CN114249777A - Method for extracting icariin - Google Patents
Method for extracting icariin Download PDFInfo
- Publication number
- CN114249777A CN114249777A CN202111397884.5A CN202111397884A CN114249777A CN 114249777 A CN114249777 A CN 114249777A CN 202111397884 A CN202111397884 A CN 202111397884A CN 114249777 A CN114249777 A CN 114249777A
- Authority
- CN
- China
- Prior art keywords
- extraction
- extracting
- powder
- ultrasonic
- drying
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/14—Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P19/00—Preparation of compounds containing saccharide radicals
- C12P19/44—Preparation of O-glycosides, e.g. glucosides
- C12P19/60—Preparation of O-glycosides, e.g. glucosides having an oxygen of the saccharide radical directly bound to a non-saccharide heterocyclic ring or a condensed ring system containing a non-saccharide heterocyclic ring, e.g. coumermycin, novobiocin
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Biotechnology (AREA)
- Genetics & Genomics (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Molecular Biology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Engineering & Computer Science (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Extraction Or Liquid Replacement (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention discloses a method for extracting icariin, which comprises the following steps: cleaning herba Epimedii, drying, pulverizing to obtain herba Epimedii powder, performing microwave treatment for 1-3min, mixing with enzyme solution A, performing enzymolysis at 47-50 deg.C for 10-25min, mixing with enzyme solution B, performing enzymolysis at 47-50 deg.C for 20-30min, performing microwave treatment for 2-5min, mixing with ethanol solution and ammonia water, soaking at room temperature for 20-60min, performing ultrasonic extraction at 60-75 deg.C, concentrating, drying, and placing in supercritical CO2Extracting in an extraction device to obtain icariin, wherein the extraction comprises primary extraction and secondary extraction, and the primary extraction is performedThe temperature is 45-55 deg.C, the pressure is 25-30MPa, and the time is T1min; the secondary extraction temperature is 50-60 deg.C, pressure is 32-38MPa, and time is T2min，T1+T2＝80‑130。
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, in particular to a method for extracting icariin.
Background
Herba Epimedii is perennial herb of Epimedium of berberidaceae, and icariin is an extract of dry stem and leaf of herba Epimedii, is the main component of herba Epimedii, and has important effects of regulating immunity, resisting aging, increasing cardiovascular and cerebrovascular flow, promoting hematopoiesis, regulating endocrine, and resisting tumor. Various icariin extraction methods are disclosed at present, mainly comprising a water extraction method, an alcohol extraction method, a microwave method, an ultrasonic method and the like, but the existing methods have the defects of low extraction rate and low purity and limit the application of the methods.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for extracting icariin, which has high extraction rate and good purity of the obtained icariin.
The invention provides a method for extracting icariin, which comprises the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder;
s2, carrying out primary microwave treatment on the epimedium powder for 1-3min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.005-0.015 percent, enzymolysis is carried out for 10-25min at the temperature of 47-50 ℃, and then the mixture and enzyme solution B are mixed according to the mass ratio of 1: 0.005-0.015, performing enzymolysis at 47-50 deg.C for 20-30min, and performing secondary microwave treatment for 2-5min to obtain pretreated herba Epimedii powder; wherein the enzyme solution A is a mixture of cellulase, rhamnosidase and water, and the enzyme solution B is a mixture of pectinase, cellulase, xylosidase and water;
s3, mixing the pretreated epimedium powder, an ethanol solution and ammonia water, soaking at room temperature for 20-60min, performing ultrasonic extraction at 60-75 ℃, and concentrating and drying an extracting solution to obtain an ultrasonic extract;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 45-55 ℃, the pressure is 25-30MPa, and the time is T1min; the temperature of the secondary extraction is 50-60 ℃, the pressure is 32-38MPa, and the time is T2min, and T1+T2＝80-130。
Preferably, in S1, the drying includes drying at 70-80 ℃ for 10-25min and microwave drying for 30-90S.
Preferably, in S1, the epimedium powder with a particle size of more than 20 meshes accounts for 6.5-7 wt%, the epimedium powder with a particle size of 20-50 meshes accounts for 15-21 wt%, the epimedium powder with a particle size of 50-70 meshes accounts for 55-60 wt%, and the epimedium powder with a particle size of 70-100 meshes accounts for 10-15 wt%.
Preferably, in S2, the power of the primary microwave treatment is 400-; the power of the secondary microwave treatment is 550-650W.
Preferably, in S2, the enzyme solution a is cellulase, rhamnosidase, and water at a weight ratio of 1: 1: 5-10 of a mixture; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 5-12.
Preferably, in S3, the ratio of material to liquid in mixing is 1 g: 5-10 ml; the ethanol solution is an ethanol solution with the mass fraction of 40-45%, the ammonia water is ammonia water with the mass fraction of 20-25%, and the volume ratio of the ethanol solution to the ammonia water is 95-99: 1-5.
Preferably, in S3, the ultrasonic extraction includes primary ultrasonic extraction, secondary ultrasonic extraction, and tertiary ultrasonic extraction; the power of the primary ultrasonic extraction is 300-500W, and the time is t1min, the power of the secondary ultrasonic extraction is 600-2min, the power of the three ultrasonic extractions is 300-3min, and t1+t3＝t2＝30-60。
Preferably, in S4, during the extraction, CO2The flow rate of (A) is 18-20L/h.
Preferably, in S4, ethanol with the mass fraction of 60-70% is used as an entrainer in the primary extraction process, and the flow rate of the entrainer is 2-3 ml/min.
Preferably, in S4, T1≥2×T2+10。
Preferably, in S2, before the step of subjecting the epimedium powder to the microwave treatment, the step of subjecting the epimedium powder to an acidification treatment is further included.
Preferably, in S4, the extraction includes a first extraction and a second extraction of the raffinate of the first extraction, and the products of the first and second extractions are combined to obtain icariin.
According to the method for extracting icariin, the crushed epimedium powder is pretreated under the action of microwaves and specific enzymes, and pretreatment process parameters are controlled, so that components in epimedium are converted into icariin as much as possible, the content of icariin is increased, and the yield of subsequent steps is ensured; the epimedium powder obtained by pretreatment is subjected to ultrasonic extraction in a mixture of ethanol solution and ammonia water, the extraction rate is high, then the ultrasonic extract is subjected to supercritical extraction, the extraction has the characteristics of low-temperature extraction and inertia protection, and the purity of the obtained icariin is good while the loss of the activity of beneficial components is avoided by optimizing the extraction process conditions.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
The invention provides a method for extracting icariin, which comprises the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder; the drying comprises drying and microwave drying, wherein the drying temperature is 80 ℃, the drying time is 10min, and the microwave drying time is 90 s; in the epimedium powder, 6.5 wt% of epimedium powder with the granularity of more than 20 meshes, 20 wt% of epimedium powder with the granularity of 20-50 meshes, 58 wt% of epimedium powder with the granularity of 50-70 meshes, 10 wt% of epimedium powder with the granularity of 70-100 meshes and the balance of epimedium powder with the granularity of less than 100 meshes are adopted;
s2, carrying out primary microwave treatment on the epimedium powder for 3min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.005, performing enzymolysis for 10min at the temperature of 50 ℃, and then mixing the mixture with an enzyme solution B according to the mass ratio of 1: 0.015 mixing, carrying out enzymolysis for 28min at the temperature of 47 ℃, and then carrying out secondary microwave treatment for 5min to obtain pretreated epimedium powder; wherein the power of the primary microwave treatment is 500W; the power of the secondary microwave treatment is 550W; the enzyme solution A is prepared from cellulase, rhamnosidase and water in a weight ratio of 1: 1: 5 with a mixture of; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 12 with a solvent;
s3, according to the weight ratio of 1 g: mixing pretreated herba Epimedii powder, ethanol solution, and ammonia water at a material-to-liquid ratio of 5ml, soaking at room temperature for 50min, performing ultrasonic extraction at 60 deg.C, concentrating the extractive solution, and drying to obtain ultrasonic extract; the ethanol solution is 42% by mass, the ammonia water is 20% by mass, and the volume ratio of the ethanol solution to the ammonia water is 99: 1; the ultrasonic extraction comprises primary ultrasonic extraction, secondary ultrasonic extraction and tertiary ultrasonic extraction; the power of the primary ultrasonic extraction is 300W, the time is 20min, the power of the secondary ultrasonic extraction is 700W, the time is 60min, the power of the tertiary ultrasonic extraction is 500W, and the time is 40 min;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain the icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 55 ℃, the pressure is 25MPa, and the time is 90 min; the temperature of the secondary extraction is 60 ℃, the pressure is 32MPa, and the time is 40 min; in the extraction process, CO2The flow rate of (2) is 18L/h; in the primary extraction process, ethanol with the mass fraction of 60% is used as an entrainer, the flow rate of the entrainer is 3ml/min, and in the secondary extraction process, the entrainer is not contained.
Example 2
The invention provides a method for extracting icariin, which comprises the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder; the drying comprises drying and microwave drying, wherein the drying temperature is 70 ℃, the drying time is 25min, and the microwave drying time is 30 s; in the epimedium powder, 7 wt% of epimedium powder with the granularity of more than 20 meshes, 15 wt% of epimedium powder with the granularity of 20-50 meshes, 60 wt% of epimedium powder with the granularity of 50-70 meshes, 15 wt% of epimedium powder with the granularity of 70-100 meshes and the balance of epimedium powder with the granularity of less than 100 meshes are used;
s2, carrying out primary microwave treatment on the epimedium powder for 1min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.015, carrying out enzymolysis for 25min at the temperature of 47 ℃, and then mixing the mixture with an enzyme solution B according to the mass ratio of 1: 0.005 mixing, performing enzymolysis at 48 deg.C for 30min, and performing secondary microwave treatment for 4min to obtain pretreated herba Epimedii powder; wherein the power of the primary microwave treatment is 400W; the power of the secondary microwave treatment is 650W; the enzyme solution A is prepared from cellulase, rhamnosidase and water in a weight ratio of 1: 1: 10, a mixture of; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 5 with a mixture of;
s3, mixing the pretreated epimedium powder, an ethanol solution and ammonia water, soaking for 60min at room temperature, carrying out ultrasonic extraction at 75 ℃, and concentrating and drying an extracting solution to obtain an ultrasonic extract; wherein, the ratio of material to liquid in mixing is 1 g: 8ml of the solution; the ethanol solution is an ethanol solution with the mass fraction of 45%, the ammonia water is ammonia water with the mass fraction of 25%, and the volume ratio of the ethanol solution to the ammonia water is 95: 5; the ultrasonic extraction comprises primary ultrasonic extraction, secondary ultrasonic extraction and tertiary ultrasonic extraction; the power of the primary ultrasonic extraction is 500W, the time is 10min, the power of the secondary ultrasonic extraction is 600W, the time is 30min, the power of the tertiary ultrasonic extraction is 300W, and the time is 20 min;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain the icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 45 ℃, the pressure is 30MPa, and the time is 60 min; the temperature of the secondary extraction is 50 ℃, the pressure is 38MPa, and the time is 20 min; wherein, in the extraction process, CO2The flow rate of (2) is 20L/h; in the primary extraction process, ethanol with the mass fraction of 70% is used as an entrainer, and the flow rate of the entrainer is 2 ml/min.
Example 3
The invention provides a method for extracting icariin, which comprises the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder; the drying comprises drying and microwave drying, wherein the drying temperature is 72 ℃, the drying time is 22min, and the microwave drying time is 40 s; in the epimedium powder, 6.8 wt% of epimedium powder with the granularity of more than 20 meshes, 21 wt% of epimedium powder with the granularity of 20-50 meshes, 55 wt% of epimedium powder with the granularity of 50-70 meshes, 14 wt% of epimedium powder with the granularity of 70-100 meshes and the balance of epimedium powder with the granularity of less than 100 meshes are adopted;
s2, carrying out primary microwave treatment on the epimedium powder for 2min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.008, carrying out enzymolysis for 15min at 50 ℃, and then mixing the mixture with an enzyme solution B according to the mass ratio of 1: 0.01, performing enzymolysis at 50 ℃ for 20min, and performing secondary microwave treatment for 2min to obtain pretreated herba Epimedii powder; wherein the power of the primary microwave treatment is 480W; the power of the secondary microwave treatment is 550W; the enzyme solution A is prepared from cellulase, rhamnosidase and water in a weight ratio of 1: 1: 6; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 10, a mixture of;
s3, mixing the pretreated epimedium powder, an ethanol solution and ammonia water, soaking for 20min at room temperature, performing ultrasonic extraction at 65 ℃, and concentrating and drying an extracting solution to obtain an ultrasonic extract; wherein, the ratio of material to liquid in mixing is 1 g: 10 ml; the ethanol solution is an ethanol solution with the mass fraction of 40%, the ammonia water is ammonia water with the mass fraction of 24%, and the volume ratio of the ethanol solution to the ammonia water is 97: 3; the ultrasonic extraction comprises primary ultrasonic extraction, secondary ultrasonic extraction and tertiary ultrasonic extraction; the power of the primary ultrasonic extraction is 300W, the time is 20min, the power of the secondary ultrasonic extraction is 700W, the time is 50min, the power of the tertiary ultrasonic extraction is 300W, and the time is 30 min;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain the icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 50 ℃, the pressure is 26MPa, and the time is 70 min; the temperature of the secondary extraction is 52 ℃, the pressure is 35MPa, and the time is 30 min; wherein, in the extraction process，CO2The flow rate of (2) is 19L/h; in the primary extraction process, ethanol with the mass fraction of 70% is used as an entrainer, and the flow rate of the entrainer is 2.2 ml/min.
Example 4
The invention provides a method for extracting icariin, which comprises the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder;
s2, carrying out primary microwave treatment on the epimedium powder for 1min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.01, performing enzymolysis for 20min at the temperature of 48 ℃, and then mixing the mixture with an enzyme solution B according to the mass ratio of 1: 0.005 mixing, performing enzymolysis at 47 deg.C for 30min, and performing secondary microwave treatment for 3min to obtain pretreated herba Epimedii powder;
s3, mixing the pretreated epimedium powder, an ethanol solution and ammonia water, soaking for 30min at room temperature, carrying out ultrasonic extraction at 72 ℃, and concentrating and drying an extracting solution to obtain an ultrasonic extract;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain the icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 48 ℃, the pressure is 28MPa, and the time is 70 min; the temperature of the secondary extraction is 58 ℃, the pressure is 37MPa, and the time is 20 min;
in S1, the drying includes drying at 78 deg.C for 16min and microwave drying for 80S; in the epimedium powder, 6.9 wt% of epimedium powder with the granularity of more than 20 meshes, 17 wt% of epimedium powder with the granularity of 20-50 meshes, 58 wt% of epimedium powder with the granularity of 50-70 meshes and 12 wt% of epimedium powder with the granularity of 70-100 meshes are contained;
in S2, the power of the primary microwave treatment is 450W; the power of the secondary microwave treatment is 600W; the enzyme solution A is prepared from cellulase, rhamnosidase and water in a weight ratio of 1: 1: 8, a mixture of; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 7;
in S3, the ratio of the materials to the liquid is 1 g: 8ml of the solution; the ethanol solution is 43% by mass, the ammonia water is 22% by mass, and the volume ratio of the ethanol solution to the ammonia water is 98: 2; the ultrasonic extraction comprises primary ultrasonic extraction, secondary ultrasonic extraction and tertiary ultrasonic extraction; the power of the primary ultrasonic extraction is 500W, the time is 10min, the power of the secondary ultrasonic extraction is 600W, the time is 40min, the power of the tertiary ultrasonic extraction is 500W, and the time is 30 min;
in S4, CO is introduced into the extraction process2The flow rate of (A) is 18.6L/h; in the primary extraction process, 65% by mass of ethanol is used as an entrainer, the flow rate of the entrainer is 2.7ml/min, and in the secondary extraction process, the entrainer is not contained.
Example 5
The invention provides a method for extracting icariin, which comprises the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder; the drying comprises drying and microwave drying, wherein the drying temperature is 75 ℃, the drying time is 22min, and the microwave drying time is 45 s; in the epimedium powder, 7 wt% of epimedium powder with the granularity of more than 20 meshes, 20 wt% of epimedium powder with the granularity of 20-50 meshes, 57 wt% of epimedium powder with the granularity of 50-70 meshes and 11 wt% of epimedium powder with the granularity of 70-100 meshes are contained;
s2, carrying out primary microwave treatment on the epimedium powder for 2min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.01, carrying out enzymolysis for 15min at the temperature of 50 ℃, and then mixing the mixture with an enzyme solution B according to the mass ratio of 1: 0.01, performing enzymolysis at 50 ℃ for 20min, and performing secondary microwave treatment for 4min to obtain pretreated herba Epimedii powder; wherein the power of the primary microwave treatment is 400W; the power of the secondary microwave treatment is 650W; the enzyme solution A is prepared from cellulase, rhamnosidase and water in a weight ratio of 1: 1: 7; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 9, a mixture thereof;
s3, mixing the pretreated epimedium powder, an ethanol solution and ammonia water, soaking for 30min at room temperature, carrying out ultrasonic extraction at 70 ℃, and concentrating and drying an extracting solution to obtain an ultrasonic extract; wherein, the ratio of material to liquid in mixing is 1 g: 8ml of the solution; the ethanol solution is 42% by mass, the ammonia water is 23% by mass, and the volume ratio of the ethanol solution to the ammonia water is 97: 3; the ultrasonic extraction comprises primary ultrasonic extraction, secondary ultrasonic extraction and tertiary ultrasonic extraction; the power of the primary ultrasonic extraction is 400W, the time is 30min, the power of the secondary ultrasonic extraction is 600W, the time is 45min, the power of the tertiary ultrasonic extraction is 300W, and the time is 15 min;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain the icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 50 ℃, the pressure is 27MPa, and the time is 80 min; the temperature of the secondary extraction is 53 ℃, the pressure is 36MPa, and the time is 30 min; wherein, in the extraction process, CO2The flow rate of (2) is 19L/h; in the primary extraction process, 65% by mass of ethanol is used as an entrainer, and the flow rate of the entrainer is 2 ml/min.
Comparative example 1
The only difference from example 5 is that: it does not include S2, but the epimedium powder in S1 is directly subjected to the ultrasonic extraction process of S3.
Comparative example 2
The only difference from example 5 is that: it does not include S3, but directly performs the extraction process of S4 on the pretreated epimedium powder obtained from S2.
Comparative example 3
The only difference from example 5 is that: it does not include S2 and S3, but directly performs the extraction process of S4 on the epimedium powder obtained from S1.
Comparative example 4
The only difference from example 5 is that: the extraction process of S4 included only one extraction, and did not involve a second extraction.
Comparative example 5
The only difference from example 5 is that: the extraction process of S4 was performed only for the second extraction process, and not for the first extraction process.
Comparative example 6
The only difference from example 5 is that: in S1, the herba Epimedii powder is 20-50 mesh.
Comparative example 7
The only difference from example 5 is that: in S4, the primary extraction time is 80 min; the time of the secondary extraction is 50 min.
Analysis of the products prepared by the methods of examples 1-5 and comparative examples 1-7 of the present invention shows that the purity of icariin of examples 1-5 is greater than or equal to 65.9%, and the recovery rate is greater than or equal to 93.3%, while the purity of icariin of comparative examples 1-7 is less than 64.5%, and the recovery rate is less than 84.7%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A method for extracting icariin is characterized by comprising the following steps:
s1, cleaning herba Epimedii, drying, and pulverizing to obtain herba Epimedii powder;
s2, carrying out primary microwave treatment on the epimedium powder for 1-3min, and mixing the epimedium powder with the enzyme solution A according to the mass ratio of 1: 0.005-0.015 percent, enzymolysis is carried out for 10-25min at the temperature of 47-50 ℃, and then the mixture and enzyme solution B are mixed according to the mass ratio of 1: 0.005-0.015, performing enzymolysis at 47-50 deg.C for 20-30min, and performing secondary microwave treatment for 2-5min to obtain pretreated herba Epimedii powder; wherein the enzyme solution A is a mixture of cellulase, rhamnosidase and water, and the enzyme solution B is a mixture of pectinase, cellulase, xylosidase and water;
s3, mixing the pretreated epimedium powder, an ethanol solution and ammonia water, soaking at room temperature for 20-60min, performing ultrasonic extraction at 60-75 ℃, and concentrating and drying an extracting solution to obtain an ultrasonic extract;
s4, placing the ultrasonic extract obtained in S3 in supercritical CO2Extracting in an extraction device to obtain icariin, wherein the extraction comprises primary extraction and secondary extraction, the temperature of the primary extraction is 45-55 ℃, the pressure is 25-30MPa, and the time is T1min; the temperature of the secondary extraction is 50-60 ℃, the pressure is 32-38MPa, and the time is T2min, and T1+T2＝80-130。
2. The method for extracting icariin according to claim 1, wherein in S1, the drying includes oven drying at 70-80 ℃ for 10-25min and microwave drying for 30-90S.
3. The method for extracting icariin according to claim 1 or 2, wherein in S1, in the epimedium powder, 6.5 to 7 wt% of epimedium powder with a particle size of more than 20 meshes, 15 to 21 wt% of epimedium powder with a particle size of 20 to 50 meshes, 55 to 60 wt% of epimedium powder with a particle size of 50 to 70 meshes, and 10 to 15 wt% of epimedium powder with a particle size of 70 to 100 meshes are contained.
4. The method for extracting icariin according to any one of claims 1 to 3, wherein in S2, the power of the primary microwave treatment is 400-500W; the power of the secondary microwave treatment is 550-650W.
5. The method for extracting icariin according to any one of claims 1 to 4, wherein in S2, the enzyme solution A is cellulase, rhamnosidase and water in a weight ratio of 1: 1: 5-10 of a mixture; the enzyme solution B is prepared from pectinase, cellulase, xylosidase and water in a weight ratio of 1: 1: 1: 5-12.
6. The method for extracting icariin according to any one of claims 1 to 5, wherein in S3, the ratio of feed to liquid at the time of mixing is 1 g: 5-10 ml; the ethanol solution is an ethanol solution with the mass fraction of 40-45%, the ammonia water is ammonia water with the mass fraction of 20-25%, and the volume ratio of the ethanol solution to the ammonia water is 95-99: 1-5.
7. The method for extracting icariin according to any one of claims 1 to 6, wherein in S3, the ultrasonic extraction includes one ultrasonic extraction, two ultrasonic extractions, and three ultrasonic extractions; the power of the primary ultrasonic extraction is 300-500W, and the time is t1min, the power of the secondary ultrasonic extraction is 600-2min, the power of the three ultrasonic extractions is 300-3min, and t1+t3＝t2＝30-60。
8. The method for extracting icariin according to any one of claims 1 to 7, wherein in S4, CO is added during the extraction process2The flow rate of (A) is 18-20L/h.
9. The method for extracting icariin according to any one of claims 1 to 8, wherein in S4, ethanol with a mass fraction of 60 to 70% is used as an entrainer in the primary extraction process, and the flow rate of the entrainer is 2 to 3 ml/min.
10. The process for extracting icariin according to any one of claims 1 to 9, wherein in S4, T is1≥2×T2+10。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111397884.5A CN114249777A (en) | 2021-11-19 | 2021-11-19 | Method for extracting icariin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111397884.5A CN114249777A (en) | 2021-11-19 | 2021-11-19 | Method for extracting icariin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN114249777A true CN114249777A (en) | 2022-03-29 |
Family
ID=80791085
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111397884.5A Pending CN114249777A (en) | 2021-11-19 | 2021-11-19 | Method for extracting icariin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114249777A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807595A (en) * | 2011-06-02 | 2012-12-05 | 汉中天然谷生物科技有限公司 | Technique for preparing high-content (98 percent) icariin from Epimedium plant |
| CN103865913A (en) * | 2014-04-02 | 2014-06-18 | 济南诺能生物工程有限公司 | Compound enzyme and method for extracting effective ingredients in Chinese herbal medicines by virtue of compound enzyme |
| CN106146574A (en) * | 2016-06-17 | 2016-11-23 | 蚌埠市华东生物科技有限公司 | A kind of method of stevioside in microwave ultrasound compound collecting leaf of Folium Stevlae Rebaudianae |
| CN107412429A (en) * | 2017-09-11 | 2017-12-01 | 江西华太药业有限公司 | A kind of bone increases capsule for eliminating and preparation method |
| CN108440620A (en) * | 2018-04-26 | 2018-08-24 | 赣州禾绿康健生物技术有限公司 | A kind of preparation method of high-content icariin extract |
| CN109295121A (en) * | 2018-11-05 | 2019-02-01 | 重庆大学 | A kind of method that enzymatic isolation method prepares icariin |
| CN111440222A (en) * | 2020-05-22 | 2020-07-24 | 汉中天然谷生物科技股份有限公司 | Method for extracting icariin |
| CN111560409A (en) * | 2020-05-08 | 2020-08-21 | 陕西嘉禾生物科技股份有限公司 | Preparation method of icariine |
| CN111635439A (en) * | 2020-06-10 | 2020-09-08 | 劲牌持正堂药业有限公司 | Process method for improving yield of icariin |
-
2021
- 2021-11-19 CN CN202111397884.5A patent/CN114249777A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807595A (en) * | 2011-06-02 | 2012-12-05 | 汉中天然谷生物科技有限公司 | Technique for preparing high-content (98 percent) icariin from Epimedium plant |
| CN103865913A (en) * | 2014-04-02 | 2014-06-18 | 济南诺能生物工程有限公司 | Compound enzyme and method for extracting effective ingredients in Chinese herbal medicines by virtue of compound enzyme |
| CN106146574A (en) * | 2016-06-17 | 2016-11-23 | 蚌埠市华东生物科技有限公司 | A kind of method of stevioside in microwave ultrasound compound collecting leaf of Folium Stevlae Rebaudianae |
| CN107412429A (en) * | 2017-09-11 | 2017-12-01 | 江西华太药业有限公司 | A kind of bone increases capsule for eliminating and preparation method |
| CN108440620A (en) * | 2018-04-26 | 2018-08-24 | 赣州禾绿康健生物技术有限公司 | A kind of preparation method of high-content icariin extract |
| CN109295121A (en) * | 2018-11-05 | 2019-02-01 | 重庆大学 | A kind of method that enzymatic isolation method prepares icariin |
| CN111560409A (en) * | 2020-05-08 | 2020-08-21 | 陕西嘉禾生物科技股份有限公司 | Preparation method of icariine |
| CN111440222A (en) * | 2020-05-22 | 2020-07-24 | 汉中天然谷生物科技股份有限公司 | Method for extracting icariin |
| CN111635439A (en) * | 2020-06-10 | 2020-09-08 | 劲牌持正堂药业有限公司 | Process method for improving yield of icariin |
Non-Patent Citations (3)
| Title |
|---|
| 何晨，等: "淫羊藿中活性成分淫羊藿苷提取工艺研究现状", 亚太传统医药, vol. 12, no. 02, pages 56 * |
| 廖华军;: "中药提取新技术研究进展", 福建分析测试, no. 01, pages 25 - 30 * |
| 曾惠玲: "中药化学成分提取新技术研究进展", 海峡药学, no. 05, pages 5 - 7 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106146574B (en) | A kind of method that microwave-ULTRASONIC COMPLEX extracts steviol glycoside in stevioside leaf | |
| CN105505558A (en) | Method for synchronously extracting soybean oil, soybean milk powder and soybean dietary fiber by aqueous enzymatic method | |
| CN102432480A (en) | Method for extracting lycine from Chinese wolfberry leaves | |
| CN110437931A (en) | A kind of processing technology of low acid value Fructus Zanthoxyli oil | |
| CN104289007A (en) | Continuous phase change-based method for extracting tea polyphenol | |
| CN115137092B (en) | Method for preparing tobacco extract by using low-temperature plasma-assisted ionic liquid | |
| CN114249777A (en) | Method for extracting icariin | |
| CN108570350A (en) | A kind of extracting method of Fructus cinnamomi camphorae volatile oil | |
| CN102824291A (en) | Dandruff-removing and itching-relieving shampoo and preparation method thereof | |
| CN101982191A (en) | Method for extracting fat-reducing compound functional materials from lotus leaves | |
| CN102178739A (en) | Method for extracting flavone by using surfactant from herb to coordinate with enzymolysis-microwave | |
| CN111484500A (en) | Preparation method of tetrandrine | |
| CN105348405A (en) | Microwave extraction method for spirulina polysaccharide | |
| CN103059158A (en) | Method for inhibiting foam generation in tea flower polysaccharide extraction | |
| CN104152262A (en) | Method for co-producing eucommia seed oil, eucommia rubber and eucommia extract by refining eucommia fruits through steam explosion | |
| CN105395592A (en) | Method for preparing maea extract through ultrasonic wave countercurrent | |
| CN103467534B (en) | Method for extracting punicalagin from pomegranate bark | |
| CN111187321A (en) | Preparation method of myricitrin | |
| CN106344725A (en) | Method for extracting flavone from herba violae | |
| KR20140002315A (en) | Method for converting and producing functional saponin from ginseng extract using subcritical water and composition using the same | |
| CN107163016B (en) | The method for extracting isoflavones using soy molasses | |
| CN105198952A (en) | Extraction method of tea saponin | |
| CN102366518B (en) | Method for ultrasonic assisted aqueous two-phase extraction of total dioscin | |
| CN106866836A (en) | A kind of method that pectin is extracted from pear skin | |
| CN112521525A (en) | Production process for separating and purifying beta-glucan from oat bran |
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 |