CN109705128A - A method of extracting high-purity dendrobine from dendrobium nobile - Google Patents
A method of extracting high-purity dendrobine from dendrobium nobile Download PDFInfo
- Publication number
- CN109705128A CN109705128A CN201811574062.8A CN201811574062A CN109705128A CN 109705128 A CN109705128 A CN 109705128A CN 201811574062 A CN201811574062 A CN 201811574062A CN 109705128 A CN109705128 A CN 109705128A
- Authority
- CN
- China
- Prior art keywords
- dendrobine
- filtrate
- dendrobium nobile
- filter residue
- added
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Saccharide Compounds (AREA)
Abstract
The present invention discloses a kind of method that high-purity dendrobine is extracted from dendrobium nobile, includes the following steps: to carry out multiple broken wall treatment after dendrobium nobile is freeze-dried by (1), obtains dendrobe powder；(2) using ethyl alcohol as Extraction solvent, the pH=3-6 that hydrochloric acid adjusts mixed solvent is added, ultrasonic extraction after dendrobe powder is impregnated is added, is collected by filtration to obtain the first filtrate and the first filter residue；(3) hydrochloric acid solution is added into the first filter residue to impregnate, distilled water heating water bath is added, is collected by filtration to obtain the second filtrate and the second filter residue；(4) the second filter residue is continued to add water to cook, is collected by filtration to obtain third filtrate；(5) pH to 7.6-8, chloroform extraction are adjusted after mixing the first filtrate, the second filtrate and third filtrate, then merging filtrate crystallizes chloroform evaporated up to the dendrobine to doing.The present invention uses multiple extraction process, penetrates into dendrobe powder in solvent, is more advantageous to the dissolution of dendrobine, shortens extraction time, improves the recovery rate of dendrobine.
Description
Technical field
The present invention relates to Chinese medicine processing technique fields, and in particular to a kind of side that high-purity dendrobine is extracted from dendrobium nobile
Method.
Background technique
Dendrobium nobile, also known as celestial dry measure used in former times orchid rhythm, not dead grass, whorlleaf stonecrop herb, are a kind of rare common Chinese herbal medicines, be known as " a thousand pieces of gold grass " it
Claim, with impairment of yin body fluid deficiency, dry polydipsia, the after being ill dark unknown effect of abnormal heat, mesh, is known as first of Chinese nine big mesonas.Dendrobium nobile
In contain dendrobium polysaccharide, dendrobine, dendrophnol, dendramine, amino acid, also contain special luxuriant and rich with fragrance class, bibenzyl anticancer component, tool
There is the effects of antitumor, hypoglycemic, antibacterial, anti-aging, anti-cancer, anticancer, analgesic are brought down a fever.
Dendrobine is most important active constituent in dendrobium nobile medicinal material, have the effects that analgesic, it is antipyretic, antitumor, can reduce
Heart rate, blood pressure slow down breathing, research and development value with higher.The Technical comparing for extracting dendrobine at present is few, and extraction side
Method is comparatively laborious, and reagent loss amount is bigger, and ideal purpose is not achieved in yield, and purity compares lower.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above, provide it is a kind of it is easy to operate, recovery rate is high from dendrobium nobile
The middle method for extracting high-purity dendrobine.
In order to solve the above-mentioned technical problem, the technical solution of the present invention is as follows:
A method of it extracting high-purity dendrobine from dendrobium nobile, specifically comprises the following steps:
(1) dendrobium nobile removal impurity is cleaned up, is then freeze-dried, multiple broken wall treatment is carried out to dendrobium nobile after dry,
Obtain dendrobe powder；
(2) using the ethyl alcohol of volumetric concentration 60-90% as Extraction solvent, it is molten that hydrochloric acid adjusting mixing is added into Extraction solvent
Step (1) described dendrobe powder is added in the pH=3-6 of agent, after 30-40 DEG C of immersion 10-30min, ultrasonic extraction 2-10min, and mistake
Filter collects and obtains the first filtrate, and the first filter residue is stand-by；
(3) hydrochloric acid solution is added into the first filter residue obtained by step (2) and impregnates 20-40min, distilled water, water is then added
Bath heating 30-50min, is collected by filtration to obtain the second filtrate, the second filter residue is stand-by；
(4) the second filter residue is continued to add water to cook 10-20min, repeats 1-2 times, is collected by filtration to obtain third filtrate；
(5) NaOH is added after mixing the first filtrate, the second filtrate and third filtrate and adjusts pH to 7.6-8, isometric chlorine
Then chloroform evaporated is repeated and is operated 2-3 times to doing by imitative extraction 2-3 times, merging filtrate, addition dehydrated alcohol dissolution, and -20
DEG C crystallization is placed, the dendrobine crystal of precipitation is repeated to crystallization in ether twice up to the dendrobine.
Preferably, the dendrobium nobile is HERBA DENDROBII, any one in dendrobium candidum, preferably HERBA DENDROBII.
Preferably, step (1) freeze-drying is the dry 1-3h at -30--40 DEG C, vacuum degree 50-80Pa.
Preferably, the mass concentration of step (2) described hydrochloric acid is 5-10%.
Preferably, step (2) dendrobe powder and mixed solvent are sufficiently mixed by solid-liquid ratio for 1:10-20g/ml.
Preferably, step (2) ultrasonic power is 600-800W, and ultrasonic temperature is 40-50 DEG C.
Preferably, step (3) first filter residue: hydrochloric acid solution is that 1:10-20g/ml is sufficiently mixed by solid-liquid ratio.
Preferably, step (3) first filter residue: the solid-liquid ratio of distilled water is 1:20-30g/ml.
Preferably, step (4) amount of water is 5-7 times of the second filter residue total weight.
Compared with prior art the beneficial effects of the present invention are:
(1) present invention dendrobium nobile is freeze-dried, broken wall and ultrasonic treatment, initial physical breaking apart has been carried out to cell wall
It is released a part of total dendrobine, improves the recovery rate of dendrobine.
(2) present invention uses multiple extraction process, will carry out broken dendrobe powder after the freeze-drying of dendrobium nobile raw material, then into
Row impregnates certain time, and acidic mixed Extraction solvent can be fully penetrated into dendrobium nobile fine particle, is easier to dendrobine at salt
It is dissolved in mixing Extraction solvent, dendrobine is dissolved faster in the mixed solvent, is conducive to the extraction of subsequent dendrobine；Then it carries out
Ultrasonic extraction is that dendrobe powder penetrates into solvent, is more advantageous to the dissolution of dendrobine, shortens extraction time, improves dendrobine
Recovery rate.
(3) dendrobine is extracted using present invention process, recovery rate is high, and the purity of dendrobine is up to 95% or more.
Specific embodiment
Specific embodiments of the present invention will be further explained below.It should be noted that for these implementations
The explanation of mode is used to help understand the present invention, but and does not constitute a limitation of the invention.In addition, invention described below
Technical characteristic involved in each embodiment can be combined with each other as long as they do not conflict with each other.
Embodiment 1
A method of it extracting high-purity dendrobine from dendrobium nobile, specifically comprises the following steps:
(1) HERBA DENDROBII removal impurity is cleaned up, then at -30 DEG C, vacuum degree 50Pa, is freeze-dried 3h, it is dry
Multiple broken wall treatment is carried out to dendrobium nobile afterwards, obtains dendrobe powder；
(2) using the ethyl alcohol of volumetric concentration 60% as Extraction solvent, the salt that mass concentration is 5% is added into Extraction solvent
The solid-liquid ratio of the pH=3 of acid adjusting mixed solvent, addition step (1) described 100g dendrobe powder, dendrobe powder and mixed solvent is 1:
10g/ml is 600W in power after 30 DEG C of immersion 30min, and temperature is 40 DEG C of ultrasonic extraction 10min, is collected by filtration to obtain the
One filtrate, the first filter residue are stand-by；
It (3) is that hydrochloric acid solution immersion 20min is added in 1:10g/ml by solid-liquid ratio into the first filter residue obtained by step (2), so
Press the first filter residue afterwards: the solid-liquid ratio of distilled water is that 1:20g/ml is added distilled water, heating water bath 30min, is collected by filtration to obtain the
Two filtrates, the second filter residue are stand-by；
(4) the second filter residue is continued plus 5 times of water decocts 10min, be repeated 1 times, be collected by filtration to obtain third filtrate；
(5) NaOH is added after mixing the first filtrate, the second filtrate and third filtrate and adjusts pH to 7.6, isometric chloroform
Then chloroform evaporated is repeated operation 2 times to doing by extraction 2 times, merging filtrate, dehydrated alcohol dissolution, -20 DEG C of placements are added
The dendrobine crystal of precipitation is repeated crystallization twice up to the dendrobine 0.54g by crystallization in ether.
Use the purity of the dendrobine of the present embodiment method acquisition for 95.5%.
Embodiment 2
A method of it extracting high-purity dendrobine from dendrobium nobile, specifically comprises the following steps:
(1) HERBA DENDROBII removal impurity is cleaned up, then at -35 DEG C, vacuum degree 70Pa, is freeze-dried 2h, it is dry
Multiple broken wall treatment is carried out to dendrobium nobile afterwards, obtains dendrobe powder；
(2) using the ethyl alcohol of volumetric concentration 80% as Extraction solvent, the salt that mass concentration is 8% is added into Extraction solvent
The solid-liquid ratio of the pH=5 of acid adjusting mixed solvent, addition step (1) described 100g dendrobe powder, dendrobe powder and mixed solvent is 1:
15g/ml is 700W in power after 35 DEG C of immersion 20min, and temperature is 45 DEG C of ultrasonic extraction 6min, is collected by filtration to obtain first
Filtrate, the first filter residue are stand-by；
It (3) is that hydrochloric acid solution immersion 30min is added in 1:15g/ml by solid-liquid ratio into the first filter residue obtained by step (2), so
Press the first filter residue afterwards: the solid-liquid ratio of distilled water is that 1:25g/ml is added distilled water, heating water bath 40min, is collected by filtration to obtain the
Two filtrates, the second filter residue are stand-by；
(4) the second filter residue is continued plus 6 times of water decocts 15min, be repeated 1 times, be collected by filtration to obtain third filtrate；
(5) NaOH is added after mixing the first filtrate, the second filtrate and third filtrate and adjusts pH to 8, isometric chloroform extraction
It takes 3 times, merging filtrate, chloroform evaporated is then repeated into operation 2 times to doing, dehydrated alcohol dissolution, -20 DEG C of placements knots are added
The dendrobine crystal of precipitation is repeated crystallization twice up to the dendrobine 0.55g by crystalline substance in ether.
Use the purity of the dendrobine of the present embodiment method acquisition for 97.3%.
Embodiment 3
A method of it extracting high-purity dendrobine from dendrobium nobile, specifically comprises the following steps:
(1) HERBA DENDROBII removal impurity is cleaned up, then at -40 DEG C, vacuum degree 80Pa, is freeze-dried 1h, it is dry
Multiple broken wall treatment is carried out to dendrobium nobile afterwards, obtains dendrobe powder；
(2) using the ethyl alcohol of volumetric concentration 90% as Extraction solvent, it is 10% that mass concentration is added into Extraction solvent
Hydrochloric acid adjusts the pH=6 of mixed solvent, and step (1) described 100g dendrobe powder is added, and the solid-liquid ratio of dendrobe powder and mixed solvent is
1:20g/ml is 800W in power after 40 DEG C of immersion 10min, and temperature is 50 DEG C of ultrasonic extraction 2min, is collected by filtration to obtain the
One filtrate, the first filter residue are stand-by；
It (3) is that hydrochloric acid solution immersion 40min is added in 1:20g/ml by solid-liquid ratio into the first filter residue obtained by step (2), so
Press the first filter residue afterwards: the solid-liquid ratio of distilled water is that 1:30g/ml is added distilled water, heating water bath 50min, is collected by filtration to obtain the
Two filtrates, the second filter residue are stand-by；
(4) the second filter residue is continued plus 7 times of water decocts 20min, be repeated 2 times, be collected by filtration to obtain third filtrate；
(5) NaOH is added after mixing the first filtrate, the second filtrate and third filtrate and adjusts pH to 8, isometric chloroform extraction
It takes 2 times, merging filtrate, chloroform evaporated is then repeated into operation 3 times to doing, dehydrated alcohol dissolution, -20 DEG C of placements knots are added
The dendrobine crystal of precipitation is repeated crystallization twice up to the dendrobine 0.49g by crystalline substance in ether.
Use the purity of the dendrobine of the present embodiment method acquisition for 96.2%.
The above are present pre-ferred embodiments, it is only applicable to the principle for helping to understand the embodiment of the present invention；Meanwhile for this
The those skilled in the art in field, according to the present embodiment, there will be changes in terms of specific embodiments and scope of application, comprehensive
Upper described, the contents of this specification are not to be construed as limiting the invention.
Claims (8)
1. a kind of method for extracting high-purity dendrobine from dendrobium nobile, feature exist: specifically comprising the following steps:
(1) dendrobium nobile removal impurity is cleaned up, is then freeze-dried, multiple broken wall treatment is carried out to dendrobium nobile after dry, is obtained
Dendrobe powder；
(2) using the ethyl alcohol of volumetric concentration 60-90% as Extraction solvent, hydrochloric acid is added into Extraction solvent and adjusts mixed solvent
Step (1) described dendrobe powder is added in pH=3-6, and after 30-40 DEG C of immersion 10-30min, ultrasonic extraction 2-10min, filtering is received
Collection obtains the first filtrate, and the first filter residue is stand-by；
(3) hydrochloric acid solution is added into the first filter residue obtained by step (2) and impregnates 20-40min, distilled water is then added, water-bath adds
Hot 30-50min is collected by filtration to obtain the second filtrate, and the second filter residue is stand-by；
(4) the second filter residue is continued to add water to cook 10-20min, repeats 1-2 times, is collected by filtration to obtain third filtrate；
(5) NaOH is added after mixing the first filtrate, the second filtrate and third filtrate and adjusts pH to 7.6-8, isometric chloroform extraction
It takes 2-3 times, merging filtrate, chloroform evaporated is then repeated into operation 2-3 times to doing, dehydrated alcohol dissolution is added, -20 DEG C put
Crystallization is set, the dendrobine crystal of precipitation is repeated to crystallization in ether twice up to the dendrobine.
2. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (1) institute
Stating freeze-drying is the dry 1-3h at -30--40 DEG C, vacuum degree 50-80Pa.
3. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (2) institute
The mass concentration for stating hydrochloric acid is 5-10%.
4. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (2) institute
It is that 1:10-20g/ml is sufficiently mixed that dendrobe powder and mixed solvent, which are stated, by solid-liquid ratio.
5. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (2) institute
Stating ultrasonic power is 600-800W, and ultrasonic temperature is 40-50 DEG C.
6. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (3) institute
State the first filter residue: hydrochloric acid solution is that 1:10-20g/ml is sufficiently mixed by solid-liquid ratio.
7. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (3) institute
State the first filter residue: the solid-liquid ratio of distilled water is 1:20-30g/ml.
8. the method according to claim 1 for extracting high-purity dendrobine from dendrobium nobile, it is characterised in that: step (4) institute
State 5-7 times that amount of water is the second filter residue total weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811574062.8A CN109705128A (en) | 2018-12-21 | 2018-12-21 | A method of extracting high-purity dendrobine from dendrobium nobile |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811574062.8A CN109705128A (en) | 2018-12-21 | 2018-12-21 | A method of extracting high-purity dendrobine from dendrobium nobile |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109705128A true CN109705128A (en) | 2019-05-03 |
Family
ID=66256035
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811574062.8A Pending CN109705128A (en) | 2018-12-21 | 2018-12-21 | A method of extracting high-purity dendrobine from dendrobium nobile |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109705128A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114231382A (en) * | 2021-11-09 | 2022-03-25 | 赤水信天斛满堂药业有限公司 | Dendrobium nobile vinegar, preparation method and device |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265548A (en) * | 2013-05-23 | 2013-08-28 | 南京泽朗医药科技有限公司 | Extraction method of dendrobine |
| CN104557956A (en) * | 2014-12-24 | 2015-04-29 | 贵州师范大学 | Method for preparing dendrobine of which content is more than 95% |
| CN104844723A (en) * | 2015-06-05 | 2015-08-19 | 云南金九地生物科技有限公司 | Preparation method and application of dendrobium officinale extract |
| CN108164541A (en) * | 2018-01-18 | 2018-06-15 | 贵州独秀峰药业有限公司 | The method that dendrobine is extracted in dendrobium candidum |
| CN108693265A (en) * | 2018-05-16 | 2018-10-23 | 遵义医学院 | The extraction and purifying of HERBA DENDROBII total alkaloid and content assaying method |
-
2018
- 2018-12-21 CN CN201811574062.8A patent/CN109705128A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265548A (en) * | 2013-05-23 | 2013-08-28 | 南京泽朗医药科技有限公司 | Extraction method of dendrobine |
| CN104557956A (en) * | 2014-12-24 | 2015-04-29 | 贵州师范大学 | Method for preparing dendrobine of which content is more than 95% |
| CN104844723A (en) * | 2015-06-05 | 2015-08-19 | 云南金九地生物科技有限公司 | Preparation method and application of dendrobium officinale extract |
| CN108164541A (en) * | 2018-01-18 | 2018-06-15 | 贵州独秀峰药业有限公司 | The method that dendrobine is extracted in dendrobium candidum |
| CN108693265A (en) * | 2018-05-16 | 2018-10-23 | 遵义医学院 | The extraction and purifying of HERBA DENDROBII total alkaloid and content assaying method |
Non-Patent Citations (2)
| Title |
|---|
| 徐德林，等: "不同产地的铁皮石斛和金钗石斛石斛多糖、石斛碱、氨基酸含量的比较", 《时珍国医国药》 * |
| 李志平，等: "不同附生树种对金钗石斛石斛碱含量的影响", 《安徽农业科学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114231382A (en) * | 2021-11-09 | 2022-03-25 | 赤水信天斛满堂药业有限公司 | Dendrobium nobile vinegar, preparation method and device |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104829743B (en) | A kind of preparation method and its usage of Polysaccharides from Leaves of Moringa oleifera | |
| CN102875562B (en) | Method for preparing psoralen and isopsoralen or extract containing psoralen and isopsoralen | |
| CN103145660A (en) | Andrographolide and preparation method thereof | |
| CN103896890B (en) | A kind of extraction process of rographolide | |
| CN102964466A (en) | Abelmoschus manihot polysaccharide with anti-tumor activity and preparation method thereof | |
| CN103340841B (en) | A kind of Chinese medicine membrane, Preparation Method And The Use | |
| CN103304576A (en) | Method for extracting artemisinin through enzymatic hydrolysis | |
| CN106831808A (en) | A kind of technique of the rapid extraction eurycomanone from Tongkat Ali | |
| CN102688276B (en) | Extraction method for rhodiola rosea injection with assistance of microwave cell disruption | |
| CN107823400A (en) | A kind of QI invigorating, which rises, falls into ball and preparation method thereof | |
| CN109010615A (en) | The preparation method of cold soluble type dendrobium candidum extract | |
| CN109705128A (en) | A method of extracting high-purity dendrobine from dendrobium nobile | |
| CN104513218B (en) | A kind of method of petunidin in high speed adverse current chromatogram separation black fruit fructus lycii | |
| CN105168376A (en) | Method for extracting and gathering total alkaloids of hypecoum leptocarpum | |
| CN107098942A (en) | A kind of method of kaempferia galamga glycosides in Subcritical Water Extraction radish leaves | |
| CN104098634A (en) | Technology for jointly extracting synephrine, hesperidin and PMFs (polymethoxy latednavones) from fructus aurantii immaturus | |
| CN104926719B (en) | A kind of method that trigonelline is extracted from fructus cannabis | |
| CN112266399B (en) | High-purity separation and extraction method of epimedium extract | |
| CN105327148B (en) | The preparation method of dendrobium nobile cream | |
| CN101973856A (en) | Process for extracting schizandrin A from schizandra | |
| CN103585208B (en) | Preparation method of high-quality andrographolide component | |
| CN103800418B (en) | Composition for promoting blood circulation and stopping pain, capsule preparation technology and application thereof | |
| CN108864219A (en) | A kind of method of High-pressure supercritical carbon dioxide abstraction Gastrodin | |
| CN103524578A (en) | Method for extraction and separation of paeoniflorin compounds from stamens of peony | |
| CN109512935B (en) | Cape jasmine-ophiopogon root tablet for clearing internal heat and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190503 |