CN116077570A - Preparation method of pollen typhae extract - Google Patents
Preparation method of pollen typhae extract Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- 239000000843 powder Substances 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 238000001914 filtration Methods 0.000 claims abstract description 25
- 239000006228 supernatant Substances 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229920005989 resin Polymers 0.000 claims abstract description 11
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- 238000000034 method Methods 0.000 claims description 18
- 240000001398 Typha domingensis Species 0.000 claims description 15
- 238000005292 vacuum distillation Methods 0.000 claims description 15
- 238000000926 separation method Methods 0.000 claims description 10
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- 238000003756 stirring Methods 0.000 claims description 7
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- 238000001179 sorption measurement Methods 0.000 claims description 6
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- 239000011148 porous material Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract 1
- 238000001694 spray drying Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
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- QHLKSZBFIJJREC-SPSUIZEHSA-N Isorhamnetin-3-O-nehesperidine Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)=C1 QHLKSZBFIJJREC-SPSUIZEHSA-N 0.000 description 1
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- POMAQDQEVHXLGT-QDYYQVSOSA-N Typhaneoside Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]3[C@@H]([C@H](O)[C@@H](O)[C@H](C)O3)O)O2)O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)=C1 POMAQDQEVHXLGT-QDYYQVSOSA-N 0.000 description 1
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- 230000003993 interaction Effects 0.000 description 1
- POMAQDQEVHXLGT-UHFFFAOYSA-N isorhamnetin 3-(2-rhamnosyl rutinoside) Natural products C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)OC2C(C(O)C(O)C(COC3C(C(O)C(O)C(C)O3)O)O2)OC2C(C(O)C(O)C(C)O2)O)=C1 POMAQDQEVHXLGT-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- FRBRLXJEQSHWAA-UHFFFAOYSA-N typhaneoside Natural products COc1cc(ccc1O)C2=C(OC3OC(COC4OC(C)C(O)C(O)C4OC5OC(C)C(O)C(O)C5O)C(O)C(O)C3O)C(=O)c6c(O)cc(O)cc6O2 FRBRLXJEQSHWAA-UHFFFAOYSA-N 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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)
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- A—HUMAN NECESSITIES
- 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
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- A—HUMAN NECESSITIES
- 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A—HUMAN NECESSITIES
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- A—HUMAN NECESSITIES
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
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Abstract
The invention discloses a preparation method of a pollen typhae extract, which comprises the steps of preparing dry pollen typhae powder by low-temperature drying and mixing the dry pollen typhae powder 8:1, adding aqueous ethanol in proportion, heating and concentrating until the total liquid amount is reduced by 40%, then centrifugally separating to obtain supernatant, filtering and filtering to remove solid matters, then adsorbing by macroporous resin and eluting by aqueous lower alcohol, concentrating eluent to a certain volume, precipitating by ethanol, removing water by using a semipermeable membrane, finally concentrating by reduced pressure and heating until the ethanol is dried or removed, and then spray-drying to obtain the pollen typhae extract.
Description
Technical Field
The invention relates to the field of Chinese patent medicine processing, in particular to a preparation method of a cattail pollen extract.
Background
Pollen Typhae is common medicinal material, and is derived from pollen of multiple plants such as Typhaceae Typhaea L, vaccinium bracteatum Typha angustifolia L, typhagus bracteatum Typha angustata Bory et Chaub, and Typhagus latifolia L. Aliases pollen Typhae, etc. Its medicinal history is long, and the Han dynasty's Shen nong Ben Cao Jing' is listed as the top grade. Has hemostatic, blood stasis dispelling, and stranguria treating effects. Can be used for treating hematemesis, epistaxis, hemoptysis, metrorrhagia, traumatic hemorrhage, amenorrhea, abdominal pain, traumatic injury, swelling and pain, and stranguria. The description of Ben Cao gang mu: the blood-separating herbs of Pu Huang and Jueyin of hand and foot also can treat pain caused by blood, while the raw one can treat pain caused by blood, while the cooked one can stop, so it can be combined with Wu Ling Zhi to treat all kinds of pain of heart and abdomen. The symptoms of chest and spleen and eucardialgia described by traditional Chinese medicine are similar to those of coronary heart disease and angina pectoris, and clinical reports show that the smiling powder mainly composed of cattail pollen and trogopterus dung has a certain curative effect on coronary heart disease. Pollen Typhae mainly contains steroid, flavonoid, long chain aliphatic hydrocarbon compound, amino acids, inorganic component, etc.
Based on the requirements of industrialization and standardization of modern traditional Chinese medicine, the administration forms of traditional medicinal decoction and paste cannot be met, the development direction is to develop a processing preparation method capable of realizing high-efficiency extraction for the cattail pollen raw material, wherein the development direction is to develop western medicine forms such as tablets, capsules and medicinal granules, and the like, so that mass standard production can be met, and high-efficiency automatic production can be realized.
Disclosure of Invention
The invention aims to: the invention aims at overcoming the defects of the prior art and provides a preparation method of a cattail pollen extract.
The technical scheme is as follows: the preparation method of the cattail pollen extract comprises the following steps:
s1, placing the crude pollen typhae powder into a low-temperature drying box, drying the crude pollen typhae powder with 30% of relative humidity, controlling the drying temperature to be between 45 and 60 ℃ and continuously lifting at a speed of 1 ℃/1min and continuously executing for 60min, then taking out the dried crude pollen typhae powder, placing the dried crude pollen typhae powder into a to-be-treated end of a vibrating screen, and treating the dried crude pollen typhae powder by the vibrating screen to obtain dried pollen typhae powder;
s2, placing the dried pollen typhae powder into a container, and placing the dried pollen typhae powder and the dried pollen typhae powder 8 in the container: 1, then placing a container loaded with dry pollen typhae powder and the aqueous ethanol on a heating magnetic stirrer, continuously stirring, heating and concentrating until the total volume is reduced to 60% of the total volume before heating;
s3, taking out the mixture obtained in the step S2 after heating and concentrating, then carrying out centrifugal separation, and taking supernatant liquid after the centrifugal separation for later use;
s4, configuring a filtering mechanism, arranging a filtering container, installing a filter paper layer in the container, pouring supernatant into the filtering container, and further filtering out solids to obtain low-concentration extract supernatant;
s5, adsorbing the low-concentration extract clear liquid with macroporous resin, eluting with water to remove impurities, eluting with aqueous lower alcohol, concentrating the eluent to a certain volume, precipitating with ethanol, and filtering again to remove precipitate to obtain an extract solution;
s6, performing semipermeable membrane exudation operation on the extract solution, and pressurizing one side of the extract solution when the semipermeable membrane exudation is performed until the moisture in the extract solution is completely exuded, so as to obtain the extract solution;
s7, decompressing, heating and concentrating the extract solution to dryness to obtain the pollen typhae extract.
Preferably, the low concentration extract supernatant side is pressurized to 1.3MPa during the pressurizing in S6 until the moisture in the low concentration extract supernatant is completely exuded.
Preferably, in S7, the extract solution is placed in a vacuum distillation bin, the vacuum distillation bin is depressurized to a vacuum degree of-0.737 MPa, and the vacuum distillation bin is heated to 48.3-55.8 ℃ as a whole until the ethanol and the lower alcohol in the extract solution are completely evaporated and discharged.
Preferably, the filter paper layer used in S4 has a pore size of 15 microns.
Preferably, the macroporous resin is a polystyrene type porous adsorption resin.
Preferably, the lower alcohol includes a C2-C3 lower alcohol.
Preferably, the concentration of the aqueous lower alcohol is 52%.
Preferably, the final concentration of ethanol precipitated with ethanol in S5 is 95%.
Preferably, the temperature at which stirring and heat concentration are continued in S2 is 80 ℃.
Compared with the prior art, the invention has the following beneficial effects: (1) The two purification processes of extraction filtration, macroporous resin adsorption, aqueous lower alcohol elution and alcohol precipitation are adopted, so that impurities in the finished pollen typhae extract product can be sufficiently removed, and the purity is extremely high;
(2) The temperature of the heating environment in the whole treatment process is controlled below 80 ℃, and the heating temperature is further controlled by reducing pressure and heating when the cattail pollen is finally concentrated to be dry, so that the temperature of the whole mixture is prevented from being too high in the final stage of concentrating to be dry, and the inactivation of active ingredients in the cattail pollen extract caused by high-temperature heating is effectively avoided;
(3) The solid matters in the whole set of treatment process are all wastes to be discharged, and the effective materials to be reserved in the material transferring process are all liquid-phase materials, so that the automatic transferring stage of the materials can be realized through a liquid-phase single-phase pipeline in the process of adapting to the automatic pipeline production, thereby being capable of completely adapting to the automatic pipeline production and meeting the requirements of the modern traditional Chinese medicine industry on batch standard production and high-efficiency automatic production.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments 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.
In the description of the present invention, it should be understood that the terms "center," "longitudinal," "transverse," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "axial," "radial," "circumferential," and the like indicate directional or positional relationships for convenience in describing the invention and simplifying the description, and do not indicate or imply that the devices or elements in question must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention.
In the present invention, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; the device can be mechanically connected, electrically connected and communicated; either directly, or indirectly, through intermediaries, may be in communication with each other, or may be in interaction with each other, unless explicitly defined otherwise. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The technical scheme of the invention is described in detail below by specific examples. The following embodiments may be combined with each other, and some embodiments may not be repeated for the same or similar concepts or processes.
Example 1: a preparation method of pollen Typhae extract comprises the following steps:
s1, placing the crude pollen typhae powder into a low-temperature drying box, drying the crude pollen typhae powder with 30% of relative humidity, controlling the drying temperature to be between 45 and 60 ℃ and continuously lifting at a speed of 1 ℃/1min and continuously executing for 60min, then taking out the dried crude pollen typhae powder, placing the dried crude pollen typhae powder into a to-be-treated end of a vibrating screen, and treating the dried crude pollen typhae powder by the vibrating screen to obtain dried pollen typhae powder;
s2, placing the dried pollen typhae powder into a container, and placing the dried pollen typhae powder and the dried pollen typhae powder 8 in the container: 1, then placing a container loaded with dry pollen typhae powder and the aqueous ethanol on a heating magnetic stirrer, continuously stirring and heating to 80 ℃ and concentrating until the total volume is reduced to 60% of the total volume before heating;
s3, taking out the mixture obtained in the step S2 after heating and concentrating, then carrying out centrifugal separation, and taking supernatant liquid after the centrifugal separation for later use;
s4, configuring a filtering mechanism, arranging a filtering container, arranging a filter paper layer in the container, wherein the aperture of the filter paper layer is 15 microns, pouring the supernatant into the filtering container to further filter solids, and obtaining low-concentration extract supernatant;
s5, adsorbing the low-concentration extract clear liquid by using polystyrene porous adsorption resin, eluting with water to remove impurities, eluting with aqueous lower alcohol, wherein the concentration of the aqueous lower alcohol is 52%, the lower alcohol comprises lower alcohols with C2-C3, concentrating the eluent to a certain volume, precipitating with ethanol to obtain an ethanol final concentration of 95%, and filtering again to remove precipitate to obtain an extract solution;
s6, performing semipermeable membrane exudation operation on the extract solution, and pressurizing one side of the extract solution when the semipermeable membrane exudation is performed, wherein the pressure on one side of the extract solution is 1.3MPa when the pressure is performed until the water in the low-concentration extract solution is completely exuded;
s7, placing the extract solution into a vacuum distillation bin, decompressing the vacuum distillation bin to the vacuum degree of-0.737 MPa, and simultaneously heating the whole vacuum distillation bin to 48.3-55.8 ℃ until the ethanol and lower alcohol in the extract solution are completely evaporated and discharged to obtain the cattail pollen extract.
Example 2: a preparation method of pollen Typhae extract comprises the following steps:
s1, placing the crude pollen typhae powder into a low-temperature drying box, drying the crude pollen typhae powder with 30% of relative humidity, controlling the drying temperature to be between 45 and 60 ℃ and continuously lifting at a speed of 1 ℃/1min and continuously executing for 60min, then taking out the dried crude pollen typhae powder, placing the dried crude pollen typhae powder into a to-be-treated end of a vibrating screen, and treating the dried crude pollen typhae powder by the vibrating screen to obtain dried pollen typhae powder;
s2, placing the dried pollen typhae powder into a container, and placing the dried pollen typhae powder and the dried pollen typhae powder 8 in the container: 1, then placing a container loaded with dry pollen typhae powder and the aqueous ethanol on a heating magnetic stirrer, continuously stirring and heating to 80 ℃ and concentrating until the total volume is reduced to 60% of the total volume before heating;
s3, taking out the mixture obtained in the step S2 after heating and concentrating, then carrying out centrifugal separation, and taking supernatant liquid after the centrifugal separation for later use;
s4, configuring a filtering mechanism, arranging a filtering container, arranging a filter paper layer in the container, wherein the aperture of the filter paper layer is 15 microns, pouring the supernatant into the filtering container to further filter solids, and obtaining low-concentration extract supernatant;
s5, performing semipermeable membrane exudation operation on the low-concentration extract clear liquid, and pressurizing one side of the low-concentration extract clear liquid when the semipermeable membrane exudation is performed, wherein the pressure is 1.3MPa on one side of the low-concentration extract clear liquid until the water in the low-concentration extract clear liquid is completely exuded;
s7, placing the extract solution into a vacuum distillation bin, decompressing the vacuum distillation bin to the vacuum degree of-0.737 MPa, and simultaneously heating the whole vacuum distillation bin to 48.3-55.8 ℃ until the ethanol and lower alcohol in the extract solution are completely evaporated and discharged to obtain the cattail pollen extract.
Example 3: a preparation method of pollen Typhae extract comprises the following steps:
s1, placing the crude pollen typhae powder into a low-temperature drying box, drying the crude pollen typhae powder with 30% of relative humidity, controlling the drying temperature to be between 45 and 60 ℃ and continuously lifting at a speed of 1 ℃/1min and continuously executing for 60min, then taking out the dried crude pollen typhae powder, placing the dried crude pollen typhae powder into a to-be-treated end of a vibrating screen, and treating the dried crude pollen typhae powder by the vibrating screen to obtain dried pollen typhae powder;
s2, placing the dried pollen typhae powder into a container, and placing the dried pollen typhae powder and the dried pollen typhae powder 8 in the container: 1, then placing a container loaded with dry pollen typhae powder and the aqueous ethanol on a heating magnetic stirrer, continuously stirring and heating to 80 ℃ and concentrating until the total volume is reduced to 60% of the total volume before heating;
s3, taking out the mixture obtained in the step S2 after heating and concentrating, then carrying out centrifugal separation, and taking supernatant liquid after the centrifugal separation for later use;
s4, configuring a filtering mechanism, arranging a filtering container, arranging a filter paper layer in the container, wherein the aperture of the filter paper layer is 15 microns, pouring the supernatant into the filtering container to further filter solids, and obtaining low-concentration extract supernatant;
s5, adsorbing the low-concentration extract clear liquid by using polystyrene porous adsorption resin, eluting with water to remove impurities, eluting with aqueous lower alcohol, wherein the concentration of the aqueous lower alcohol is 52%, the lower alcohol comprises lower alcohols with C2-C3, concentrating the eluent to a certain volume, precipitating with ethanol to obtain an ethanol final concentration of 95%, and filtering again to remove precipitate to obtain an extract solution;
s6, placing the extract solution into a vacuum distillation bin, decompressing the vacuum distillation bin to the vacuum degree of-0.737 MPa, and simultaneously heating the whole vacuum distillation bin to 48.3-55.8 ℃ until the ethanol and lower alcohol in the extract solution are completely evaporated and discharged to obtain the cattail pollen extract.
The purity of the pollen Typhae extract could not be judged by the content of a single compound because the pollen Typhae extract is not a single compound but the sum of various effective chemical components contained in the raw materials of the pollen Typhae, but the main effective components in the pollen Typhae are flavonoid components represented by isorhamnetin-3-O-beta-D-galactoside, isorhamnetin-3-O-neohesperidin, typha neoside and the like, as can be seen from pharmacology, the purity of the pollen Typhae extract can be judged by using the total flavonoid content as a basis for judgment and adopting an ultraviolet spectrophotometry, and the total flavonoid content of examples 1, 2 and 3 is shown in the following table.
| Example 1 | Example 2 | Example 3 | |
| Total flavone content (%) | 56.1 | 50.2 | 51.9 |
As can be seen from the above table, the pollen Typhae extract prepared in example 1 had the highest purity.
In conclusion, the technical scheme provided by the invention has the advantages that two purification processes of extraction filtration, macroporous resin adsorption, water-containing lower alcohol elution and alcohol precipitation are adopted, so that impurities in a finished pollen typhae extract product can be sufficiently removed, and the purity is extremely high; the temperature of the heating environment in the whole treatment process is controlled below 80 ℃, and the heating temperature is further controlled by reducing pressure and heating when the cattail pollen is finally concentrated to be dry, so that the temperature of the whole mixture is prevented from being too high in the final stage of concentrating to be dry, and the inactivation of active ingredients in the cattail pollen extract caused by high-temperature heating is effectively avoided; the solid matters in the whole set of treatment process are all wastes to be discharged, and the effective materials to be reserved in the material transferring process are all liquid-phase materials, so that the automatic transferring stage of the materials can be realized through a liquid-phase single-phase pipeline in the process of adapting to the automatic pipeline production, thereby being capable of completely adapting to the automatic pipeline production and meeting the requirements of the modern traditional Chinese medicine industry on batch standard production and high-efficiency automatic production.
In the present invention, unless expressly stated or limited otherwise, a first feature "up" or "down" a second feature may be a direct contact between the first feature and the second feature, or an indirect contact between the first feature and the second feature through an intervening medium. Moreover, a first feature "above," "over" and "on" a second feature may be a first feature directly above or obliquely above the second feature, or simply indicate that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature may be the first feature being directly under or obliquely below the second feature, or simply indicating that the first feature is at a lower level than the second feature. In the description of the present specification, reference to the description of the terms "one embodiment," "some embodiments," "examples," "particular examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, schematic representations of the above terms are not necessarily directed to the same embodiment or example.
Furthermore, the particular features, structures, materials, or characteristics may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, the different embodiments or examples described in this specification and the features of the different embodiments or examples may be combined and combined by those skilled in the art without contradiction.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features can be replaced equivalently; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. A preparation method of a cattail pollen extract is characterized in that: the method comprises the following steps:
s1, placing the crude pollen typhae powder into a low-temperature drying box, drying the crude pollen typhae powder with 30% of relative humidity, controlling the drying temperature to be between 45 and 60 ℃ and continuously lifting at a speed of 1 ℃/1min and continuously executing for 60min, then taking out the dried crude pollen typhae powder, placing the dried crude pollen typhae powder into a to-be-treated end of a vibrating screen, and treating the dried crude pollen typhae powder by the vibrating screen to obtain dried pollen typhae powder;
s2, placing the dried pollen typhae powder into a container, and placing the dried pollen typhae powder and the dried pollen typhae powder 8 in the container: 1, then placing a container loaded with dry pollen typhae powder and the aqueous ethanol on a heating magnetic stirrer, continuously stirring, heating and concentrating until the total volume is reduced to 60% of the total volume before heating;
s3, taking out the mixture obtained in the step S2 after heating and concentrating, then carrying out centrifugal separation, and taking supernatant liquid after the centrifugal separation for later use;
s4, configuring a filtering mechanism, arranging a filtering container, installing a filter paper layer in the container, pouring supernatant into the filtering container, and further filtering out solids to obtain low-concentration extract supernatant;
s5, adsorbing the low-concentration extract clear liquid with macroporous resin, eluting with water to remove impurities, eluting with aqueous lower alcohol, concentrating the eluent to a certain volume, precipitating with ethanol, and filtering again to remove precipitate to obtain an extract solution;
s6, performing semipermeable membrane exudation operation on the extract solution, and pressurizing one side of the extract solution when the semipermeable membrane exudation is performed until the moisture in the extract solution is completely exuded, so as to obtain the extract solution;
s7, decompressing, heating and concentrating the extract solution to dryness to obtain the pollen typhae extract.
2. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: in the step S6, the pressure is applied to the side of the low-concentration extract supernatant to 1.3MPa until the water in the low-concentration extract supernatant is completely exuded.
3. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: and S7, placing the extract solution into a vacuum distillation bin, decompressing the vacuum distillation bin to the vacuum degree of-0.737 MPa, and simultaneously heating the whole vacuum distillation bin to 48.3-55.8 ℃ until the ethanol and the lower alcohol in the extract solution are completely evaporated and discharged.
4. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: the pore size of the filter paper layer used in S4 was 15 microns.
5. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: the macroporous resin is polystyrene type porous adsorption resin.
6. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: the lower alcohol includes a C2-C3 lower alcohol.
7. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: the concentration of the aqueous lower alcohol was 52%.
8. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: the final concentration of ethanol precipitated with ethanol in S5 was 95%.
9. The method for preparing the pollen typhae extract according to claim 1, which is characterized in that: the temperature at which stirring and heat concentration were continued in S2 was 80 ℃.
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| CN1434042A (en) * | 2003-02-25 | 2003-08-06 | 中国人民解放军第二军医大学 | Cattail pollen extract and preparation process and use thereof |
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| CN110538247A (en) * | 2018-05-29 | 2019-12-06 | 南京泽朗生物科技有限公司 | a method for extracting total flavone from pollen Typhae |
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| CN1434042A (en) * | 2003-02-25 | 2003-08-06 | 中国人民解放军第二军医大学 | Cattail pollen extract and preparation process and use thereof |
| CN108095117A (en) * | 2018-01-02 | 2018-06-01 | 广州泽力医药科技有限公司 | Gadol extract and its extracting method and application |
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