CN111214559A - Method for preparing anthraquinone components in madder - Google Patents

Method for preparing anthraquinone components in madder Download PDF

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Publication number
CN111214559A
CN111214559A CN201811413922.XA CN201811413922A CN111214559A CN 111214559 A CN111214559 A CN 111214559A CN 201811413922 A CN201811413922 A CN 201811413922A CN 111214559 A CN111214559 A CN 111214559A
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China
Prior art keywords
ethanol
radix rubiae
extract
collecting
separating
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Pending
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CN201811413922.XA
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Chinese (zh)
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不公告发明人
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Qidong Xingteng Trade Co Ltd
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Qidong Xingteng Trade Co Ltd
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Priority to CN201811413922.XA priority Critical patent/CN111214559A/en
Publication of CN111214559A publication Critical patent/CN111214559A/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)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/74Rubiaceae (Madder family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P7/00Drugs for disorders of the blood or the extracellular fluid
    • A61P7/04Antihaemorrhagics; Procoagulants; Haemostatic agents; Antifibrinolytic agents
    • 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
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • 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
    • A61K2236/55Liquid-liquid separation; Phase separation

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  • Health & Medical Sciences (AREA)
  • Natural Medicines & Medicinal Plants (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Animal Behavior & Ethology (AREA)
  • Biotechnology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Epidemiology (AREA)
  • Microbiology (AREA)
  • Medical Informatics (AREA)
  • Botany (AREA)
  • Alternative & Traditional Medicine (AREA)
  • Mycology (AREA)
  • Diabetes (AREA)
  • Hematology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The invention discloses a method for preparing anthraquinone components in madder, which comprises the following steps: reflux-extracting radix Rubiae coarse powder with ethanol for 1-3 times, each for 2.5-3.5 hr, mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, separating with macroporous adsorbent resin column chromatography, gradient eluting with pure water and ethanol with volume fraction of 10%, 35%, 55%, 70%, 80%, 95%, collecting 80% ethanol eluate, separating with silica gel column chromatography, eluting with chloroform-methanol with volume ratio of 65:1, 45:1, 24:1, 5:1, collecting 24:1 eluate, and concentrating. The method can comprehensively and effectively extract anthraquinone components from radix Rubiae, has good hemostatic effect, and can be used as effective component of radix Rubiae in medicine preparation.

Description

Method for preparing anthraquinone components in madder
Technical Field
The invention relates to a method for preparing anthraquinone components in madder.
Background
Rubia cordifolia is the root and rhizome of Rubia cordifolia of Rubiaceae. Collected in spring and autumn, removed of silt and dried in the sun. The rootstock is in irregular knot shape, the upper side is provided with a rootstock, and the lower side is provided with roots with different thicknesses. The root is cylindrical, is wavy and curved, has a length of 10-25 cm, a diameter of 0.2-1 cm, and has a reddish brown or dark brown surface with fine longitudinal lines and a few fine root marks. Crisp, flat cross section, purple red bark and yellowish red wood. Slight smell. Slightly bitter in taste. Cold in nature and bitter in taste. Fond warm and humid climates. High adaptability and high safety. Can be cultivated in all regions of the north. Is suitable for cultivating fertile sandy loam. Grows beside hillside rocks or in grass clusters at the sides of ditches. The main productions are Anwei, Hebei, Shaanxi, Henan and Shandong.
The main functional indications are as follows: cool blood and activate blood, dispel stasis, dredge meridians. Can be used for treating hematemesis, epistaxis, metrorrhagia, traumatic hemorrhage, amenorrhea, blood stasis, arthralgia, and traumatic injury with swelling and pain. It can stop bleeding without retaining stasis, and is indicated for bleeding due to heat syndrome, amenorrhea and abdominal pain, and traumatic injury. The cuttlefish bone has stronger haemostasis.
Disclosure of Invention
The invention aims to provide a method for preparing anthraquinone components in madder.
The invention is realized by the following technical scheme:
a method for preparing anthraquinone components in madder comprises the following steps: reflux-extracting radix Rubiae coarse powder with 10 times of 75-85% ethanol for 1-3 times (each for 2.5-3.5 hr), mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, separating with macroporous adsorbent resin column chromatography, gradient eluting with pure water and ethanol with volume fractions of 10%, 35%, 55%, 70%, 80%, and 95%, collecting 80% ethanol eluate, separating with silica gel column chromatography, eluting with chloroform-methanol with volume ratios of 65:1, 45:1, 24:1, and 5:1, collecting 24:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
Preferably, in the method, the madder coarse powder is extracted by refluxing with 10 times of ethanol with the volume fraction of 80%.
Preferably, in the method, the reflux extraction is performed for 2 times.
Preferably, in the method, each time is 3 hours.
Preferably, in the method, the macroporous adsorption resin column is AB-8 type.
The invention has the technical effects that:
the method can comprehensively and effectively extract anthraquinone components from radix Rubiae, has good hemostatic effect, and can be used as effective component of radix Rubiae in medicine preparation.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
A method for preparing anthraquinone components in madder comprises the following steps: reflux-extracting radix Rubiae coarse powder with 10 times of 80% ethanol for 2 times, each for 3 hr, mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, separating with AB-8 type macroporous adsorbent resin column chromatography, gradient eluting with pure water and ethanol with volume fraction of 10%, 35%, 55%, 70%, 80%, 95%, collecting 80% ethanol eluate, separating with silica gel column chromatography, eluting with chloroform-methanol with volume ratio of 65:1, 45:1, 24:1, 5:1, collecting 24:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
Example 2
A method for preparing anthraquinone components in madder comprises the following steps: reflux-extracting radix Rubiae coarse powder with 10 times of 75% ethanol for 1 time, each time for 2.5 hr, mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, separating with AB-8 type macroporous adsorbent resin column chromatography, gradient eluting with pure water and ethanol with volume fraction of 10%, 35%, 55%, 70%, 80%, 95%, collecting 80% ethanol eluate, separating with silica gel column chromatography, eluting with chloroform-methanol with volume ratio of 65:1, 45:1, 24:1, 5:1, collecting 24:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
Example 3
A method for preparing anthraquinone components in madder comprises the following steps: reflux-extracting radix Rubiae coarse powder with 10 times of 85% ethanol for 3 times, each time for 3.5 hr, mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, separating with AB-8 type macroporous adsorbent resin column chromatography, gradient eluting with pure water and ethanol with volume fraction of 10%, 35%, 55%, 70%, 80%, 95%, collecting 80% ethanol eluate, separating with silica gel column chromatography, eluting with chloroform-methanol with volume ratio of 65:1, 45:1, 24:1, 5:1, collecting 24:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
The method can comprehensively and effectively extract anthraquinone components from radix Rubiae, has good hemostatic effect, and can be used as effective component of radix Rubiae in medicine preparation.

Claims (5)

1. A method for preparing anthraquinone components in madder is characterized by comprising the following steps: reflux-extracting radix Rubiae coarse powder with 10 times of 75-85% ethanol for 1-3 times (each for 2.5-3.5 hr), mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, separating with macroporous adsorbent resin column chromatography, gradient eluting with pure water and ethanol with volume fractions of 10%, 35%, 55%, 70%, 80%, and 95%, collecting 80% ethanol eluate, separating with silica gel column chromatography, eluting with chloroform-methanol with volume ratios of 65:1, 45:1, 24:1, and 5:1, collecting 24:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
2. The method of claim 1, wherein: reflux-extracting radix Rubiae coarse powder with 10 times of 80% ethanol.
3. The method of claim 2, wherein: reflux extracting for 2 times.
4. The method of claim 3, wherein: 3h each time.
5. The method of claim 1, wherein: the macroporous absorption resin column is AB-8 type.
CN201811413922.XA 2018-11-26 2018-11-26 Method for preparing anthraquinone components in madder Pending CN111214559A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811413922.XA CN111214559A (en) 2018-11-26 2018-11-26 Method for preparing anthraquinone components in madder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811413922.XA CN111214559A (en) 2018-11-26 2018-11-26 Method for preparing anthraquinone components in madder

Publications (1)

Publication Number Publication Date
CN111214559A true CN111214559A (en) 2020-06-02

Family

ID=70828914

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811413922.XA Pending CN111214559A (en) 2018-11-26 2018-11-26 Method for preparing anthraquinone components in madder

Country Status (1)

Country Link
CN (1) CN111214559A (en)

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Application publication date: 20200602

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