CN108653430A - A kind of preparation method of the shaggy-fruited dittany extract with antitumor action - Google Patents
A kind of preparation method of the shaggy-fruited dittany extract with antitumor action Download PDFInfo
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- 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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- A61K2236/30—Extraction of the material
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- 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
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- 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 kind of preparation methods of the shaggy-fruited dittany extract with antitumor action, and steps are as follows：The dry root skin of shaggy-fruited dittany is crushed, it is that 85 95% ethyl alcohol impregnate 2 4d first to use volume fraction, and then at 60 70 DEG C of circumfluence distillations 13 times, 80 100min, merges extracting solution every time, and extracting solution is concentrated under reduced pressure to give medicinal extract；By medicinal extract to use large pore resin absorption column chromatographic isolation after appropriate water dissolution, pure water, ethanol gradient elution are used successively, collects 85% alcohol elution, then detach through silica gel column chromatography, use volume ratio 65 successively:1、45:1、22:1、5:1 chloroform methanol elution, collects 22:1 elution fraction, concentrates to obtain the final product.The method that the present invention is combined using extraction and heat reflux, can comprehensively, effectively extract the ingredient with antitumor action in shaggy-fruited dittany root skin, can be prepared applied to drug as the active component of shaggy-fruited dittany.
Description
Technical field
The present invention relates to a kind of preparation methods of the shaggy-fruited dittany extract with antitumor action.
Background technology
Shaggy-fruited dittany（Dictamnus dasycarpusTurcz.）It is under the jurisdiction of Rutaceae（Rutaceae）Shaggy-fruited dittany category
（DictamnusL.）, it is perennial herbaceous plant, plant has strong peat-reek, is distributed mainly on Europe and Asia
Continent some areas.About 5 kinds of the category whole world, Chinese Plants will record a kind.According to history tree and《Chinese Pharmacopoeia》2010 editions one
Record is recorded, Dictamnus dasycarpus Turcz is the dry root skin of Rutaceae shaggy-fruited dittany platymiscium shaggy-fruited dittany, is Chinese conventional Chinese medicine, also known as north is fresh
Skin, Zanthoxylum simulans root skin, smelly root skin etc..Modern pharmacology research show Dictamnus dasycarpus Turcz have heat-clearing and damp-drying drug, dispelling wind and arresting itching and
Removing toxic substances and other effects, to treat the diseases such as dripping yellow water, eczema, beriberoid pyretic arthralgia, mange sore leprosy, jaundice, so as to cause extensive
Concern.
Currently, identifying a variety of chemical compositions, including volatile oil, biology from shaggy-fruited dittany root skin and aerial part are separated
The ingredients such as bases, limonin, compound of polysaccharide and cumarin, flavonoids, steroid.Alkaloid contained in the root bark of shaggy-fruited dittany
For furoquinoline Alkaloid, mainly have dictamine, skimmianine, trigonelline, choline, γ-fagarine, different spot Buddhist woods potash,
7,8-dimethoxymyrtopsine、O-ethylnor-γ-fagarine、platydesmine、O-ethylnor
Dictamine, O-ethylnorskimmianin, 7,8-dimethoxyplaty desmine etc., wherein dictamine are shaggy-fruited dittany
One of index components of skin.In addition, limonoid is that most commonly used a kind of compound is distributed in shaggy-fruited dittany platymiscium,
For a major class important activity ingredient in the root bark of shaggy-fruited dittany.
Shaggy-fruited dittany plant volatile oil substance such as sesquiterpenoids etc. has antitumor hyperplasia and cellular cytoxicity activity,
It significantly inhibits the growth of 6 kinds of tumor cell lines, such as human breast tumor's cell strain（MCF-7, ZR-75-30
And MDA-MB-435S）, human liver cancer cell line（Bel-7402 and HepG2）And human adrenal cells' cell strain
（ACHN）.In addition, volatile oil also has strong inhibition Methicillin-resistant Staphylococcus aureus and staphylococcus aureus in the root bark of shaggy-fruited dittany
The activity of ATCC 25923.Alkaloid has the effects that cardiac stimulant, anti-inflammatory, vasoconstriction smooth muscle, resisting pathogenic microbes.Wherein,
Dictamine is its important activity ingredient, has antibacterial, antiviral and skin eczema, pruitus and Anticancer Activity in vitro etc. a variety of
Bioactivity.Lemon hardship chlorins compound fraxinellone in the root bark of shaggy-fruited dittany has Anticancer Activity in vitro, and can be used as a kind of novel liver
Sick medicine has the effects that good protecting liver, lowering enzymes and inhibits liver fibrosis.Pharmacological evaluation shows root bark of shaggy-fruited dittany Thick many candies energy
Obviously increase the weight of normal mouse thymus gland and spleen, improve reticuloendothelial system phagocytic function, have antifatigue, resist oxygen lack,
Resisting stress capability is improved, mouse choleresis can be remarkably promoted, accelerates poisonous substance excretion in liver, to protect liver.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of the shaggy-fruited dittany extract with antitumor action.
The present invention is realized by following technical solution：
A kind of preparation method of the shaggy-fruited dittany extract with antitumor action, includes the following steps：By the dry root skin powder of shaggy-fruited dittany
It is broken, it is first that 85-95% ethyl alcohol impregnates 2-4d with volume fraction, then at 60-70 DEG C of circumfluence distillation 1-3 times, each 80-100min,
Merge extracting solution, extracting solution is concentrated under reduced pressure to give medicinal extract；By medicinal extract to use large pore resin absorption column chromatography point after appropriate water dissolution
From, successively with pure water, the ethanol gradient elution of volume fraction 10%, 35%, 55%, 85%, 95%, 85% alcohol elution is collected,
It is detached again through silica gel column chromatography, uses volume ratio 65 successively:1、45:1、22:1、5:1 chloroform-methanol elution, collects 22:1 elution
Part concentrates to obtain the final product.
Preferably, it is that 90% ethyl alcohol impregnates 3d with volume fraction in the preparation method.
Preferably, in the preparation method, in 65 DEG C of circumfluence distillations.
Preferably, in the preparation method, circumfluence distillation 2 times.
Preferably, in the preparation method, each 90min.
Preferably, in the preparation method, 1kg shaggy-fruited dittanies root skin is extracted using 11-13L solvents.
Preferably, in the preparation method, by medicinal extract first to use cotton filtering to be inhaled again with macropore after appropriate water dissolution
Attached resin column chromatography separation.
Preferably, in the preparation method, the 7-9mL water dissolutions of 1g medicinal extract.
Preferably, in the preparation method, the large pore resin absorption column is AB-8 types.
The technology of the present invention effect：
The present invention comprehensively, can be extracted effectively in shaggy-fruited dittany root skin using the method extracted and heat reflux combines with antitumor
The ingredient of effect can be prepared as the active component of shaggy-fruited dittany applied to drug.
Specific implementation mode
The essentiality content of the present invention is specifically introduced with reference to embodiment.
Embodiment 1
A kind of preparation method of the shaggy-fruited dittany extract with antitumor action, includes the following steps：By the dry root skin powder of shaggy-fruited dittany
Broken, it is that 90% ethyl alcohol impregnates 3d first to use volume fraction, then at 65 DEG C of circumfluence distillations 2 times, each 90min, merges extracting solution, carries
Liquid is taken to be concentrated under reduced pressure to give medicinal extract；By medicinal extract first to use cotton filtering to use AB-8 type macroporous absorbent resins again after appropriate water dissolution
Pillar layer separation is collected 85% ethyl alcohol and is washed successively with pure water, the ethanol gradient elution of volume fraction 10%, 35%, 55%, 85%, 95%
De- position, then detached through silica gel column chromatography, volume ratio 65 is used successively:1、45:1、22:1、5:1 chloroform-methanol elution, is collected
22:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg shaggy-fruited dittanies root skin is extracted using 12L solvents, the 8mL water dissolutions of 1g medicinal extract.
Embodiment 2
A kind of preparation method of the shaggy-fruited dittany extract with antitumor action, includes the following steps：By the dry root skin powder of shaggy-fruited dittany
Broken, it is that 85% ethyl alcohol impregnates 2d first to use volume fraction, then at 60 DEG C of circumfluence distillations 1 time, each 80min, merges extracting solution, carries
Liquid is taken to be concentrated under reduced pressure to give medicinal extract；By medicinal extract first to use cotton filtering to use AB-8 type macroporous absorbent resins again after appropriate water dissolution
Pillar layer separation is collected 85% ethyl alcohol and is washed successively with pure water, the ethanol gradient elution of volume fraction 10%, 35%, 55%, 85%, 95%
De- position, then detached through silica gel column chromatography, volume ratio 65 is used successively:1、45:1、22:1、5:1 chloroform-methanol elution, is collected
22:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg shaggy-fruited dittanies root skin is extracted using 11L solvents, the 7mL water dissolutions of 1g medicinal extract.
Embodiment 3
A kind of preparation method of the shaggy-fruited dittany extract with antitumor action, includes the following steps：By the dry root skin powder of shaggy-fruited dittany
Broken, it is that 95% ethyl alcohol impregnates 4d first to use volume fraction, then at 70 DEG C of circumfluence distillations 3 times, each 100min, merges extracting solution, carries
Liquid is taken to be concentrated under reduced pressure to give medicinal extract；By medicinal extract first to use cotton filtering to use AB-8 type macroporous absorbent resins again after appropriate water dissolution
Pillar layer separation is collected 85% ethyl alcohol and is washed successively with pure water, the ethanol gradient elution of volume fraction 10%, 35%, 55%, 85%, 95%
De- position, then detached through silica gel column chromatography, volume ratio 65 is used successively:1、45:1、22:1、5:1 chloroform-methanol elution, is collected
22:1 elution fraction, concentrates to obtain the final product.
Wherein, 1kg shaggy-fruited dittanies root skin is extracted using 13L solvents, the 9mL water dissolutions of 1g medicinal extract.
The present invention comprehensively, can be extracted effectively in shaggy-fruited dittany root skin using the method extracted and heat reflux combines with anti-
The ingredient of function of tumor can be prepared as the active component of shaggy-fruited dittany applied to drug.
Claims (9)
1. a kind of preparation method of the shaggy-fruited dittany extract with antitumor action, it is characterised in that include the following steps：By shaggy-fruited dittany
Dry root skin crush, be first that 85-95% ethyl alcohol impregnates 2-4d with volume fraction, then at 60-70 DEG C of circumfluence distillation 1-3 times, often
Secondary 80-100min, merges extracting solution, and extracting solution is concentrated under reduced pressure to give medicinal extract；By medicinal extract to use macroporous absorption after appropriate water dissolution
Resin column chromatography detaches, and successively with pure water, the ethanol gradient elution of volume fraction 10%, 35%, 55%, 85%, 95%, collects 85% second
Alcohol elutes position, then is detached through silica gel column chromatography, uses volume ratio 65 successively:1、45:1、22:1、5:1 chloroform-methanol elution,
Collect 22:1 elution fraction, concentrates to obtain the final product.
2. preparation method according to claim 1, it is characterised in that：It is that 90% ethyl alcohol impregnates 3d with volume fraction.
3. preparation method according to claim 1, it is characterised in that：In 65 DEG C of circumfluence distillations.
4. preparation method according to claim 3, it is characterised in that：Circumfluence distillation 2 times.
5. preparation method according to claim 4, it is characterised in that：Each 90min.
6. preparation method according to claim 1, it is characterised in that：1kg shaggy-fruited dittanies root skin is carried using 11-13L solvents
It takes.
7. preparation method according to claim 1, it is characterised in that：By medicinal extract first to use cotton mistake after appropriate water dissolution
Large pore resin absorption column chromatographic isolation is used in filter again.
8. preparation method according to claim 7, it is characterised in that：The 7-9mL water dissolutions of 1g medicinal extract.
9. preparation method according to claim 7, it is characterised in that：The large pore resin absorption column is AB-8 types.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109394870A (en) * | 2018-11-14 | 2019-03-01 | 哈尔滨职业技术学院 | The preparation method at anticancer activity position, content assaying method and its application in cortex dictamni |
| CN115414421A (en) * | 2022-08-31 | 2022-12-02 | 上海川跃生物科技有限公司 | Extraction method and application of cortex dictamni active ingredients |
| CN116693485A (en) * | 2023-06-07 | 2023-09-05 | 齐齐哈尔医学院 | Dittany ester C and preparation method and application thereof |
| CN116715707A (en) * | 2023-06-07 | 2023-09-08 | 齐齐哈尔医学院 | Dictamni-containing phenolic glycoside D and preparation method and application thereof |
-
2018
- 2018-07-24 CN CN201810817914.5A patent/CN108653430A/en not_active Withdrawn
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109394870A (en) * | 2018-11-14 | 2019-03-01 | 哈尔滨职业技术学院 | The preparation method at anticancer activity position, content assaying method and its application in cortex dictamni |
| CN109394870B (en) * | 2018-11-14 | 2021-03-19 | 哈尔滨职业技术学院 | Preparation method, content determination method and application of anticancer active site in cortex dictamni |
| CN115414421A (en) * | 2022-08-31 | 2022-12-02 | 上海川跃生物科技有限公司 | Extraction method and application of cortex dictamni active ingredients |
| CN115414421B (en) * | 2022-08-31 | 2023-07-18 | 上海川跃生物科技有限公司 | Extraction method and application of active ingredients of cortex dictamni |
| CN116693485A (en) * | 2023-06-07 | 2023-09-05 | 齐齐哈尔医学院 | Dittany ester C and preparation method and application thereof |
| CN116715707A (en) * | 2023-06-07 | 2023-09-08 | 齐齐哈尔医学院 | Dictamni-containing phenolic glycoside D and preparation method and application thereof |
| CN116693485B (en) * | 2023-06-07 | 2023-11-21 | 齐齐哈尔医学院 | Dittany ester C and preparation method and application thereof |
| CN116715707B (en) * | 2023-06-07 | 2024-02-02 | 齐齐哈尔医学院 | Dictamni-containing phenolic glycoside D and preparation method and application thereof |
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