CN102846683A - Method for subcritical water extraction of Rhinacanthus nasutus (L.) Lindau element - Google Patents
Method for subcritical water extraction of Rhinacanthus nasutus (L.) Lindau element Download PDFInfo
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- CN102846683A CN102846683A CN 201210353627 CN201210353627A CN102846683A CN 102846683 A CN102846683 A CN 102846683A CN 201210353627 CN201210353627 CN 201210353627 CN 201210353627 A CN201210353627 A CN 201210353627A CN 102846683 A CN102846683 A CN 102846683A
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Abstract
The invention discloses a method for subcritical water extraction of a Rhinacanthus nasutus (L.) Lindau element. The method comprises the steps of: drying and crushing a Rhinacanthus nasutus (L.) Lindau raw material, then putting the material in a subcritical extraction kettle, introducing deionized water to conduct extraction, and cooling the obtained extract to room temperature, adding the extract into a macroporous resin column to perform adsorption, carrying out ethanol solution gradient elution, subjecting the eluent to pressure reduced concentration, extracting the concentrated solution with petroleum ether, collecting a petroleum ether phase, and recovering petroleum ether, thus obtaining the Rhinacanthus nasutus (L.) Lindau element. Employment of the method for production has the characteristics of high extraction efficiency, simple operation, and easy industrialization.
Description
Technical field
The invention belongs to the Natural Medicine Chemistry field, particularly a kind of method of utilizing the Subcritical Water Extraction rhinacanthin.
Background technology
Subcritical abstraction is to utilize subcritical fluids as extractant, in the pressure vessel of airtight, anaerobic, pressure, according to the similar principle that mixes of Organic substance, by extraction material and the molecular diffusion process of extractant in immersion process, the liposoluble constituent that reaches in the solid material is transferred in the liquid extractant, the process of passing through reduction vaporization again finally obtains a kind of novel extraction and the isolation technics of purpose product with extractant and purpose product separation.Subcritical fluid extraction is compared other separation method many advantages, and the biologically active prod that can keep extract does not destroy, not oxidation, but the large large-scale industrialization production of production capacity is energy-conservation, operating cost is low, is easy to and product separation.
Ramulus et Folium Rhinacanthi nasuti Rhinacanthus nasutus (L.) Lindau is acanthaceous plant, and the another name euphorbia peplus has the function of lung moistening pathogenic fire reducing, killing parasites for relieving itching, cures mainly the diseases such as pulmonary tuberculosis, oedema due to nephritis, tinea corporis, eczema.The modern study discovery contains multiple naphthoquinone compound in the Ramulus et Folium Rhinacanthi nasuti, such as rhinacanthin A, rhinacanthin B, Rhinacanthin C, Ramulus et Folium Rhinacanthi nasuti D etc., this compounds has than the powerful antitumor effect.
By literature search, find no the industrial method of the method for extraction rhinacanthin from Ramulus et Folium Rhinacanthi nasuti.
Summary of the invention
The objective of the invention is to solve the deficiencies in the prior art, a kind of industrial method that utilizes the Subcritical Water Extraction rhinacanthin is provided.
To achieve these goals, the present invention is by the following technical solutions:
A kind of method of utilizing the Subcritical Water Extraction rhinacanthin, it is characterized in that: pulverize behind the Ramulus et Folium Rhinacanthi nasuti raw material drying, drop into the subcritical abstraction still, pass into deionized water and extract, the gained extract is chilled to room temperature, add in the macroporous resin column and adsorb alcoholic solution gradient elution, eluent concentrating under reduced pressure, the eluent concentrating under reduced pressure, the concentrated solution petroleum ether extraction is collected the petroleum ether phase, reclaims petroleum ether and namely gets rhinacanthin.
The subcritical abstraction condition is: extraction temperature is that 120 ~ 180 ℃, pressure are that 0.3 ~ 2MPa, time are 30 ~ 60min.
A kind of among the optional D101 of macroporous resin model, AB-8, HPD100 and the HZ816.
Ethanol gradient elution is used 4 ~ 7 column volumes, 60 ~ 95% ethanol elution effective ingredient again for 3 ~ 5 column volumes, 10 ~ 50% alcoholic solution eluting impurity.
The present invention adopts Subcritical Water Extraction, is the principle of utilizing Ramulus et Folium Rhinacanthi nasuti to mix at high temperature, high pressure and subcritical water, and is not only can extraction efficiency high, and consumption of organic solvent is few, can also shorten the production cycle and reduce environmental pollution, whole simple for process, be fit to suitability for industrialized production.
The specific embodiment
Embodiment 1:
The Ramulus et Folium Rhinacanthi nasuti raw material, crushed after being dried is got 4kg and is dropped in the subcritical abstraction still, pass into deionized water, set 150 ℃ of extraction temperature, pressure is 0.5MPa, dynamic extraction 30min, extract is chilled to room temperature, adds in the D101 macroporous resin column to adsorb, 3 column volumes, 40% alcoholic solution eluting impurity is used 4 column volumes, 90% ethanol elution effective ingredient, the eluent concentrating under reduced pressure again, concentrated solution petroleum ether extraction 2 times, collect petroleum ether layer, reclaim petroleum ether, get grease rhinacanthin 10g.
Embodiment 2:
The Ramulus et Folium Rhinacanthi nasuti raw material, crushed after being dried is got 4kg and is dropped in the subcritical abstraction still, pass into deionized water, set 120 ℃ of extraction temperature, pressure is 0.3MPa, dynamic extraction 40min, extract is chilled to room temperature, adds in the AB-8 macroporous resin column to adsorb, 3 column volumes, 50% alcoholic solution eluting impurity is used 5 column volumes, 80% ethanol elution effective ingredient, the eluent concentrating under reduced pressure again, concentrated solution petroleum ether extraction 3 times, collect petroleum ether layer, reclaim petroleum ether, get grease rhinacanthin 7.5g.
Embodiment 3:
The Ramulus et Folium Rhinacanthi nasuti raw material, crushed after being dried is got 4kg and is dropped in the subcritical abstraction still, pass into deionized water, set 130 ℃ of extraction temperature, pressure is 0.6MPa, dynamic extraction 50min, extract is chilled to room temperature, adds in the HPD100 macroporous resin column to adsorb, 5 column volumes, 40% alcoholic solution eluting impurity is used 6 column volumes, 70% ethanol elution effective ingredient, the eluent concentrating under reduced pressure again, concentrated solution petroleum ether extraction 3 times, collect petroleum ether layer, reclaim petroleum ether, get grease rhinacanthin 8.1g.
Embodiment 4:
The Ramulus et Folium Rhinacanthi nasuti raw material, crushed after being dried is got 4kg and is dropped in the subcritical abstraction still, pass into deionized water, set 140 ℃ of extraction temperature, pressure is 0.4MPa, dynamic extraction 30min, extract is chilled to room temperature, adds in the HZ816 macroporous resin column to adsorb, 4 column volumes, 50% alcoholic solution eluting impurity is used 4 column volumes, 80% ethanol elution effective ingredient, the eluent concentrating under reduced pressure again, concentrated solution petroleum ether extraction 2 times, collect petroleum ether layer, reclaim petroleum ether, get grease rhinacanthin 7.8g.
Claims (4)
1. method of utilizing the Subcritical Water Extraction rhinacanthin, it is characterized in that: pulverize behind the Ramulus et Folium Rhinacanthi nasuti raw material drying, drop into the subcritical abstraction still, pass into deionized water and extract, the gained extract is chilled to room temperature, add in the macroporous resin column and adsorb, the alcoholic solution gradient elution, eluent concentrating under reduced pressure, concentrated solution petroleum ether extraction, collect the petroleum ether phase, reclaim petroleum ether and namely get rhinacanthin.
2. a kind of method of utilizing the Subcritical Water Extraction rhinacanthin according to claim 1 is characterized in that described subcritical abstraction condition is: extraction temperature is that 120 ~ 180 ℃, pressure are that 0.3 ~ 2MPa, time are 30 ~ 60min.
3. a kind of method of utilizing the Subcritical Water Extraction rhinacanthin according to claim 1 is characterized in that a kind of among the optional D101 of described macroporous resin model, AB-8, HPD100 and the HZ816.
4. a kind of method of utilizing the Subcritical Water Extraction rhinacanthin according to claim 1 is characterized in that described ethanol gradient elution is with 3 ~ 5 column volumes, 10 ~ 50% alcoholic solution eluting impurity, uses 4 ~ 7 column volumes, 60 ~ 95% ethanol elution effective ingredient again.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201210353627 CN102846683A (en) | 2012-09-21 | 2012-09-21 | Method for subcritical water extraction of Rhinacanthus nasutus (L.) Lindau element |
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| CN 201210353627 CN102846683A (en) | 2012-09-21 | 2012-09-21 | Method for subcritical water extraction of Rhinacanthus nasutus (L.) Lindau element |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103356749A (en) * | 2013-07-19 | 2013-10-23 | 苏州市天灵中药饮片有限公司 | Subcritical water extraction process of shuanghuanglian |
| CN115385795A (en) * | 2022-10-11 | 2022-11-25 | 广西中医药大学赛恩斯新医药学院 | Preparation method and application of rhinacanthus nasutus and ganoderma naphthoquinone monomer rhinacanthin-C |
-
2012
- 2012-09-21 CN CN 201210353627 patent/CN102846683A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103356749A (en) * | 2013-07-19 | 2013-10-23 | 苏州市天灵中药饮片有限公司 | Subcritical water extraction process of shuanghuanglian |
| CN115385795A (en) * | 2022-10-11 | 2022-11-25 | 广西中医药大学赛恩斯新医药学院 | Preparation method and application of rhinacanthus nasutus and ganoderma naphthoquinone monomer rhinacanthin-C |
| CN115385795B (en) * | 2022-10-11 | 2023-11-17 | 广西中医药大学赛恩斯新医药学院 | Preparation method and application of Rhinacanthus nasuta (L.) kurz naphthoquinone monomer Rhinacanthin-C |
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Application publication date: 20130102 |