CN104557956A - Method for preparing dendrobine of which content is more than 95% - Google Patents
Method for preparing dendrobine of which content is more than 95% Download PDFInfo
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- CN104557956A CN104557956A CN201410816877.8A CN201410816877A CN104557956A CN 104557956 A CN104557956 A CN 104557956A CN 201410816877 A CN201410816877 A CN 201410816877A CN 104557956 A CN104557956 A CN 104557956A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D491/00—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
- C07D491/02—Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains two hetero rings
- C07D491/08—Bridged systems
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Abstract
The invention discloses a method for preparing dendrobine of which the content is more than 95%. The method comprises the following steps: step 1, acquiring dendrobium stems, adding an ethanol solution to the dendrobium stems for reflux extraction, adding ethanol solution again for reflux extraction, and combining extraction solutions, and concentrating the combined extraction solutions so as to obtain pasty extracts; step 2, adding an HCl solution to the pasty extracts, stirring the HCl solution and the pasty extracts, extracting dendrobine, and leaching the dendrobine so as to obtain an HCl extraction solution; step 3, repeating the step 2 until no alkaloid is detected in the HCl extraction solution; step 4, performing chloroform extraction on the HCl extraction solution for three times, alkalizing the HCl extraction solution by ammonium hydroxide until the pH value of the HCl extraction solution is 8, and performing chloroform extraction on the alkalized HCI extraction solution to obtain dendrobine; step 5, evaporating the chloroform, and retreating the step 2, step 3 and the step 4, and then evaporating the chloroform again to obtain crude dendrobine; step 6, dissolving the crude dendrobine in a small volume of ethyl ether, placing the ethyl ether with the crude dendrobine under minus 20 DEG C for crystallization, and repeating crystallization on the precipitated dendrobine crystals in the ethyl ether twice so as to obtain refined dendrobine of which the content is more than 95%. The method disclosed by the invention is simple and easy to operate, low in cost, environment-friendly, and high in purification efficiency.
Description
Technical field
The invention belongs to field of natural medicinal chemistry, be specifically related to a kind of method of purification of dendrobine.
Background technology
At present, the domestic preparation about dendrobine stays in the optimization of extraction conditions mostly, as the optimization of the conditions such as organic solvent extraction, enzyme process assisted extraction, ultrasonic-assisted extraction, co_2 supercritical fluid extraction, and does not do further purification work; Enzyme process assisted extraction needs to consume expensive biological catalyst enzyme, and cost is increased; Ultrasonic wave or microwave―assisted extraction also have particular requirement to equipment, not easily amplify; The disposable input of co_2 supercritical fluid extraction device is comparatively large, and cost is increased.What some documents and patent related to dendrobine is further purified technology, but need to use ion exchange chromatography and silica gel column chromatography or even preparative high performance liquid chromatography, the consumables cost of chromatographic separation is high, operational requirement is high, consuming time, particularly the production cost of HPLC is the highest.
Summary of the invention
An object of the present invention extracts that consumables cost is high, operational requirement is high, consuming time, production cost is a high difficult problem for solving dendrobine, provides that a kind of method is simple, easy to operate, cost is low, environmental friendliness and the high method preparing content more than 95% dendrobine of purification efficiency.
The invention provides a kind of method preparing content more than 95% dendrobine, comprise following steps:
S1: get certain mass dendrobium stem stem section, add the ethanolic soln refluxing extraction 3h-5h of 6-10 times of volume, then with 4-6 times of volume ethanolic soln refluxing extraction 3h-5h, united extraction liquid also concentrated to obtain paste extract;
S2: the 2%HCl solution stirring described paste extract being added to two volumes extracts dendrobine, and drop goes out to obtain HCl extracting solution;
Alkaloid is can't detect in S3: repeating said steps S2 to described HCl extracting solution;
S4: HCl extracting solution described in chloroform extraction 3 times, extracts dendrobine to the rear chloroform of pH 8 by described HCl extracting solution alkalization with ammoniacal liquor from extracting solution;
S5: evaporate to dryness chloroform, repeating said steps S2, S3 and S4, obtain the dendrobine crude product of content more than 80.0% again after evaporate to dryness chloroform;
S6: the dendrobine crude product of described content more than 80.0% is dissolved in the ether of small volume, and place crystallization in-20 DEG C, the dendrobine crystal of precipitation is repeated in ether crystallization and namely obtain content more than 95% dendrobine fine work twice.
Further, described ethanol solution concentration is 70%-90%.
Further, detect alkaloid method in described step S3 and adopt thin layer plate detection method.
Beneficial effect of the present invention is, uses a kind of method preparing content more than 95% dendrobine provided by the invention namely to obtain dendrobine fine work when not relying on chromatographic technique by carrying out 3 recrystallizations in ether.The method is simple, easy to operate, cost is low, environmental friendliness and purification efficiency is high.
Embodiment
Hereafter in detail the specific embodiment of the invention will be described.It should be noted that the combination of technical characteristic or the technical characteristic described in following embodiment should not be considered to isolated, they can mutually be combined thus be reached better technique effect.
The invention provides a kind of method preparing content more than 95% dendrobine, comprise following steps:
S1: get certain mass dendrobium stem stem section, add the ethanolic soln refluxing extraction 3h-5h of 6-10 times of volume, then with 4-6 times of volume ethanolic soln refluxing extraction 3h-5h, united extraction liquid also concentrated to obtain paste extract;
S2: the 2%HCl solution stirring described paste extract being added to two volumes extracts dendrobine, and drop goes out to obtain HCl extracting solution;
Alkaloid is can't detect in S3: repeating said steps S2 to described HCl extracting solution;
S4: HCl extracting solution described in chloroform extraction 3 times, extracts dendrobine to the rear chloroform of pH 8 by described HCl extracting solution alkalization with ammoniacal liquor from extracting solution;
S5: evaporate to dryness chloroform, repeating said steps S2, S3 and S4, obtain the dendrobine crude product of content more than 80.0% again after evaporate to dryness chloroform;
S6: the dendrobine crude product of described content more than 80.0% is dissolved in the ether of small volume, and place crystallization in-20 DEG C, the dendrobine crystal of precipitation is repeated in ether crystallization and namely obtain content more than 95% dendrobine fine work twice.
Further, described ethanol solution concentration is 70%-90%.
Further, detect alkaloid method in described step S3 and adopt thin layer plate detection method.
Embodiment:
Get 1kg dendrobium stem stem section dried powder and cross 20 orders, add the alcohol reflux 3h of 10L 70%, then use the alcohol reflux 3h of 4L 70%, united extraction liquid is also concentrated into paste; Stir from ethanol extract with the 2%HCl solution of two volumes and extract dendrobine, repeat to extract once; Chloroform extraction 2%HCl extracting solution 3 times; With ammoniacal liquor, the alkalization of HCl extracting solution is extracted dendrobine to the rear chloroform of pH 8 from extracting solution; After evaporate to dryness chloroform, the 2%HCl solution again adding two volumes in extract extracts dendrobine; With chloroform extraction 2%HCl extracting solution removing impurity; Use chloroform extraction dendrobine after liquid ammonia alkalinization to pH 8, again after evaporate to dryness chloroform, namely obtain the dendrobine crude product 3.43g that content is 81.4%.
The 3.43g dendrobine crude product of acquisition is dissolved in the ether of small volume, and places crystallization in-20 DEG C, the dendrobine crystal of precipitation is repeated in ether crystallization and namely obtain the dendrobine fine work 0.597g that purity is 96.1% twice.
A kind of method preparing content more than 95% dendrobine provided by the invention is used namely to obtain dendrobine fine work when not relying on chromatographic technique by carrying out 3 recrystallizations in ether.The method is simple, easy to operate, cost is low, environmental friendliness and purification efficiency is high.
Although give some embodiments of the present invention, it will be understood by those of skill in the art that without departing from the spirit of the invention herein, can change embodiment herein.Above-described embodiment is exemplary, should using embodiment herein as the restriction of interest field of the present invention.
Claims (3)
1. prepare a method for content more than 95% dendrobine, it is characterized in that, comprise following steps:
S1: get certain mass dendrobium stem stem section, add the ethanolic soln refluxing extraction 3h-5h of 6-10 times of volume, then with 4-6 times of volume ethanolic soln refluxing extraction 3h-5h, united extraction liquid also concentrated to obtain paste extract;
S2: the 2%HCl solution stirring described paste extract being added to two volumes extracts dendrobine, and drop goes out to obtain HCl extracting solution;
Alkaloid is can't detect in S3: repeating said steps S2 to described HCl extracting solution;
S4: HCl extracting solution described in chloroform extraction 3 times, extracts dendrobine with described chloroform by described HCl extracting solution alkalization with ammoniacal liquor to pH 8 from extracting solution;
S5: chloroform described in evaporate to dryness, repeating said steps S2, S3 and S4, obtain the dendrobine crude product of content more than 80.0% again after chloroform described in evaporate to dryness;
S6: the dendrobine crude product of described content more than 80.0% is dissolved in the ether of small volume, and place crystallization in-20 DEG C, the dendrobine crystal of precipitation is repeated in ether crystallization and namely obtain content more than 95% dendrobine fine work twice.
2. a kind of method preparing content more than 95% dendrobine as claimed in claim 1, it is characterized in that, described ethanol solution concentration is 70%-90%.
3. a kind of method preparing content more than 95% dendrobine as claimed in claim 1, is characterized in that, detects alkaloid method and adopt thin layer plate detection method in described step S3.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107441047A (en) * | 2017-09-06 | 2017-12-08 | 遵义医学院附属医院 | A kind of preparation method of the dendrobine liposome based on Active loading mode |
| CN109283269A (en) * | 2018-09-29 | 2019-01-29 | 合肥工业大学 | The analysis method of feature alkaloid composition in a kind of fresh Huoshan rice dry measure used in former times |
| CN109705128A (en) * | 2018-12-21 | 2019-05-03 | 云南金九地生物科技有限公司 | A method of extracting high-purity dendrobine from dendrobium nobile |
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| CN101735231A (en) * | 2010-01-20 | 2010-06-16 | 遵义医学院 | Method for extracting purified dendrobine from dendrobium stem |
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2014
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| CN101698059A (en) * | 2007-05-31 | 2010-04-28 | 北京和润创新医药科技发展有限公司 | Method for separating dendrobium total alkaloids by ion exchange resin |
| CN101735231A (en) * | 2010-01-20 | 2010-06-16 | 遵义医学院 | Method for extracting purified dendrobine from dendrobium stem |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107441047A (en) * | 2017-09-06 | 2017-12-08 | 遵义医学院附属医院 | A kind of preparation method of the dendrobine liposome based on Active loading mode |
| CN107441047B (en) * | 2017-09-06 | 2020-03-27 | 遵义医学院附属医院 | Preparation method of dendrobine liposome based on active drug loading mode |
| CN109283269A (en) * | 2018-09-29 | 2019-01-29 | 合肥工业大学 | The analysis method of feature alkaloid composition in a kind of fresh Huoshan rice dry measure used in former times |
| CN109705128A (en) * | 2018-12-21 | 2019-05-03 | 云南金九地生物科技有限公司 | A method of extracting high-purity dendrobine from dendrobium nobile |
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Application publication date: 20150429 |