CN102093214A - Method for preparing Buddledin A - Google Patents
Method for preparing Buddledin A Download PDFInfo
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- CN102093214A CN102093214A CN2010105541640A CN201010554164A CN102093214A CN 102093214 A CN102093214 A CN 102093214A CN 2010105541640 A CN2010105541640 A CN 2010105541640A CN 201010554164 A CN201010554164 A CN 201010554164A CN 102093214 A CN102093214 A CN 102093214A
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- buddledin
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- ethanol
- reflux
- decompression
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to a method for preparing Buddledin A, which is simple and convenient in operation, low in pollution and low in energy consumption. The method for preparing the Buddledin A comprises the following technological steps of: adding 60 to 80 percent ethanol into Buddleja davidii franch. leaf to perform reflux under heating; merging the reflux solution; filtering; recovering ethanol under reduced pressure and concentrating; performing multi-level countercurrent extraction by using an ethyl acetate-water mixed solvent according to the ratio of ethyl acetate to water of 10:2; merging extract liquid; recovering the solvent under reduced pressure; adding on a macroporous absorption resin column to perform absorption; performing elution by using ethanol; collecting eluent; recovering the solvent under reduced pressure; adding methanol to crystallize; performing fractional crystallization; and washing and drying to obtain the Buddledin A. The Buddledin A prepared by the method has high purity and realizes industrialized amplification easily.
Description
Technical field
The present invention relates to the preparation method of a kind of buddledin A, especially a kind of preparation method who from plant, extracts buddledin A.
Background technology
Buddledin A (Buddledin A), molecular formula: C
17H
24O
3, molecular weight: 276.375, CAS accession number: 62346-20-7.Mainly be present in the Buddlejaceae various plants, wherein content is higher in the Buddlejaceae plant butterfly bush Buddleja davidii Franch. leaf, and raw material sources are abundant.Its molecular formula is as follows:
Modern study shows that buddledin A has antimycotic, malicious fish isoreactivity, and it is also as the raw material that synthesizes other reactive derivative simultaneously.
Buddlejaceae plant butterfly bush Buddleja davidii Franch. leaf is used as the Chinese medicine orangeeye butterflybush branchlet and leaf or root-bark and uses, and has effects such as expelling wind and cold, promoting blood circulation and stopping pain, detoxifcation desinsection.
In the prior art, still be not applicable to preparation technology's report of high purity buddledin A industrialized production.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method who is beneficial to big production operation, buddledin A that product purity is high.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get the butterfly bush leaf, add its quality 8-12 and doubly measure 60-80% alcohol heating reflux 1-3 time of volume, each 1-2 hour, merge phegma, filter, decompression recycling ethanol also concentrates, and is that ethyl acetate-water mixed solvent of 10: 2 carries out the 4-8 stage countercurrent and extracts combining extraction liquid with ratio, decompression and solvent recovery, join on the macroporous adsorptive resins and adsorb, the 30-50% ethanol elution is collected 3-8 and is doubly measured the column volume elutriant, decompression and solvent recovery, add methanol crystallization, fractional crystallization washs, is drying to obtain.
Reflux is preferably 70% with concentration of ethanol, and consumption is preferably 10 times of amount volumes of raw materials quality.
The number of times of reflux is preferably 2 times, each 1.5 hours.
The progression of counter-current extraction is preferably 6 grades
Macroporous adsorbent resin is selected from a kind of in D101 type, D102 type, the AB8 type macroporous adsorbent resin.
The macroporous adsorbent resin wash-out is preferably 40% with concentration of ethanol.
The collecting amount of macroporous adsorbent resin elutriant is preferably 5 times of amount column volumes.
Preparation gained buddledin A can adopt following method to detect:
Test example 1 HPLC method is measured buddledin A purity
Chromatographic condition
Chromatographic column: octadecylsilane bonding glue silica gel is weighting agent; Moving phase: methanol-water solution (90: 10); Flow velocity: 1.0mL/min; Detect wavelength: 280nm; Column temperature: 30 ℃.
Measuring method
Precision takes by weighing buddledin A2mg, places the 50mL measuring bottle, adds people's methyl alcohol 20mL, and sonic oscillation makes dissolving, and methanol constant volume is drawn 10 μ L to scale, injects high performance liquid chromatograph, adopts normalization method working sample purity.
Adopt the present invention to prepare buddledin A, be beneficial to big production operation, energy consumption is little, pollutes little.
The present invention is further elaborated below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1
Get butterfly bush leaf 10Kg, 60% alcohol heating reflux of adding 80L 1 time, 1 hour, fetch flow liquid, filter, decompression recycling ethanol also concentrates, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 4 stage countercurrents, combining extraction liquid, decompression and solvent recovery, join on the D101 type macroporous adsorptive resins and adsorb, 30% ethanol elution is collected 3 times of amount column volume elutriants, decompression and solvent recovery, add methanol crystallization, fractional crystallization washs, is drying to obtain colourless platelet buddledin A45.8g, detects through HPLC, purity is 94.3%, UV, IR, MS,
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 2
Get butterfly bush leaf 10Kg, 80% alcohol heating reflux of adding 120L 3 times, each 2 hours, merge phegma, filter, decompression recycling ethanol also concentrates, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 8 stage countercurrents, combining extraction liquid, decompression and solvent recovery, join on the D102 type macroporous adsorptive resins and adsorb, 50% ethanol elution is collected 8 times of amount column volume elutriants, decompression and solvent recovery, add methanol crystallization, fractional crystallization, washing, be drying to obtain colourless platelet buddledin A51.3g, detect through HPLC, purity is 93.3%, UV, IR, MS;
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Embodiment 3
Get butterfly bush leaf 10Kg, 70% alcohol heating reflux of adding 100L 2 times, each 1.5 hours, merge phegma, filter, decompression recycling ethanol also concentrates, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 6 stage countercurrents, combining extraction liquid, decompression and solvent recovery, join on the macroporous adsorptive resins and adsorb, 40% ethanol elution is collected 5 times of amount column volume elutriants, decompression and solvent recovery, add methanol crystallization, fractional crystallization washs, is drying to obtain colourless platelet buddledin A46.9g, detects through HPLC, purity is 98.3%, UV, IR, MS,
2HNMR,
13The data of its physical behavior of sign such as CNMR are consistent with prior art.
Claims (7)
1. the preparation method of a buddledin A, it is characterized in that described method is made up of the following step: get the butterfly bush leaf, add its quality 8-12 and doubly measure 60-80% alcohol heating reflux 1-3 time of volume, each 1-2 hour, merge phegma, filter, decompression recycling ethanol also concentrates, with ratio is that ethyl acetate-water mixed solvent of 10: 2 carries out the extraction of 4-8 stage countercurrent, combining extraction liquid, decompression and solvent recovery joins on the macroporous adsorptive resins and adsorbs, the 30-50% ethanol elution, collect 3-8 and doubly measure the column volume elutriant, decompression and solvent recovery adds methanol crystallization, fractional crystallization, washing, be drying to obtain.
2. according to the preparation method of the described a kind of buddledin A of claim 1, it is characterized in that described reflux concentration of ethanol is 70%, consumption is 10 times of amount volumes of raw materials quality.
3. according to the preparation method of the described a kind of buddledin A of claim 1, the number of times that it is characterized in that described reflux is 2 times, each 1.5 hours.
4. according to the preparation method of the described a kind of buddledin A of claim 1, the progression that it is characterized in that described counter-current extraction is 6 grades.
5. according to the preparation method of the described a kind of buddledin A of claim 1, it is characterized in that described macroporous adsorbent resin is selected from a kind of in D101 type, D102 type, the AB8 type macroporous adsorbent resin.
6. according to the preparation method of the described a kind of buddledin A of claim 1, it is characterized in that described macroporous adsorbent resin wash-out concentration of ethanol is 40%.
7. according to the preparation method of the described a kind of buddledin A of claim 1, the collecting amount that it is characterized in that described macroporous adsorbent resin elutriant is 5 times of amount column volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105541640A CN102093214A (en) | 2010-11-23 | 2010-11-23 | Method for preparing Buddledin A |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105541640A CN102093214A (en) | 2010-11-23 | 2010-11-23 | Method for preparing Buddledin A |
Publications (1)
| Publication Number | Publication Date |
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| CN102093214A true CN102093214A (en) | 2011-06-15 |
Family
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| Application Number | Title | Priority Date | Filing Date |
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| CN2010105541640A Pending CN102093214A (en) | 2010-11-23 | 2010-11-23 | Method for preparing Buddledin A |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991024A (en) * | 2018-07-21 | 2018-12-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of technique that effective component in Lindley Butterflybush Herb is enriched with by solvent extraction method |
| CN109042571A (en) * | 2018-09-21 | 2018-12-21 | 泉州黄章智能科技有限公司 | A kind of Lindley Butterflybush Herb bait |
| CN109498521A (en) * | 2018-12-23 | 2019-03-22 | 广州素颜皮肤管理科技有限公司 | It is a kind of to have effects that the plant extracts of antiallergy and its application |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1969954A (en) * | 2005-08-10 | 2007-05-30 | 郑乐建 | Use of lindley butterflybush root in preparation of medicament for treating acute and chronic gastroenteritis |
-
2010
- 2010-11-23 CN CN2010105541640A patent/CN102093214A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1969954A (en) * | 2005-08-10 | 2007-05-30 | 郑乐建 | Use of lindley butterflybush root in preparation of medicament for treating acute and chronic gastroenteritis |
Non-Patent Citations (2)
| Title |
|---|
| 张海平，陶靓: "巴东醉鱼草化学成分的研究(II)", 《中药材》, vol. 33, no. 6, 30 June 2010 (2010-06-30), pages 922 - 924 * |
| 李治伟等: "巴东醉鱼草不同方法提取物的杀虫活性", 《西北农业学报》, vol. 18, no. 5, 31 December 2009 (2009-12-31), pages 109 - 112 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108991024A (en) * | 2018-07-21 | 2018-12-14 | 安溪县凤城建金产品外观设计服务中心 | A kind of technique that effective component in Lindley Butterflybush Herb is enriched with by solvent extraction method |
| CN109042571A (en) * | 2018-09-21 | 2018-12-21 | 泉州黄章智能科技有限公司 | A kind of Lindley Butterflybush Herb bait |
| CN109498521A (en) * | 2018-12-23 | 2019-03-22 | 广州素颜皮肤管理科技有限公司 | It is a kind of to have effects that the plant extracts of antiallergy and its application |
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Application publication date: 20110615 |