CN110101666A - The production method that a kind of low ash divides Horsetail P.E - Google Patents

The production method that a kind of low ash divides Horsetail P.E Download PDF

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Publication number
CN110101666A
CN110101666A CN201910427622.5A CN201910427622A CN110101666A CN 110101666 A CN110101666 A CN 110101666A CN 201910427622 A CN201910427622 A CN 201910427622A CN 110101666 A CN110101666 A CN 110101666A
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horsetail
production method
divides
low ash
ash according
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刘星勋
王志
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Hunan Huakang Biological Polytron Technologies Inc
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Hunan Huakang Biological Polytron Technologies Inc
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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
    • A61K36/11—Pteridophyta or Filicophyta (ferns)
    • 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
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • 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
    • A61K47/30—Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36—Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/38—Cellulose; Derivatives thereof
    • 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
    • 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
    • A61K9/19—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles lyophilised, i.e. freeze-dried, solutions or dispersions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P33/00—Antiparasitic agents
    • A61P33/14—Ectoparasiticides, e.g. scabicides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P7/00—Drugs for disorders of the blood or the extracellular fluid
    • A61P7/10—Antioedematous agents; Diuretics
    • 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
    • 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
    • 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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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Medicinal Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Engineering & Computer Science (AREA)
  • Epidemiology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • General Chemical & Material Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Botany (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Tropical Medicine & Parasitology (AREA)
  • Medical Informatics (AREA)
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  • Mycology (AREA)
  • Diabetes (AREA)
  • Hematology (AREA)
  • Medicines Containing Plant Substances (AREA)
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Abstract

The present invention provides the production method that a kind of low ash divides Horsetail P.E, includes the following steps: S1, stock: raw material is shredded or be ground into broken section, is crushed, sieving；S2, alcohol extracting: it is extracted with ethanol water secondary；S3, concentration: vacuum concentration, after recycling ethyl alcohol, concentrate specific gravity is 1.05 ~ 1.1；S4, sedimentation: Ca (OH) is added in concentrate2Aqueous solution places precipitating after stirring evenly, and takes supernatant liquid filtering；S5, ingredient: auxiliary material dry after mixing, crushing, sieving, packaging, storage are added into filtrate.Production method provided by the invention promotes the purity of Horsetail P.E, improves the utilization rate and nutritive value of meadow pine.

Description

The production method that a kind of low ash divides Horsetail P.E
Technical field
The present invention relates to plant extracts technical fields, and in particular to the production method that a kind of low ash divides Horsetail P.E.
Background technique
Meadow pine also known as Drilgrass, Sambucus thunbergiana, hollow grass etc. are Equisetaceae Equisetum herbaceos perennial, bitter, property It is cool, distributed in lung channel, stomach meridian, Liver Channel." Shaanxi Chinese herbal medicine " is recorded: " reducing fever and causing diuresis is stopped blooding, detumescence.Urinary tract infections is controlled, urine is puckery Bitterly, it fractures, nosebleed epistaxis, hemoptysis, enterorrhagia, menorrhalgia." there are the health-care effects such as clearing heat and cooling blood, removing toxic substances diuresis.
CN200810101676.4 discloses a kind of Horsetail P.E and its new application, and the mite killing of open Horsetail P.E is used On the way；CN201811047333.4 discloses a kind of brewage process of meadow pine sanchi leaf wine, and wine body color stability, the mouthfeel of preparation are continuous It is soft, have the effect of clearing heat and cooling blood, removing toxic substances diuresis.
Summary of the invention
The present invention provides the production method that a kind of low ash divides Horsetail P.E, promotes the purity of Horsetail P.E, raising is asked The utilization rate and nutritive value of chaste tree.
To achieve the above object, the invention provides the following technical scheme:
On the one hand, the present invention provides the production method that a kind of low ash divides Horsetail P.E, includes the following steps:
S1, stock: shredding or be ground into broken section for raw material, crush, sieving；
S2, alcohol extracting: it is extracted with ethanol water secondary；
S3, concentration: vacuum concentration, after recycling ethyl alcohol, concentrate specific gravity is 1.05 ~ 1.1；
S4, sedimentation: Ca (OH) is added in concentrate2Aqueous solution places precipitating after stirring evenly, and takes supernatant liquid filtering；
S5, ingredient: auxiliary material dry after mixing, crushing, sieving, packaging, storage are added into filtrate.
Further, in S1, the sieving referred to 10 ~ 40 meshes；Preferably 20 meshes.
Further, the concentration of the ethanol water is 40 ~ 80%.Further, the ethanol water and raw material Proportion is 4-8ml/1g.
Further, in S2, the temperature of the extraction is 70~90 DEG C, extraction time is respectively 2h.
Further, the vacuum degree of the vacuum concentration is -0.05MPa~0.088MPa；Thickening temperature: 65 DEG C of <.
Further, the Ca (OH)2Aqueous solution is saturation Ca (OH)2Aqueous solution.
Further, the Ca (OH)2The dosage of aqueous solution is 0.1 ~ 0.5 times, preferably 0.3 times of concentrate volume.
Further, in S4, the time of the precipitating is 12 ~ 36h.
Further, the auxiliary material is maltodextrin, beta-cyclodextrin, starch, carboxymethyl cellulose etc.；The auxiliary material adds Adding ratio is about the 1 ~ 10% of the weight of final products.
Further, the drying is spray drying or freeze-drying.
Further, the condition of the spray drying is inlet air temperature 160~200 DEG C, leaving air temp 90~100℃； The condition of the freeze-drying be vacuum degree be -0.07MPa~-0.088MPa, < -10 DEG C of temperature.
Beneficial effect
Compared with prior art, the present invention having the following beneficial effects:
The present invention provides the production method that a kind of low ash divides Horsetail P.E, passes through stock, alcohol extracting, concentration, sedimentation and ingredient etc. Step is made, during this, strict control parameter, for example (,) it is extraction time, Extraction solvent amount, Extracting temperature, extraction time, dense Contracting temperature, drying temperature etc. avoid certain components in extract from being destroyed；By adding calcium hydroxide solution, by concentrate In the species precipitates such as impurity, reduce the ash content in extract；By stirring and evenly mixing, accelerate flocculated formation；It is heavy by placing It forms sediment, can make to precipitate automatic decline, be conducive to subsequent filter；By adding auxiliary material in filtrate, stored conducive to the stability of extract, By being freeze-dried or being spray-dried, drying temperature is controlled, avoids component by high temperature；Production side provided by the present invention Method, can significantly improve the quality of Horsetail P.E, bring economic benefit to company；The medical value of Horsetail P.E is improved, It avoids the wasting of resources and causes environmental pollution.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail, but should not be interpreted as this, this hair The bright subject area is only limitted to following embodiment.
The process equipment or device not indicated specifically in the following example are all made of conventional equipment or device in the art； All reagents may be from commercially available.
Embodiment 1:
The production method that a kind of low ash divides Horsetail P.E, includes the following steps:
S1, stock: 50g raw material is shredded or is ground into broken section, crushed 10-40 mesh；
S2, alcohol extracting: secondary, Extracting temperature 70 is extracted with the ethanol water 200-400ml of 40-80%~90 DEG C, extraction time Respectively 2h, 2h；
S3, concentration: (vacuum degree is -0.05MPa~0.088MPa to vacuum concentration.Thickening temperature: 65 DEG C of <；), after recycling ethyl alcohol, Concentrate specific gravity is 1.05-1.1；
S4, sedimentation: the Ca (OH) of 0.1 times of concentrate volume is added in concentrate2Aqueous solution, stir evenly after place precipitating 12h ~ 36h takes supernatant liquid filtering；General flavone content is 4.46%
S5, ingredient: into filtrate be added maltodextrin (about the 10% of final products weight) after mixing spray drying (into Air temperature 160~200 DEG C, leaving air temp 90~100 DEG C), crush, cross 80 ~ 200 meshes, packaging, storage.
Ash content in extract obtained is substantially reduced, and ash content is about the 4.2% of total weight, and general flavone content is about total weight 4.5%, the recovery rate of general flavone is 95.6%.
Embodiment 2:
The production method that a kind of low ash divides Horsetail P.E, includes the following steps:
S1, stock: 100g raw material is shredded or is ground into broken section, crushed 10-40 mesh；
S2, alcohol extracting: secondary, Extracting temperature 70 is extracted with the ethanol water 100ml of 40-80%~90 DEG C, extraction time difference For 2h, 2h；
S3, concentration: (vacuum degree is -0.05MPa~0.088MPa to vacuum concentration；Thickening temperature: 65 DEG C of <；), after recycling ethyl alcohol, Concentrate specific gravity is 1.05-1.1；
S4, sedimentation: the Ca (OH) of 0.3 times of concentrate volume is added in concentrate2Aqueous solution places precipitating for 24 hours after stirring evenly, and takes Supernatant liquid filtering；General flavone content is 5.65%
S5, ingredient: maltodextrin (about the 10% of final products total weight) is added into filtrate and is spray-dried after mixing (inlet air temperature 160~200 DEG C, leaving air temp 90~100 DEG C) or freeze-drying (vacuum degree is -0.07MPa~-0.088MPa, < -10 DEG C of temperature), crush, cross 80 ~ 200 meshes, packaging, storage.
Ash content in extract obtained is substantially reduced, and ash content is about the 3.2% of total weight, and general flavone content is about total weight 5.7%, the recovery rate of general flavone is 95.8%.
Embodiment 3:
The production method that a kind of low ash divides Horsetail P.E, includes the following steps:
S1, stock: 200g raw material is shredded or is ground into broken section, crushed 10-40 mesh；
S2, alcohol extracting: secondary, Extracting temperature 70 is extracted with the ethanol water 200ml of 40-80%~90 DEG C, extraction time difference For 2h, 2h；
S3, concentration: (vacuum degree is -0.05MPa~0.088MPa to vacuum concentration.Thickening temperature: 65 DEG C of <；), after recycling ethyl alcohol, Concentrate specific gravity is 1.05-1.1；
S4, sedimentation: the Ca (OH) of 0.5 times of concentrate volume is added in concentrate2Aqueous solution places precipitating for 24 hours after stirring evenly, and takes Supernatant liquid filtering, general flavone content 5.89%；
S5, ingredient: maltodextrin (about the 10% of final products total weight) is added into filtrate and is freeze-dried after mixing (vacuum degree is -0.07MPa~-0.088MPa, < -10 DEG C of temperature) crushes, crosses 80 ~ 200 meshes, packaging, storage.
Ash content in the extract is substantially reduced, and ash content is about the 2.6% of total weight, and general flavone content is about total weight 6.3%, the recovery rate of general flavone is 96.2%.
It is understood that the principle that embodiment of above is intended to be merely illustrative of the present and the exemplary implementation that uses Mode, however the present invention is not limited thereto.For those skilled in the art, essence of the invention is not being departed from Mind and essence in the case where, various changes and modifications can be made therein, these variations and modifications be also considered as be comprised in it is of the invention In protection scope.

Claims (10)

1. the production method that a kind of low ash divides Horsetail P.E, which comprises the steps of:
S1, stock: raw material is chopped into broken section, or is ground into coarse powder；
S2, alcohol extracting: it is extracted with ethanol water secondary；
S3, concentration: vacuum concentration, after recycling ethyl alcohol, concentrate specific gravity is 1.05 ~ 1.1；
S4, sedimentation: Ca (OH) is added in concentrate2Aqueous solution places precipitating after stirring evenly, and takes supernatant liquid filtering；
S5, ingredient: auxiliary material dry after mixing, crushing, sieving, packaging, storage are added into filtrate.
2. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that in S1, the sieving Referred to 10 ~ 40 meshes.
3. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that the ethanol water Concentration be 40 ~ 80%；The proportion of the ethanol water and raw material is 4-8ml/1g.
4. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that in S2, the extraction Temperature be 70~90 DEG C, extraction time is respectively 2h.
5. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that the vacuum concentration Vacuum degree is -0.05MPa~0.088MPa；Thickening temperature: 65 DEG C of <.
6. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that the Ca (OH)2It is water-soluble Liquid is saturation Ca (OH)2Aqueous solution.
7. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that the Ca (OH)2It is water-soluble The dosage of liquid is 0.1 ~ 0.5 times of concentrate volume.
8. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that in S4, the precipitating Time be 12 ~ 36h.
9. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that the auxiliary material is malt Dextrin, beta-cyclodextrin, starch, carboxymethyl cellulose, the adding proportion of the auxiliary material are the 1 ~ 10% of final products weight.
10. the production method that low ash according to claim 1 divides Horsetail P.E, which is characterized in that the drying is spray Mist is dry or is freeze-dried；
The condition of the spray drying is inlet air temperature 160~200 DEG C, leaving air temp 90~100℃；The item of the freeze-drying Part be vacuum degree be -0.07MPa~-0.088MPa, < -10 DEG C of temperature.
CN201910427622.5A 2019-05-22 2019-05-22 The production method that a kind of low ash divides Horsetail P.E Pending CN110101666A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117224436A (en) * 2023-11-07 2023-12-15 成都乾坤动物药业股份有限公司 Extraction method of sun-proof component of pteridophyte

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117224436A (en) * 2023-11-07 2023-12-15 成都乾坤动物药业股份有限公司 Extraction method of sun-proof component of pteridophyte
CN117224436B (en) * 2023-11-07 2024-01-26 成都乾坤动物药业股份有限公司 Extraction method of sun-proof component of pteridophyte

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