CN116392557A - Fructus alpiniae oxyphyllae extract and extraction process thereof - Google Patents
Fructus alpiniae oxyphyllae extract and extraction process thereof Download PDFInfo
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/906—Zingiberaceae (Ginger family)
- A61K36/9062—Alpinia, e.g. red ginger or galangal
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/50—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates
- A61K47/69—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit
- A61K47/6949—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes
- A61K47/6951—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient the non-active ingredient being chemically bound to the active ingredient, e.g. polymer-drug conjugates the conjugate being characterised by physical or galenical forms, e.g. emulsion, particle, inclusion complex, stent or kit inclusion complexes, e.g. clathrates, cavitates or fullerenes using cyclodextrin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
- A61K9/141—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers
- A61K9/146—Intimate drug-carrier mixtures characterised by the carrier, e.g. ordered mixtures, adsorbates, solid solutions, eutectica, co-dried, co-solubilised, co-kneaded, co-milled, co-ground products, co-precipitates, co-evaporates, co-extrudates, co-melts; Drug nanoparticles with adsorbed surface modifiers with organic macromolecular compounds
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- 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
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- 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
- B01D11/0261—Solvent extraction of solids comprising vibrating mechanisms, e.g. mechanical, acoustical
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
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- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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Abstract
The invention relates to the technical field of extraction of plant active ingredients, in particular to a fructus alpiniae oxyphyllae extract and an extraction process thereof, wherein the extraction process specifically comprises the following steps: s1, pretreatment of medicinal materials; s2, extracting volatile oil components; s3, filtering and concentrating; s4, standing and removing impurities; s5, shearing inclusion; s6, vacuum concentration; s7, drying, crushing and sieving to obtain the target extract. The method has the advantages of convenient operation and strong flexibility, and the method pretreats the medicinal material fine powder by microwaves and then passes through supercritical CO 2 Extracting, and wrapping with HH-beta-CD, HP-beta-CD, beta-CD complexThe volatile oil substances in the fructus alpiniae oxyphyllae can finally obtain the product in the form of powder. Through detection, the content of the active substance nocardione in the fructus alpiniae oxyphyllae extract provided by the invention is obviously improved, the stability of the active ingredient is high, the fructus alpiniae oxyphyllae extract is convenient for long-term storage, and the fructus alpiniae oxyphyllae extract is suitable for the combined preparation of various later dosage forms.
Description
Technical Field
The invention relates to the technical field of extraction of plant active ingredients, in particular to a fructus alpiniae oxyphyllae extract and an extraction process thereof.
Background
Fructus Alpinae Oxyphyllae is fruit of Alpinia oxyphylla of Zingiberaceae, and is a pungent and warm Chinese medicinal material. The fructus alpiniae oxyphyllae medicinal material contains more volatile oil components, so the fructus alpiniae oxyphyllae medicinal material has the characteristics of difficult water dissolution, easy volatilization, easy oxidation and instability, is not suitable for independently preparing a traditional Chinese medicine preparation in the prior art, and generally forms a medicament in the form of wine soaking or a compound preparation. The method has low efficiency and low treatment efficiency. Nootkatone, also known as naringin, is a naturally occurring sesquiterpene compound, and is a herbal extract with a beneficial effect. Nocarpus is generally extracted from grapefruits by chemical combination or biochemical oxidation and is found in both Alaska yellow tree and vetiveria zizanioides. The effective component in the fructus alpiniae oxyphyllae medicinal material is also nocardiac ketone, and the content of nocardiac ketone in the raw medicinal material is lower than 0.2%, so that the production of the subsequent medicinal preparation cannot be satisfied, and therefore, an extraction process for extracting the extract with the improved content of the effective component is required.
The patent CN104127468B discloses a preparation and extraction process of a maca extract, and particularly discloses a method for preparing the extract by leaching, filtering and freeze-drying, wherein the patent is concentrated powder of active ingredients in maca roots, which is extracted by adopting the technologies of ultrahigh pressure enzyme deactivation, superfine wall breaking and crushing, surfactant ultrasonic synergistic extraction, ultrafiltration concentration and ultralow temperature drying. The extraction process does not involve a shearing inclusion process, and the content of the obtained maca extract is measured by detecting the content of three substances, namely benzyl glucosinolate, total flavone and total saponin, and the quality of the extract cannot be directly, obviously and objectively reflected.
Disclosure of Invention
The invention aims to provide a fructus alpiniae oxyphyllae extract and an extraction process thereof, so as to solve the problems in the background art.
The invention is realized by the following technical scheme:
an extraction process of fructus alpiniae oxyphyllae extract specifically comprises the following steps:
s1, pretreatment of medicinal materials: removing impurities from fructus alpiniae oxyphyllae raw materials, crushing the fructus alpiniae oxyphyllae raw materials by a crusher, sieving the crushed raw materials to obtain medicinal fine powder, carrying out microwave pretreatment on the obtained medicinal fine powder by a solvent-free microwave method, wherein the heating time of the microwave pretreatment is set to be 25-30 min, the microwave is set to be 300-450W when the heating time is 0-20 min, the microwave is set to be 180-280W when the heating time exceeds 20min, and extracting solutions are collected once every 5-10 min, and the extracting solutions are obtained after the mixing;
s2, extracting volatile oil components: then the combined extracting solution obtained in the step S1 is put into an extraction kettle, and supercritical CO is utilized 2 (SC-CO 2 ) Extracting CO 2 The flow is 8-15 kg/h, after extraction, the liquid is fed into a separating kettle which is cooled to room temperature in a stepped way for separation to obtain extraction liquid, the extraction time is 0.5-2 h each time, and the extraction times are not less than 2 times;
s3, filtering and concentrating: filtering the extracting solution obtained in the step S2 to obtain filtrate, and concentrating the filtrate in vacuum to obtain concentrated solution;
s4, standing and impurity removal: cooling the concentrated solution obtained in the step S3 to 2-8 ℃, standing for 8-12 hours to obtain layered extract and upper solution, discarding a liquid part, adding the extract into an extraction solvent, stirring in a water bath at 50-80 ℃ until the extract is completely dissolved, and carrying out suction filtration through filter paper to obtain filtrate;
s5, shearing inclusion: adding 0.5-1.0% of emulsifying agent into the filtrate obtained in the step S4, namely, the adding amount of the emulsifying agent is 0.5-1.0% of the weight of the medicinal materials, stirring for 20-30 min at the water bath of 40-60 ℃ at the rotating speed of 8000-10000 r/min, adding 5-10% of compound, namely, the adding amount of the compound is 5-10% of the weight of the medicinal materials, and continuing homogenizing for 20-30 min at the rotating speed of 8000-10000 r/min to obtain a uniformly mixed clathrate compound solution;
s6, vacuum concentration: feeding the inclusion compound solution obtained in the step S5 into a rotary evaporator, concentrating in vacuum until the relative density is 1.1-1.3, and discharging to obtain a concentrate;
s7, drying and crushing: drying the concentrate obtained in the step S6 in a hot air circulation drying box at 60-90 ℃ until the concentrate is pasty, transferring the concentrate into a vacuum drying box, drying the concentrate for 24-48 hours at 60-70 ℃ and-0.1 MPa, crushing the concentrate, and sieving the crushed concentrate with a 80-mesh sieve to obtain the target extract.
Preferably, in the step S1, a R40/3 series 1 medicine sieve which accords with the national standard ISO 3310-1 or the standard of Chinese pharmacopoeia is adopted for sieving, the inner diameter of a sieve hole of the adopted medicine sieve is 2000+/-70 mu m, and the mesh number of the adopted medicine sieve is 10 meshes.
Preferably, in the step S2, the temperature of the extraction kettle is set to be 35-50 ℃, and the pressure of the extraction kettle is set to be 10-18 MPa.
As a further scheme of the invention, in the step S2, the temperature of the separation kettle is reduced stepwise from 30-50 ℃ to room temperature, the temperature reduction range is 5 ℃/10min, and the pressure of the separation kettle is set to 6-10 MPa.
As a further scheme of the invention, in the steps S3 and S6, the vacuum degree is set to be-0.09 MPa and the temperature is 50-70 ℃.
In the step S4, the extracting solvent is selected from 60-90% food grade alcohol, and the ratio of the extract to the extracting solvent is 1:2 to 5.
As a further aspect of the present invention, in step S5, the emulsifier is at least one selected from the group consisting of a mono-di-glycerin fatty acid ester, sodium starch octenyl succinate, and sodium carboxymethyl cellulose.
As a further scheme of the invention, in the step S5, the compound is a mixture of HH-beta-CD, HP-beta-CD and beta-CD, wherein the weight ratio of HH-beta-CD, HP-beta-CD and beta-CD is 0.1-0.5: 0.5 to 3:1.
as a further aspect of the present invention, the HH- β -CD is selected from any one of HH-TM- β -CD, HH-HP- β -CD, HH-M- β -CD, HH-DM- β -CD.
The invention also provides the fructus alpiniae oxyphyllae extract prepared by the extraction process, and the content of the effective component of the fructus alpiniae oxyphyllae extract is at least 7 times of that of the fructus alpiniae oxyphyllae raw material.
Compared with the prior art, the invention has the beneficial effects that:
the method has the advantages of convenient operation and strong flexibility, and the method pretreats the medicinal material fine powder by microwaves and then passes through supercritical CO 2 Extracting, and coating volatile oil substances in fructus Alpinae Oxyphyllae with HH-beta-CD, HP-beta-CD, and beta-CD complex to obtain powder product. Through detection, the invention provides intelligence developmentThe content of active ingredient nocardione in the kernel extract is obviously improved, the stability of active ingredients is high, the kernel extract is convenient for long-term storage, and the kernel extract is suitable for the combined preparation of various dosage forms in the later period.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a HPLC detection spectrum of fructus Alpinae Oxyphyllae extract provided by the invention;
FIG. 2 is a HPLC detection spectrum of nocardione control;
FIG. 3 is a schematic diagram showing the detection results of the fructus Alpinae Oxyphyllae extract of the present invention after an accelerated test at 40deg.C;
FIG. 4 is a schematic diagram showing the detection results of the fructus Alpinae Oxyphyllae extract of the present invention after 30℃acceleration test;
FIG. 5 is a schematic diagram showing the results of the accelerated test of the target extract at 40℃according to the present invention;
FIG. 6 is a schematic diagram showing the results of the 30℃accelerated test of the target extract of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Unless otherwise specified, the reagents, HH-. Beta. -CD, HP-. Beta. -CD, and the like used in the examples of the present invention were readily available from commercial companies, and the differences in the model numbers thereof were all within the limits of the errors to be made in the present application.
The alcohol used in the embodiment of the invention is food grade alcohol meeting the national edible alcohol quality standard GB 10343-2008.
Example 1:
the embodiment provides an extraction process of a fructus alpiniae oxyphyllae extract, which specifically comprises the following steps:
s1, pretreatment of medicinal materials: removing impurities from fructus Alpinae Oxyphyllae, pulverizing with pulverizer, sieving with R40/3 series 1 sieve conforming to national standard ISO 3310-1 or Chinese pharmacopoeia standard to obtain fine powder, wherein the mesh diameter of the sieve is 2000+ -70 μm, and the mesh number is 10 mesh;
weighing 500g of medicinal material fine powder, performing microwave pretreatment on the medicinal material fine powder by adopting a solvent-free microwave method, setting the microwave heating time to be 25-30 min, setting the microwave to be 300W when the microwave heating time is 0-20 min, setting the microwave to be 250W after the microwave heating time exceeds 20min, collecting the extracting solution every 5-10 min, and merging to obtain the extracting solution;
s2, extracting volatile oil components: putting the combined extract obtained in the step S1 into an extraction kettle, and utilizing supercritical CO 2 Extracting and setting CO 2 The flow is 10kg/h, and after extraction, the mixture is introduced into a separating kettle which is cooled to room temperature in a stepped way to obtain extraction liquid; the temperature of the extraction kettle is set to be 50 ℃, the pressure of the extraction kettle is set to be 16MPa, the extraction time is 0.5-2 h each time, and the extraction times are not less than 2 times; the pressure of the separation kettle is set to be 6MPa, the temperature is reduced stepwise from 30-50 ℃ to room temperature, and the temperature reduction range is 5 ℃/10min;
s3, filtering and concentrating: concentrating the extracting solution obtained in the step S2 in vacuum by a rotary evaporator until no alcohol exists, and obtaining concentrated solution, wherein the vacuum degree is set to be-0.09 MPa and the temperature is 65 ℃ during vacuum concentration;
s4, standing and impurity removal: pouring out the concentrated solution obtained in the step S3 while the concentrated solution is hot, cooling to 2-8 ℃, standing for 8-12 h to obtain layered extract and upper layer solution, wherein the extract is added into 80% food grade alcohol serving as an extraction solvent, and the feed-liquid ratio is 1:4, stirring in a water bath at 70+/-5 ℃ until the mixture is completely dissolved, and carrying out suction filtration through filter paper to obtain filtrate;
s5, shearing inclusion: after the filtrate obtained in the step S4 is cooled to 55 ℃, 0.5 percent of mono-diglyceride fatty acid ester is added into the filtrate as an emulsifier, the mixture is stirred for 20 to 30 minutes at the constant temperature water bath of 55 ℃ at the rotating speed of 8000r/min, and then 5 to 10 percent of compound is added, wherein the weight ratio of the compound is 0.1:1:1 HH-beta-CD, HP-beta-CD and beta-CD, continuously homogenizing at 8000r/min for 20-30 min, and coating volatile oil substances in fructus Alpinae Oxyphyllae with the compound to obtain clathrate solution which is uniformly mixed;
wherein, HH-beta-CD is selected from HH-TM-beta-CD, HH-HP-beta-CD, HH-M-beta-CD, HH-DM-beta-CD, and HH-M-beta-CD has optimal antioxidant activity, so that HH-beta-CD adopted in the embodiment adopts HH-M-beta-CD;
s6, vacuum concentration: feeding the inclusion compound solution obtained in the step S5 into a rotary evaporator, vacuum concentrating until the relative density is 1.2, and discharging to obtain a concentrate, wherein the vacuum degree is set to be-0.09 MPa and the temperature is 65 ℃ during vacuum concentration;
s7, drying and crushing: drying the concentrate obtained in the step S6 in a hot air circulation drying oven at 85 ℃ until the concentrate is pasty, transferring the concentrate into a vacuum drying oven, drying the concentrate for 30 hours at 65 ℃ under the vacuum degree of-0.1 MPa, crushing the concentrate, and sieving the crushed powder with a 80-mesh sieve to obtain the target extract.
The embodiment also provides a fructus alpiniae oxyphyllae extract prepared by the extraction process, the yield is 13.21%, and the nootkatone content in the extract is 0.997% after HPLC detection.
Example 2:
the embodiment provides an extraction process of a fructus alpiniae oxyphyllae extract, which specifically comprises the following steps:
s1, pretreatment of medicinal materials: removing impurities from fructus Alpinae Oxyphyllae, pulverizing with pulverizer, sieving with R40/3 series 1 sieve conforming to national standard ISO 3310-1 or Chinese pharmacopoeia standard to obtain fine powder, wherein the mesh diameter of the sieve is 2000+ -70 μm, and the mesh number is 10 mesh;
weighing 500g of medicinal material fine powder, performing microwave pretreatment on the medicinal material fine powder by adopting a solvent-free microwave method, setting the microwave heating time to be 25-30 min, setting the microwave to be 400W when the microwave heating time is 0-20 min, setting the microwave to be 200W after the microwave heating time exceeds 20min, collecting the extracting solution every 5-10 min, and merging to obtain the extracting solution;
s2, extracting volatile oil components: putting the combined extract obtained in the step S1 into an extraction kettle for benefitingBy supercritical CO 2 Extracting and setting CO 2 The flow is 12kg/h, and after extraction, the mixture is introduced into a separating kettle which is cooled to room temperature in a stepped way to obtain extraction liquid; the temperature of the extraction kettle is set to 40 ℃, the pressure of the extraction kettle is set to 18MPa, the extraction time is 0.5-2 h each time, and the extraction times are not less than 2 times; the pressure of the separation kettle is set to be 8MPa, the temperature is reduced stepwise from 30-40 ℃ to room temperature, and the temperature reduction range is 5 ℃/10min;
s3, filtering and concentrating: concentrating the extracting solution obtained in the step S2 in vacuum by a rotary evaporator until no alcohol exists, and obtaining concentrated solution, wherein the vacuum degree is set to be-0.09 MPa and the temperature is 70 ℃ during vacuum concentration;
s4, standing and impurity removal: pouring out the concentrated solution obtained in the step S3 while the concentrated solution is hot, cooling to 2-8 ℃, standing for 8-12 h to obtain layered extract and upper layer solution, wherein the extract is added into 80% food grade alcohol serving as an extraction solvent, and the feed-liquid ratio is 1:5, stirring in a water bath at 70+/-5 ℃ until the mixture is completely dissolved, and carrying out suction filtration through filter paper to obtain filtrate;
s5, shearing inclusion: cooling the filtrate obtained in the step S4 to 55 ℃, adding 1.0% of mono-diglyceride fatty acid ester serving as an emulsifier into the filtrate, stirring for 20-30 min at the constant temperature water bath of 55 ℃ at the rotating speed of 8000r/min, and adding 8% of the emulsifier with the weight ratio of 0.2:2:1 HH-M-beta-CD, HP-beta-CD, continuing homogenizing at 8000r/min for 20-30 min, and coating volatile oil substances in fructus Alpinae Oxyphyllae with the compound to obtain clathrate solution;
s6, vacuum concentration: feeding the inclusion compound solution obtained in the step S5 into a rotary evaporator, vacuum concentrating until the relative density is 1.2, and discharging to obtain a concentrate, wherein the vacuum degree is set to be-0.09 MPa and the temperature is 65 ℃ during vacuum concentration;
s7, drying and crushing: drying the concentrate obtained in the step S6 in a 90 ℃ hot air circulation drying box to paste, transferring the paste into a vacuum drying box, drying the paste for 24-48 hours at 70 ℃ under the vacuum degree of-0.1 MPa, crushing the paste, and sieving the crushed paste with a 80-mesh sieve to obtain the target extract.
The embodiment also provides a fructus alpiniae oxyphyllae extract prepared by the extraction process, the yield is 13.53%, and the nootkatone content in the extract is 0.991% after HPLC detection.
Example 3:
the embodiment provides an extraction process of a fructus alpiniae oxyphyllae extract, which specifically comprises the following steps:
s1, pretreatment of medicinal materials: removing impurities from fructus Alpinae Oxyphyllae, pulverizing with pulverizer, sieving with R40/3 series 1 sieve conforming to national standard ISO 3310-1 or Chinese pharmacopoeia standard to obtain fine powder, wherein the mesh diameter of the sieve is 2000+ -70 μm, and the mesh number is 10 mesh;
weighing 500g of medicinal material fine powder, performing microwave pretreatment on the medicinal material fine powder by adopting a solvent-free microwave method, setting the microwave heating time to be 25-30 min, setting the microwave to be 450W when the microwave heating time is 0-20 min, setting the microwave to be 180W after the microwave heating time exceeds 20min, collecting the extracting solution every 5-10 min, and merging to obtain the extracting solution;
s2, extracting volatile oil components: putting the combined extract obtained in the step S1 into an extraction kettle, and utilizing supercritical CO 2 Extracting and setting CO 2 The flow is 15kg/h, and after extraction, the mixture is introduced into a separating kettle which is cooled to room temperature in a stepped way to obtain extraction liquid; the temperature of the extraction kettle is set to 45 ℃, the pressure of the extraction kettle is set to 15MPa, the extraction time is 0.5-2 h each time, and the extraction times are not less than 2 times; the pressure of the separation kettle is set to be 8MPa, the temperature is reduced stepwise from 30-40 ℃ to room temperature, and the temperature reduction range is 5 ℃/10min;
s3, filtering and concentrating: concentrating the extracting solution obtained in the step S2 in vacuum by a rotary evaporator until no alcohol exists, and obtaining concentrated solution, wherein the vacuum degree is set to be-0.09 MPa and the temperature is 60 ℃ during vacuum concentration;
s4, standing and impurity removal: pouring out the concentrated solution obtained in the step S3 while the concentrated solution is hot, cooling to 2-8 ℃, standing for 8-12 h to obtain layered extract and upper layer solution, wherein the extract is added into 90% food grade alcohol serving as an extraction solvent, and the feed-liquid ratio is 1:3, stirring in a water bath at 70+/-5 ℃ until the mixture is completely dissolved, and carrying out suction filtration through filter paper to obtain filtrate;
s5, shearing inclusion: after the filtrate obtained in the step S4 is cooled to 50 ℃, 0.8 percent of monocarboxymethyl cellulose sodium is added into the filtrate as an emulsifying agent, the mixture is stirred for 20 to 30 minutes at the constant temperature water bath of 50 ℃ at the rotating speed of 9000r/min, and then 8 percent of sodium monocarboxymethyl cellulose with the weight ratio of 0.2 is added: 3:1 HH-M-beta-CD, HP-beta-CD, continuing homogenizing at 9000r/min for 20-30 min, and coating volatile oil substances in fructus Alpinae Oxyphyllae with the compound to obtain clathrate solution;
s6, vacuum concentration: feeding the inclusion compound solution obtained in the step S5 into a rotary evaporator, vacuum concentrating until the relative density is 1.2, and discharging to obtain a concentrate, wherein the vacuum degree is set to be-0.09 MPa and the temperature is 60 ℃ during vacuum concentration;
s7, drying and crushing: drying the concentrate obtained in the step S6 in a hot air circulation drying oven at 80 ℃ until the concentrate is pasty, transferring the concentrate into a vacuum drying oven, drying the concentrate for 24-48 hours at 60 ℃ under the vacuum degree of-0.1 MPa, crushing the concentrate, and sieving the crushed concentrate with a 80-mesh sieve to obtain the target extract.
The embodiment also provides a fructus alpiniae oxyphyllae extract prepared by the extraction process, the yield is 12.86%, and the nootkatone content in the extract is 1.016% after HPLC detection.
Comparative example 1:
the fructus alpiniae oxyphyllae extract is extracted by adopting an extraction process similar to that of the embodiment 1, except that the microwave pretreatment is not adopted in the step S1, the extraction treatment is directly carried out on the obtained medicinal material fine powder, the 80% food grade alcohol is adopted in the step S2 to extract the fine powder obtained in the step S1, and specifically, the fine powder obtained in the step S1 is added into the solution with the ratio of 1: mixing evenly in 80% food grade alcohol of 4-10, extracting to obtain extracting solution, extracting at 80-90 ℃ for 1-3 h, extracting times not less than 2, and the rest steps are the same as those of example 1.
Comparative example 2:
the fructus Alpinae Oxyphyllae extract was extracted by the similar extraction process as in example 1, except that 80% food grade alcohol was used for the extraction of the fine powder obtained in step S1 in step S2, specifically, the fine powder obtained in step S1 was added in a feed-to-liquid ratio of 1: mixing evenly in 80% food grade alcohol of 4-10, extracting to obtain extracting solution, extracting at 80-90 ℃ for 1-3 h, extracting times not less than 2, and the rest steps are the same as those of example 1.
Comparative example 3:
the fructus Alpinae Oxyphyllae extract was extracted by the similar extraction process as in example 1, except that the supercritical CO was used in step S2 2 When the volatile oil components are extracted, the extracted volatile oil components are sequentially introduced into a separately arranged high-temperature and room-temperature separation kettle for separation to obtain extracted liquid, the pressure of the high-temperature and room-temperature separation kettle is set to be 8MPa, the temperature of the high-temperature separation kettle is 40-50 ℃, and the rest steps are consistent with those of the embodiment 1.
The invention adopts SHIMADZU High Performance Liquid Chromatograph (HPLC) to detect the effective component nocardione of the test sample, and can directly, obviously and objectively reflect the quality of the extract. The main analysis reagents adopted in the detection are as follows: nocardomone control (purity: 97%, model number: aladin 159076-1G), acetonitrile (chromatographic grade), phosphoric acid (chromatographic grade), ultrapure water (chromatographic grade), methanol (analytical grade); the detection method comprises the following steps:
preparing a control solution: weighing a proper amount of nocardione reference substance, and adding methanol to prepare a nocardione reference solution with the concentration of 0.02 mg/mL;
preparing a sample solution: weighing a proper amount of test sample, and adding methanol to prepare a sample solution with the concentration of 2 mg/mL;
and calculating by adopting a single-point external standard method according to the peak areas of the sample solution and the reference solution to obtain the content of the sample.
The liquid chromatography conditions are shown in Table 1.
Table 1:
| chromatographic column | C18(4.6×150mm，5μm) |
| Mobile phase | Acetonitrile: water (65:35) |
| Detection wavelength | 235nm |
| Flow rate | 1.0mL/min |
| Column temperature | 30℃ |
| Sample injection amount | 10μL |
By adopting the HPLC detection method, the content detection of the nootkatone in the nootkatone reference substance, the nootkatone raw medicinal materials and the extracts obtained in the examples 1-3 are respectively carried out, the HPLC detection spectrogram of the nootkatone extract provided by the invention is shown in figure 1, the HPLC detection spectrogram of the nootkatone reference substance is shown in figure 2, and the overall detection result is shown in table 2.
Table 2:
through detection, the content of nootkatone in the fructus alpiniae oxyphyllae raw material medicine is 0.133%, so that the content of nootkatone in the fructus alpiniae oxyphyllae extract provided in embodiments 1-3 of the application is at least 7-8 times of that in the fructus alpiniae oxyphyllae raw material medicine, and the content of the effective substances is obviously improved. As can be seen from comparison with comparative examples 1-3, the present application employs microwave pretreatment with SC-CO 2 According to the technical scheme of extraction combination, the extraction solution is subjected to stepped cooling and separation, and the product yield and the content of the effective substance nocardione in the product can be obviously improved.
As can be seen from a comprehensive comparison of the data of examples 1 to 3 in Table 2, the product yield and the nootkatone content obtained by the extraction of example 1 are relatively stable, so that the stability test is carried out on the product obtained by the extraction of example 1 according to the experimental steps and parameters set by the stability test guidelines of 9001 drugs and preparations under the guidance of China pharmacopoeia (2020 edition) (9000 guidelines), and the nootkatone content of the extract obtained in step S4 and the target extract obtained after inclusion in step S7 in the fructus alpiniae oxyphyllae extraction process provided by the example are detected under the conditions of illumination, high temperature and high humidity. In order to shorten the time of the influence factor test and the acceleration test, two conditions of the high temperature test and the high humidity test under the influence factor test item are simultaneously carried out, and two investigation conditions under the acceleration test item are also simultaneously carried out. The results of the detection are shown in tables 3 to 7.
The test results of the fructus alpiniae oxyphyllae extract and the target extract provided in example 1 after the test under the illuminance condition of 4500lx + -500 lx are shown in table 3 according to the experimental steps and parameters set according to the 9001 medicine and preparation stability test guidelines under the "Chinese pharmacopoeia (2020 edition) (9000 guidelines).
Table 3:
| fructus alpiniae oxyphyllae extract | Target extract | |
| Illuminated for 0 day | 2.86±0.01％ | 0.991±0.03％ |
| Illuminating for 5 days | 2.81±0.03％ | 0.992±0.03％ |
| Illuminating for 10 days | 2.82±0.02％ | 0.990±0.02％ |
The test results of the fructus alpiniae oxyphyllae extract and the target extract provided in example 1 after the test are shown in table 4 under the conditions of 60 ℃ and 40 ℃ according to the experimental steps and parameters set by 9001 medicine and preparation stability test guidelines under the item of Chinese pharmacopoeia (2020 edition) (9000 guidelines).
Table 4:
the test results of the fructus alpiniae oxyphyllae extract and the target extract provided in example 1 after the test under the conditions of RH 92.5% and RH 75% high humidity are shown in table 5 according to the experimental steps and parameters set by 9001 medicine and preparation stability test guidelines under the item of Chinese pharmacopoeia (2020 edition) (9000 guidelines).
Table 5:
| fructus alpiniae oxyphyllae extract | Clathrate of object extract | |
| RH 92.5% for 0 days | 2.86±0.01％ | 0.991±0.03％ |
| RH 92.5% for 5 days | 2.85±0.03％ | 0.899±0.03％ |
| RH 92.5%10 days | 2.85±0.05％ | 0.990±0.01％ |
| RH 75% for 0 day | 2.86±0.01％ | 0.991±0.03％ |
| RH 75% for 5 days | 2.81±0.02％ | 0.991±0.02％ |
| RH 75% for 10 days | 2.83±0.03％ | 0.990±0.01％ |
According to the experimental steps and parameters set by 9001 medicine and preparation stability test guidelines under the item of Chinese pharmacopoeia (2020 edition) (9000 guidelines), respectively performing accelerated experiments at 40 ℃ and 30 ℃, and the detection results of the fructus alpiniae oxyphyllae extract and the target extract provided in example 2 after the accelerated experiments are shown in tables 6-7 and figures 3-6.
Table 6 (40 ℃ acceleration experiment):
table 7 (30 ℃ acceleration experiment):
as shown by the acceleration test results, the nocardione content in the extract has a remarkable decreasing trend along with the lengthening of the time, and the decreasing is gradually accelerated along with the lengthening of the time; after inclusion of the HH-beta-CD, HP-beta-CD and beta-CD complexes, the nootkatone component is not obviously reduced under the same conditions and under the same time, so that the volatile oil substances in the fructus alpiniae oxyphyllae are wrapped by the HH-M-beta-CD, HP-beta-CD and beta-CD complexes, and finally the fructus alpiniae oxyphyllae extract in the form of powder is high in stability, convenient to store for a long time and suitable for the combined preparation of various later formulations.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
1. The extraction process of the fructus alpiniae oxyphyllae extract is characterized by comprising the following steps of:
s1, pretreatment of medicinal materials: removing impurities from fructus alpiniae oxyphyllae raw materials, crushing the fructus alpiniae oxyphyllae raw materials by a crusher, sieving the crushed raw materials to obtain medicinal fine powder, carrying out microwave pretreatment on the obtained medicinal fine powder by a solvent-free microwave method, wherein the heating time of the microwave pretreatment is set to be 25-30 min, the microwave is set to be 300-450W when the heating time is 0-20 min, the microwave is set to be 180-280W when the heating time exceeds 20min, and extracting solutions are collected once every 5-10 min, and the extracting solutions are obtained after the mixing;
s2, extracting volatile oil components: then the combined extracting solution obtained in the step S1 is put into an extraction kettle, and supercritical CO is utilized 2 Extracting，CO 2 The flow is 8-15 kg/h, after extraction, the liquid is fed into a separating kettle which is cooled to room temperature in a stepped way for separation to obtain extraction liquid, the extraction time is 0.5-2 h each time, and the extraction times are not less than 2 times;
s3, filtering and concentrating: filtering the extracting solution obtained in the step S2 to obtain filtrate, and concentrating the filtrate in vacuum to obtain concentrated solution;
s4, standing and impurity removal: standing the concentrated solution obtained in the step S3 for 8-12 h at low temperature to obtain layered extract and upper solution, discarding a liquid part, adding the extract into an extraction solvent, stirring in a water bath at 50-80 ℃ until the extract is completely dissolved, and carrying out suction filtration through filter paper to obtain filtrate;
s5, shearing inclusion: adding 0.5-1.0% of emulsifying agent into the filtrate obtained in the step S4, stirring at 8000-10000 r/min for 20-30 min at the temperature of 40-60 ℃ in water bath, adding 5-10% of compound, and continuously homogenizing at 8000-10000 r/min for 20-30 min to obtain a uniformly mixed inclusion compound solution;
s6, vacuum concentration: feeding the inclusion compound solution obtained in the step S5 into a rotary evaporator, concentrating in vacuum until the relative density is 1.1-1.3, and discharging to obtain a concentrate;
s7, drying and crushing: drying the concentrate obtained in the step S6 in a hot air circulation drying box at 60-90 ℃ until the concentrate is pasty, transferring the concentrate into a vacuum drying box, drying the concentrate for 24-48 hours at 60-70 ℃ and-0.1 MPa, crushing the concentrate, and sieving the crushed concentrate with a 80-mesh sieve to obtain the target extract.
2. The process according to claim 1, wherein in step S1, the mesh diameter of the medicine sieve used for sieving is 2000±70 μm and the mesh number is 10.
3. The process according to claim 1, wherein in step S2, the temperature of the extraction vessel is set to 35-50 ℃ and the pressure of the extraction vessel is set to 10-18 MPa.
4. The process according to claim 1, wherein in step S2, the temperature of the separation tank is lowered stepwise from 30 to 50 ℃ to room temperature with a temperature lowering range of 5 ℃/10min, and the pressure of the separation tank is set to 6 to 10MPa.
5. The process according to claim 1, wherein in steps S3 and S6, the vacuum concentration is carried out at a vacuum of-0.09 MPa and a temperature of 50 to 70 ℃.
6. The process according to claim 1, wherein in step S4, the extraction solvent is selected from 60-90% food grade alcohol, and the ratio of extract to extraction solvent is 1:2 to 5.
7. The process according to claim 1, wherein in step S5, the emulsifier is at least one selected from the group consisting of mono-di-glycerol fatty acid ester, sodium starch octenyl succinate, and sodium carboxymethyl cellulose.
8. The process according to claim 1, wherein in step S5, the compound is a mixture of HH- β -CD, HP- β -CD, wherein the weight ratio of HH- β -CD, HP- β -CD, β -CD is 0.1-0.5: 0.5 to 3:1.
9. the process for extracting alpinia oxyphylla extract according to claim 8, wherein the HH- β -CD is selected from any one of HH-TM- β -CD, HH-HP- β -CD, HH-M- β -CD, HH-DM- β -CD.
10. A fructus alpiniae oxyphyllae extract, which is prepared by the extraction process according to any one of claims 1 to 9.
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Citations (4)
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| CN104382973A (en) * | 2014-10-30 | 2015-03-04 | 广州医科大学附属第一医院 | Total volatile oil extractive of asarum, extraction method of total volatile oil extractive as well as application of total volatile oil extractive in preparation of drugs for treating chronic coughs |
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