CN111214563A - Preparation method of effective component of bighead atractylodes rhizome-immature bitter orange medicine pair - Google Patents
Preparation method of effective component of bighead atractylodes rhizome-immature bitter orange medicine pair Download PDFInfo
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- CN111214563A CN111214563A CN201811410599.0A CN201811410599A CN111214563A CN 111214563 A CN111214563 A CN 111214563A CN 201811410599 A CN201811410599 A CN 201811410599A CN 111214563 A CN111214563 A CN 111214563A
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/28—Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
- A61K36/284—Atractylodes
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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)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P1/00—Drugs for disorders of the alimentary tract or the digestive system
- A61P1/10—Laxatives
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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
- A61K2236/30—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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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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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Abstract
The invention discloses a preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine pair, which comprises the following steps: reflux-extracting Atractylodis rhizoma and fructus Aurantii Immaturus with 65-75% ethanol for 2-4 times (each for 1.5-2.5 hr), mixing extractive solutions, and concentrating under reduced pressure to obtain extract; sequentially extracting the extract with petroleum ether, chloroform, ethyl acetate and water saturated n-butanol, and concentrating under reduced pressure; separating ethyl acetate part with polyamide column chromatography, eluting with deionized water, 20% ethanol, 50% ethanol and 70% ethanol in sequence, collecting 70% ethanol eluate, concentrating under reduced pressure, separating with silica gel column chromatography, eluting with dichloromethane-methanol at volume ratio of 90:1, 78:1, 54:1, 31:1, 17:1 and 1:1 in sequence, collecting 17:1 eluate, and concentrating to obtain the final product. The method provided by the invention can quickly obtain the effective components in the bighead atractylodes rhizome-immature bitter orange medicine pair, and has the effect of relaxing bowel.
Description
Technical Field
The invention relates to a preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine pair.
Background
Slow Transit Constipation (STC) refers to constipation caused by retention of intestinal contents in the colon or slow transit of the colon due to colonic motility disorder, and is clinically manifested by decreased defecation frequency, no defecation, or involuntary defecation, and most of them are accompanied by symptoms such as abdominal distension and anorexia. With the change of dietary structure, the acceleration of life rhythm and the influence of psychosocial factors, the incidence of STC is increased year by year, which accounts for about 45.5% of chronic constipation, can occur in people of different ages, increases with the increase of ages, is a common clinical chronic gastrointestinal disease, and seriously affects the physical and mental health of human beings. Recently, many doctors propose that large dose of raw rhizoma atractylodis macrocephalae has the function of relaxing bowels, and the effect is better after the raw rhizoma atractylodis macrocephalae is combined with immature bitter orange.
Disclosure of Invention
The invention aims to provide a preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine.
The invention is realized by the following technical scheme:
a preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine pair comprises the following steps: reflux-extracting 35-45 parts of Atractylodis rhizoma and 5-15 parts of fructus Aurantii Immaturus with 6 times of 65-75% ethanol for 2-4 times (each for 1.5-2.5 hr), mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, sequentially extracting with petroleum ether, chloroform, ethyl acetate and water saturated n-butanol, and concentrating under reduced pressure; separating ethyl acetate part with polyamide column chromatography, eluting with deionized water, 20% ethanol, 50% ethanol and 70% ethanol in sequence, collecting 70% ethanol eluate, concentrating under reduced pressure, separating with silica gel column chromatography, eluting with dichloromethane-methanol at volume ratio of 90:1, 78:1, 54:1, 31:1, 17:1 and 1:1 in sequence, collecting 17:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
Preferably, in the preparation method, ethanol with the volume fraction of 70% is used for reflux extraction.
Preferably, in the preparation method, reflux extraction is performed for 3 times.
Preferably, in the preparation method, each extraction time is 2 hours.
The invention has the technical effects that:
the method provided by the invention is simple and convenient to operate, can quickly obtain the effective components in the bighead atractylodes rhizome-immature bitter orange medicine pair, has the effect of relaxing bowel, has a huge market prospect, and can be prepared in a large scale.
Detailed Description
The following describes the substance of the present invention with reference to the examples.
Example 1
A preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine pair comprises the following steps: taking 40 parts of bighead atractylodes rhizome and 10 parts of immature bitter orange, performing reflux extraction for 3 times with 6 times of ethanol with the volume fraction of 70% for 2 hours each time, combining extracting solutions, and performing reduced pressure concentration on the extracting solutions to obtain an extract; dissolving the extract with appropriate amount of water, sequentially extracting with petroleum ether, chloroform, ethyl acetate and water saturated n-butanol, and concentrating under reduced pressure; separating ethyl acetate part with polyamide column chromatography, eluting with deionized water, 20% ethanol, 50% ethanol and 70% ethanol in sequence, collecting 70% ethanol eluate, concentrating under reduced pressure, separating with silica gel column chromatography, eluting with dichloromethane-methanol at volume ratio of 90:1, 78:1, 54:1, 31:1, 17:1 and 1:1 in sequence, collecting 17:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
Example 2
A preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine pair comprises the following steps: taking 35 parts of bighead atractylodes rhizome and 5 parts of immature bitter orange, carrying out reflux extraction for 2 times by using 6 times of 65% ethanol in volume fraction, each time for 1.5 hours, combining extracting solutions, and concentrating the extracting solution under reduced pressure to obtain an extract; dissolving the extract with appropriate amount of water, sequentially extracting with petroleum ether, chloroform, ethyl acetate and water saturated n-butanol, and concentrating under reduced pressure; separating ethyl acetate part with polyamide column chromatography, eluting with deionized water, 20% ethanol, 50% ethanol and 70% ethanol in sequence, collecting 70% ethanol eluate, concentrating under reduced pressure, separating with silica gel column chromatography, eluting with dichloromethane-methanol at volume ratio of 90:1, 78:1, 54:1, 31:1, 17:1 and 1:1 in sequence, collecting 17:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
Example 3
A preparation method of an effective component of a bighead atractylodes rhizome-immature bitter orange medicine pair comprises the following steps: taking 45 parts of bighead atractylodes rhizome and 15 parts of immature bitter orange, carrying out reflux extraction for 4 times by using 6 times of 75% ethanol in volume fraction, each time for 2.5 hours, combining extracting solutions, and concentrating the extracting solution under reduced pressure to obtain an extract; dissolving the extract with appropriate amount of water, sequentially extracting with petroleum ether, chloroform, ethyl acetate and water saturated n-butanol, and concentrating under reduced pressure; separating ethyl acetate part with polyamide column chromatography, eluting with deionized water, 20% ethanol, 50% ethanol and 70% ethanol in sequence, collecting 70% ethanol eluate, concentrating under reduced pressure, separating with silica gel column chromatography, eluting with dichloromethane-methanol at volume ratio of 90:1, 78:1, 54:1, 31:1, 17:1 and 1:1 in sequence, collecting 17:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
The method provided by the invention is simple and convenient to operate, can quickly obtain the effective components in the bighead atractylodes rhizome-immature bitter orange medicine pair, has the effect of relaxing bowel, has a huge market prospect, and can be prepared in a large scale.
Claims (4)
1. A preparation method of an active ingredient of a bighead atractylodes rhizome-immature bitter orange medicine pair is characterized by comprising the following steps: reflux-extracting 35-45 parts of Atractylodis rhizoma and 5-15 parts of fructus Aurantii Immaturus with 6 times of 65-75% ethanol for 2-4 times (each for 1.5-2.5 hr), mixing extractive solutions, and concentrating under reduced pressure to obtain extract; dissolving the extract with appropriate amount of water, sequentially extracting with petroleum ether, chloroform, ethyl acetate and water saturated n-butanol, and concentrating under reduced pressure; separating ethyl acetate part with polyamide column chromatography, eluting with deionized water, 20% ethanol, 50% ethanol and 70% ethanol in sequence, collecting 70% ethanol eluate, concentrating under reduced pressure, separating with silica gel column chromatography, eluting with dichloromethane-methanol at volume ratio of 90:1, 78:1, 54:1, 31:1, 17:1 and 1:1 in sequence, collecting 17:1 eluate, and concentrating to obtain the final product; the raw materials are in parts by weight.
2. The method of claim 1, wherein: extracting with 70% ethanol under reflux.
3. The method of claim 2, wherein: reflux extracting for 3 times.
4. The production method according to claim 3, characterized in that: each time for 2 h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811410599.0A CN111214563A (en) | 2018-11-24 | 2018-11-24 | Preparation method of effective component of bighead atractylodes rhizome-immature bitter orange medicine pair |
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| CN201811410599.0A CN111214563A (en) | 2018-11-24 | 2018-11-24 | Preparation method of effective component of bighead atractylodes rhizome-immature bitter orange medicine pair |
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| CN111214563A true CN111214563A (en) | 2020-06-02 |
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| CN201811410599.0A Pending CN111214563A (en) | 2018-11-24 | 2018-11-24 | Preparation method of effective component of bighead atractylodes rhizome-immature bitter orange medicine pair |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115227752A (en) * | 2022-08-11 | 2022-10-25 | 云南曲中生物医药科技有限公司 | Traditional Chinese medicine composition for treating spleen-kidney yang deficiency type constipation, preparation and application |
-
2018
- 2018-11-24 CN CN201811410599.0A patent/CN111214563A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115227752A (en) * | 2022-08-11 | 2022-10-25 | 云南曲中生物医药科技有限公司 | Traditional Chinese medicine composition for treating spleen-kidney yang deficiency type constipation, preparation and application |
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Application publication date: 20200602 |
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