPa, the temperature of 45 ℃ and the analyzing time of 1.5h, and discharging to obtain the Keemus tataricus extract.
Example 15
A preparation method of an Aster keemun extract comprises the following steps:
cleaning radix Asteris Keemum, adding into the first mixed solvent, and homogenizing at 25 deg.C to obtain homogenized slurry of radix Asteris Keemum;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, resolving the extracted carbon dioxide fluid at a flow rate of 5kg/h, a resolving pressure of 6MPa, a temperature of 40 ℃ and a resolving time of 2.5h, and discharging to obtain the Keemus keiskei extract.
Comparative example 1
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of Qiquan, freeze-drying at-15 ℃, and crushing to obtain Qiquan powder;
s2, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s3, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s4, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Comparative example 2
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of an aster keemun, adding the cleaned root of the aster keemun into a tert-butanol aqueous solution, and homogenizing at 25 ℃ to obtain a homogeneous slurry of the aster keemun;
wherein the mass ratio of the tert-butanol aqueous solution to the root of the aster keemun is 3.7: 1, the mass ratio of the tertiary butanol to the water in the tertiary butanol aqueous solution is 1: 1;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Comparative example 3
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qiquan, adding the cleaned root of the Qiquan into a sucrose aqueous solution, and homogenizing at 25 ℃ to obtain a Qiquan homogenate liquid;
wherein the mass ratio of the sucrose aqueous solution to the root of the Qishiwan aster is 3.7: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Comparative example 4
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qiquan powder into ethanol, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the ethanol to the Qishiwan powder is 2.3: 10,
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Comparative example 5
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Comparative example 6
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate and 7.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
Comparative example 7
A preparation method of an Aster keemun extract comprises the following steps:
s1, cleaning the root of a Qishiwan aster, adding the cleaned root of the Qishiwan aster into a first mixed solvent, and homogenizing at 25 ℃ to obtain a Qishiwan homogenate liquid;
wherein the mass ratio of the first mixed solvent to the root of the aster keemun is 3.7: 1,
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution, wherein the mass ratio of tert-butyl alcohol to water in the tert-butyl alcohol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0 percent;
s2, freeze-drying the homogenate at-15 ℃ to obtain Qishiwan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
wherein the mass ratio of the second mixed solvent to the Qishiwan powder is 2.3: 10,
the second mixed solvent comprises the following components in parts by weight:
0.3 part of ethyl acetate and 4.1 parts of polydimethylsiloxane;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h;
s5, analyzing the extracted carbon dioxide fluid at the flow rate of 9kg/h, the analyzing pressure of 7MPa, the temperature of 43 ℃ and the analyzing time of 2h, and discharging to obtain the Keemus keiskei extract.
The aster keemun root and the aster keemun extract obtained in the extraction methods of examples 1 to 15 and comparative examples 1 to 7 were weighed, and the extraction rate was calculated according to the following formula:
the extraction rate (mass of aster qishiensis extract/mass of aster qishiensis root) x 100;
the asterone content analysis was performed on the aster keemun extracts obtained by the extraction methods of examples 1 to 15 and comparative examples 1 to 7, and the analysis method was as follows:
(1) preparing a reference solution by precisely weighing a proper amount of asterone reference, and dissolving with absolute ethanol to obtain a solution with the concentration of 0.200mg/mL as the reference solution;
(2) preparing a sample solution: dissolving the Aster keemun extract obtained by the extraction methods of examples 1-15 and comparative examples 1-7 with anhydrous ethanol to obtain a solution containing 0.36mg of Aster keemun extract per 1mL as a sample solution;
(3) preparation of a standard curve: precisely sucking 0.0, 1.0, 2.0, 3.0, 4.0, 5.0 and 6.0mL of the reference substance solution, respectively placing in a 25mL volumetric flask, and diluting to the scale with absolute ethyl alcohol. By ultraviolet spectrophotometry atThe absorbance of the sample is measured at the position of the maximum absorption wavelength of 390nm, and the regression equation and the related coefficient are calculated as follows: y ═ 0.0051X-5 × 10-5，r＝0.9991(n＝7)
(4) Determination of sample solution: the absorbance of each of the sample solutions of examples and comparative examples was measured under the above conditions.
The results are shown in the following table:
TABLE 1 extraction rates and Asterone contents in the obtained Aster keemun extracts of examples 1-15 and comparative examples 1-7
| Group of | Extraction ratio (%) | Aster ketone content (%) |
| Example 1 | 3.44 | 83.79 |
| Example 2 | 3.47 | 83.73 |
| Example 3 | 3.52 | 83.82 |
| Example 4 | 3.34 | 83.55 |
| Example 5 | 3.41 | 83.48 |
| Example 6 | 3.49 | 83.67 |
| Example 7 | 3.46 | 83.72 |
| Example 8 | 3.33 | 83.26 |
| Example 9 | 3.37 | 82.53 |
| Example 10 | 3.42 | 82.92 |
| Example 11 | 3.36 | 83.18 |
| Example 12 | 3.38 | 82.13 |
| Example 13 | 3.41 | 81.85 |
| Example 14 | 3.32 | 82.72 |
| Example 15 | 3.35 | 82.29 |
| Comparative example 1 | 2.66 | 60.31 |
| Comparative example 2 | 2.72 | 67.76 |
| Comparative example 3 | 2.75 | 69.47 |
| Comparative example 4 | 2.78 | 42.43 |
| Comparative example 5 | 3.05 | 55.58 |
| Comparative example 6 | 2.91 | 51.92 |
| Comparative example 7 | 2.82 | 48.79 |
As can be seen from the data in the above table, the extraction rate of the preparation methods of examples 1 to 15 is greatly improved compared with the preparation methods of comparative examples 1 to 7, and simultaneously, the content of asterone in the keemun aster extract is also significantly improved, which indicates that the preparation method of the present invention not only improves the extraction rate, but also significantly improves the content of asterone in the keemun aster extract. In the preparation method of example 3, the extraction rate of the aster keemun extract is the highest and can reach 3.52%, the extraction rate is improved by 15.41-32.33% compared with that of the extract obtained in the comparative examples 1-7, the content of asterone in the obtained aster keemun extract is also the highest and can reach 83.82%, and the content of asterone in the comparative examples 1-7 is improved by 38.98-97.55%.
The reason why the extraction rate and the asterone content in the aster keemun extract were low in the preparation methods of comparative examples 1 to 7 as compared with the preparation methods of examples 1 to 15 is that the preparation methods of comparative examples 1 to 7 are different from the preparation method of example 3 in that: comparative example 1 preparation method the aster keemun root was directly freeze-dried without adding the first mixed solvent for homogenization after washing in step S1; comparative example 2 preparation method in step S1 aster keemun roots were washed and then added to an aqueous t-butanol solution without adding an aqueous sucrose solution; comparative example 3 preparation method in step S1 aster keemun roots were washed and then added to the sucrose aqueous solution without adding the tert-butanol aqueous solution; preparation method of comparative example 4 aster keemun powder was added to ethanol without adding polydimethylsiloxane and ethyl acetate in step S3; in the production method of comparative example 5, ethyl acetate was not added to the second mixed solvent in step S3; in the preparation method of comparative example 6, polydimethylsiloxane was not added to the second mixed solvent in step S3; in the production method of comparative example 7, no ethanol was added to the second mixed solvent in step S3. In the preparation method, the keemun aster root is cleaned, the first mixed solvent is added for homogenate, the mixture is frozen and dried, the obtained keemun aster powder is mixed with the second mixed solvent, and then the supercritical carbon dioxide extraction is carried out, so that the extraction rate of the keemun aster extract is improved, the content of the asterone in the keemun aster extract is obviously improved, and the yield of the asterone in the keemun aster extract is higher.
The present invention is not limited to the above preferred embodiments, and any modifications, equivalent substitutions, improvements, etc. within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of an Aster keemun extract is characterized by comprising the following steps:
s1, cleaning the root of a Qiquan, adding the cleaned root of the Qiquan into a first mixed solvent, and homogenizing at 20-30 ℃ to obtain a Qiquan homogenate liquid;
the first mixed solvent consists of a tert-butyl alcohol aqueous solution and a sucrose aqueous solution;
s2, freeze-drying the homogenate to obtain Qiquan powder;
s3, adding the Qishiwan aster powder into a second mixed solvent, and uniformly mixing to obtain a mixed material;
the second mixed solvent comprises the following components in parts by weight:
0.2-0.5 part of ethyl acetate, 2.7-5.2 parts of polydimethylsiloxane and 5.6-8.3 parts of ethanol;
s4, continuously and circularly extracting the mixed material by using supercritical carbon dioxide fluid, wherein the extraction temperature is 38-42 ℃, the extraction pressure is 25-30 MPa, the flow rate is 22-25 kg/h, and the extraction time is 1-1.5 h;
s5, analyzing the extracted carbon dioxide fluid, wherein the flow rate of the carbon dioxide fluid is 5-13 kg/h, the analyzing pressure is 6-8 MPa, the temperature is 40-45 ℃, the analyzing time is 1.5-2.5 h, and discharging is carried out to obtain the Qizi extract.
2. The preparation method of an aster keemun extract according to claim 1, wherein the mass ratio of tert-butanol to water in the tert-butanol aqueous solution is 1: 1, the mass fraction of the sucrose aqueous solution is 5.0%.
3. The preparation method of an aster keemun extract according to claim 1, wherein the second mixed solvent consists of the following components in parts by weight:
0.3 part of ethyl acetate, 4.1 parts of polydimethylsiloxane and 7.3 parts of ethanol.
4. The preparation method of an aster keemun extract according to claim 1, wherein the mass ratio of the first mixed solvent to the aster keemun root is 2.2-5: 1.
5. the preparation method of an aster keemun extract according to claim 1, wherein the mass ratio of the first mixed solvent to the aster keemun root is 3.7: 1.
6. the preparation method of an aster keemun extract according to claim 1, wherein the mass ratio of the second mixed solvent to the aster keemun powder is 1.2-3.5: 10.
7. the preparation method of an aster keemun extract according to claim 6, wherein the mass ratio of the second mixed solvent to the aster keemun powder is 2.3: 10.
8. the preparation method of an Aster keemun extract according to claim 1, wherein the lyophilization temperature in step S2 is-10 ℃ to-20 ℃.
9. The preparation method of an Aster keemun extract according to claim 1, wherein the extraction temperature in step S4 is 40 ℃, the extraction pressure is 27MPa, the flow rate is 24kg/h, and the extraction time is 1.3 h.
10. The method for preparing an Aster keemun extract according to claim 1, wherein the flow rate of the carbon dioxide fluid during the desorption at step S5 is 9kg/h, the desorption pressure is 7MPa, the temperature is 43 ℃, and the desorption time is 2 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010057873.1A CN111228852A (en) | 2020-01-16 | 2020-01-16 | Preparation method of aster keemun extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010057873.1A CN111228852A (en) | 2020-01-16 | 2020-01-16 | Preparation method of aster keemun extract |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111228852A true CN111228852A (en) | 2020-06-05 |
Family
ID=70877952
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010057873.1A Pending CN111228852A (en) | 2020-01-16 | 2020-01-16 | Preparation method of aster keemun extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111228852A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030050334A1 (en) * | 2001-04-30 | 2003-03-13 | Murty Ram B. | Process for extraction of Delta-9-Tetrahydrocannabinol and other related cannabinoids and preparation of specific strength marijuana cigarettes |
| JP2004154702A (en) * | 2002-11-07 | 2004-06-03 | Teijin Ltd | Method for separating nitrogen-containing water soluble organic compound |
| CN1602837A (en) * | 2003-09-30 | 2005-04-06 | 花王株式会社 | Deodorant composition |
| CN102558131A (en) * | 2010-12-24 | 2012-07-11 | 苏州宝泽堂医药科技有限公司 | Method for extracting swertiamarin with supercritical fluid |
| CN105396105A (en) * | 2015-12-10 | 2016-03-16 | 杨献美 | A method of preparing a traditional Chinese medicine composition for preventing and treating recurrent common cold in children |
-
2020
- 2020-01-16 CN CN202010057873.1A patent/CN111228852A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030050334A1 (en) * | 2001-04-30 | 2003-03-13 | Murty Ram B. | Process for extraction of Delta-9-Tetrahydrocannabinol and other related cannabinoids and preparation of specific strength marijuana cigarettes |
| JP2004154702A (en) * | 2002-11-07 | 2004-06-03 | Teijin Ltd | Method for separating nitrogen-containing water soluble organic compound |
| CN1602837A (en) * | 2003-09-30 | 2005-04-06 | 花王株式会社 | Deodorant composition |
| CN102558131A (en) * | 2010-12-24 | 2012-07-11 | 苏州宝泽堂医药科技有限公司 | Method for extracting swertiamarin with supercritical fluid |
| CN105396105A (en) * | 2015-12-10 | 2016-03-16 | 杨献美 | A method of preparing a traditional Chinese medicine composition for preventing and treating recurrent common cold in children |
Non-Patent Citations (3)
| Title |
|---|
| 傅超美: "《药用辅料学》", 31 October 2008, 中国中医药出版社 * |
| 方亮: "《药剂学 第3版》", 31 March 2016, 中国医药科技出版社 * |
| 莫尚志: "超临界CO2萃取紫菀中紫菀酮的工艺研究", 《中药材》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103141832B (en) | Black fungus diet therapy health-preserving diet and preparation method thereof | |
| KR101603171B1 (en) | Method for producing red ginseng-concentrated granule with enhanced ginsenoside content | |
| CN106721742A (en) | A kind of many effect black garlic elite drinks and preparation method thereof | |
| CN104887563A (en) | Snow chrysanthemum tea anti-allergy mask cream and preparing method thereof | |
| WO2020093510A1 (en) | Separation and purification method for polysaccharide in ganoderma lucidum spores | |
| KR20140112777A (en) | Method for producing red ginseng water extract with enhanced specific ginsenoside content | |
| KR101295846B1 (en) | Red ginseng liquor with enhanced saponin content and gensenoside content and producing method thereof | |
| KR20110062000A (en) | Fermenting method of ginseng soaking syrup and liquor obtained thereby | |
| CN106617047A (en) | Mulberry ferment and production technology thereof | |
| CN103446339A (en) | Preparation method of lycium ruthenicum extract | |
| CN101683362A (en) | Method for extracting ganoderma oil by supercritical carbon dioxide | |
| CN109082357A (en) | The brewage process of health care soft-taste white spirit | |
| CN111084262A (en) | Health-care herbal tea containing water-soluble cannabidiol and preparation method thereof | |
| CN111228852A (en) | Preparation method of aster keemun extract | |
| CN100998613A (en) | Method for producing effective components of Ganoderma by supercritical technology | |
| KR20030000453A (en) | Method for preparing an improved red ginseng under oxygen atmosphere | |
| CN108210556A (en) | The extracting method of active constituent in a kind of diaphragma juglandis | |
| CN101649271B (en) | Method for brewing longan Chinese-wolfberry spirit | |
| CN106047494A (en) | An extracting method for pungent litse fruit essence oil | |
| CN103266044A (en) | Production process of ecological cordyceps sinensis wine | |
| KR101225868B1 (en) | The Method of Manufacturing of Boiled Balloon Flower Having The Effect of Alleviation of fever and the Discharge of phlegm | |
| CN107400594A (en) | A kind of dendrobium candidum health liquor and preparation method thereof | |
| CN102181352A (en) | Fleece-flower root wine and preparation method thereof | |
| CN105112213A (en) | Osmanthus honey wine for treating neuropathic stomachache | |
| CN104719534A (en) | Anti-aging tea bag and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200605 |