CN109419981A - A kind of preparation method of Sanguis Draxonis flavoniod - Google Patents

A kind of preparation method of Sanguis Draxonis flavoniod Download PDF

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Publication number
CN109419981A
CN109419981A CN201710749323.4A CN201710749323A CN109419981A CN 109419981 A CN109419981 A CN 109419981A CN 201710749323 A CN201710749323 A CN 201710749323A CN 109419981 A CN109419981 A CN 109419981A
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CN
China
Prior art keywords
ethyl acetate
sanguis draxonis
preparation
ground
draxonis flavoniod
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Pending
Application number
CN201710749323.4A
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Chinese (zh)
Inventor
苏刘花
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Nanjing Zelang Medical Technology Co Ltd
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Nanjing Zelang Medical Technology Co Ltd
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Priority to CN201710749323.4A priority Critical patent/CN109419981A/en
Publication of CN109419981A publication Critical patent/CN109419981A/en
Pending legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • A61K36/896Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Biotechnology (AREA)
  • Botany (AREA)
  • Medical Informatics (AREA)
  • Medicinal Chemistry (AREA)
  • Microbiology (AREA)
  • Mycology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Epidemiology (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Abstract

The present invention relates to a kind of preparation process of Sanguis Draxonis flavoniod, which is that Resina Draconis-drug is ground into coarse powder, and ethyl acetate backflow is added to extract, and is filtered, and recycles ethyl acetate and is concentrated to dryness;The invention also discloses Sanguis Draxonis flavoniods, and venous thronbosis, focal cerebral ischemia, preparation to be inhibited to treat new application in ischemic brain edema drug.

Description

A kind of preparation method of Sanguis Draxonis flavoniod
Technical field
The present invention relates to a kind of preparation methods of Sanguis Draxonis flavoniod, belong to traditional Chinese medicine extyaction field.
Background technique
Resina Draconis is warm-natured, flat, sweet in flavor, salty, nontoxic, enters blood system, and return lung, spleen, kidney three pass through, and there is activating microcirculation and removing stasis medicinal, detumescence to stop Bitterly, astringing to arrest bleeding, the remarkable efficacies such as resolving hard lump, myogenic sore.Modern medical studies have confirmed that dragon's blood capsule has improvement machine Body microcirculation, improves the effects of body's immunity at adjustment body metabolism.
Flavone compound refers to that basic parent nucleus is the series compound of 2- phenyl chromone, is widely present in plant kingdom, Many medium-height grass the effective elements of the medicines, it is many kinds of, have multiple biological activities, except with antibacterial, anti-inflammatory, it is disease-resistant become, decompression, Outside the effects of clearing heat and detoxicating, calm, diuresis, anti-oxidant, anticancer, anti-cancer, inhibit in terms of also have remarkable result, be A kind of important natural organic oxidation-resistant agent with development prospect.The research trend of flavone compound is medicinal in its in recent years The exploitation of value is more related to the application study of extraction process, the assay of flavone compound and preparation preparation.
Reflux extraction is to extract material composition with the volatile organic solvent such as ethyl alcohol, and leachate is heated and is distilled, Middle volatile solvent distillate after and it is cooled, repetition flow back to leach container in extracts raw material, so in cycles, until effectively at Divide the complete method of refluxing extraction.Circumfluence method extracting solution heated time in evaporation boiler is longer, therefore is not suitable for heated be subject to brokenly The leaching of bad material composition.
Summary of the invention
The present invention be directed to the deficiencies in the prior art, it is desirable to provide a kind of high efficiency and selective, easy to operate, yield It is high, by-product is few, can realization of industrialization the method for preparing Sanguis Draxonis flavoniod.
Technical solution of the present invention is carried out according to the following steps:
A. Resina Draconis-drug is ground into coarse powder, adds 6-10 times to measure ethyl acetate backflow and extracts 2-3 times, 1-2 hours each, filtration, Merge 2 filtrates, recycle ethyl acetate and is concentrated to dryness;
B. ethyl acetate extract is ground into coarse powder, and the 0.2-0.5%NaOH solution for extracting object amount with 20-40 times stirs 20-40 Minute makes to dissolve, and filters;
C. filtrate is poured out supernatant, is discarded with 5-12%HCl tune pH to 1~2, standing 8-24 hours;
D. centrifugal filtering is precipitated, sediment is collected, is washed with deionized water to pH test paper and is detected as neutrality, 60 DEG C or less vacuum are dry It is dry, it crushes to get Sanguis Draxonis flavoniod.
The extraction of ethyl acetate backflow described in step a is acetic acid and ethyl ester boiling because reversible reaction needs the time longer Point is again relatively low, in order to prevent ethyl acetate volatilization loss in reaction process, so using reflux measure.
The mass ratio of ion water consumption and raw material described in step c is 1:1.
The present invention has the advantages that
1. the present invention extracts general flavone using reflux extraction, have the advantages that production cost is low, quick, efficient, recovery rate is high.
The present invention is further illustrated below in conjunction with specific embodiment, but the scope of protection of present invention is not limited to In following embodiments.
Specific embodiment:
Embodiment 1:
Resina Draconis-drug is ground into coarse powder, 6 times of amount ethyl acetate backflows is added to extract 2-3 times, it is 1-2 hours each, it filters, merges 2 filtrates are recycled ethyl acetate and are concentrated to dryness;Ethyl acetate extract is ground into coarse powder, extracts the 0.2% of object amount with 20 times NaOH solution, which stirs 30 minutes, to be made to dissolve, and is filtered;Filtrate pours out supernatant with 5%HCl tune pH to 1~2, standing 8 hours, abandons It goes;Centrifugal filtering is precipitated, sediment is collected, is washed with deionized water to pH test paper and is detected as neutrality, 70 DEG C or less vacuum drying, powder It is broken to get Sanguis Draxonis flavoniod, yield 73%.
Embodiment 2:
Resina Draconis-drug is ground into coarse powder, adds 6 times of amount ethyl acetate backflows to extract 2 times, 1 hour every time, filtration merged 2 filters Liquid recycles ethyl acetate and is concentrated to dryness;Ethyl acetate extract is ground into coarse powder, and the 0.2%NaOH that object amount is extracted with 30 times is molten Liquid, which stirs 30 minutes, to be made to dissolve, and is filtered;Filtrate is poured out supernatant, is discarded with 5%HCl tune pH to 1~2, standing 16 hours;Precipitating Centrifugal filtering collects sediment, is washed with deionized water to pH test paper and is detected as neutrality, 80 DEG C or less vacuum drying, crushing to get Sanguis Draxonis flavoniod, yield 74%.
Embodiment 3:
Resina Draconis-drug is ground into coarse powder, adds 10 times of amount ethyl acetate backflows to extract 3 times, 2 hours every time, filtration merged 2 filters Liquid recycles ethyl acetate and is concentrated to dryness;Ethyl acetate extract is ground into coarse powder, and the 0.5%NaOH of object amount is extracted with 40 times Solution, which stirs 40 minutes, to be made to dissolve, and is filtered;Filtrate is poured out supernatant, is discarded with 12%HCl tune pH to 1~2, standing 24 hours; Centrifugal filtering is precipitated, sediment is collected, is washed with deionized water to pH test paper and is detected as neutrality, 90 DEG C or less vacuum drying crush, Up to Sanguis Draxonis flavoniod, yield 76%.

Claims (3)

1. a kind of preparation method of Sanguis Draxonis flavoniod, it is characterised in that:
A. Resina Draconis-drug is ground into coarse powder, adds 6-10 times to measure ethyl acetate backflow and extracts 2-3 times, 1-2 hours each, filtration, Merge 2 filtrates, recycle ethyl acetate and is concentrated to dryness;
B. ethyl acetate extract is ground into coarse powder, and the 0.2-0.5%NaOH solution for extracting object amount with 20-40 times stirs 20-40 Minute makes to dissolve, and filters;
C. filtrate is poured out supernatant, is discarded with 5-12%HCl tune pH to 1~2, standing 8-24 hours;
D. centrifugal filtering is precipitated, sediment is collected, is washed with deionized water to pH test paper and is detected as neutrality, 60 DEG C or less vacuum are dry It is dry, it crushes to get Sanguis Draxonis flavoniod.
2. a kind of preparation method of Sanguis Draxonis flavoniod according to claim 1, which is characterized in that described in step a Ethyl acetate backflow extraction is because reversible reaction needs the time longer, and acetic acid and ethyl ester boiling point are again relatively low, in order to prevent instead Ethyl acetate volatilization loss during answering, so using reflux measure.
3. a kind of preparation method of cordate houttuynia total flavones according to claim 1, which is characterized in that described in step c The mass ratio of ion water consumption and raw material is 1:1.
CN201710749323.4A 2017-08-28 2017-08-28 A kind of preparation method of Sanguis Draxonis flavoniod Pending CN109419981A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710749323.4A CN109419981A (en) 2017-08-28 2017-08-28 A kind of preparation method of Sanguis Draxonis flavoniod

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710749323.4A CN109419981A (en) 2017-08-28 2017-08-28 A kind of preparation method of Sanguis Draxonis flavoniod

Publications (1)

Publication Number Publication Date
CN109419981A true CN109419981A (en) 2019-03-05

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111686056A (en) * 2020-06-13 2020-09-22 云南民族大学 Method for preparing lip balm containing natural dragon's blood extract
WO2024082330A1 (en) * 2022-10-21 2024-04-25 湖南祥民制药有限公司 Method for extracting resina draconis

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111686056A (en) * 2020-06-13 2020-09-22 云南民族大学 Method for preparing lip balm containing natural dragon's blood extract
WO2024082330A1 (en) * 2022-10-21 2024-04-25 湖南祥民制药有限公司 Method for extracting resina draconis

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Application publication date: 20190305