CN101974007B - Method for extracting bergenin from traditional Chinese medicine rodgersia podophylla - Google Patents
Method for extracting bergenin from traditional Chinese medicine rodgersia podophylla Download PDFInfo
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- CN101974007B CN101974007B CN2010105211532A CN201010521153A CN101974007B CN 101974007 B CN101974007 B CN 101974007B CN 2010105211532 A CN2010105211532 A CN 2010105211532A CN 201010521153 A CN201010521153 A CN 201010521153A CN 101974007 B CN101974007 B CN 101974007B
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Abstract
The invention belongs to the field of chemical research of traditional Chinese medicine, in particular to a method for extracting bergenin from traditional Chinese medicine rodgersia podophylla. In the prior art, methanol ultrasonic is used for extracting bergenin, which is not suitable for industrial production; in addition, a method for adopting lime water wastes time. In order to overcome the defects in the prior art, the invention adopts the technical scheme that the method for extracting bergenin from traditional Chinese medicine rodgersia podophylla comprises the following steps: taking traditional Chinese medicine rodgersia podophylla coarse powder as raw material; carrying out reflux extraction on the raw material for 3 times by alcohol of which the amount is 4-6 times of that of the raw material, wherein the first time lasts for 1-3 hours, and the second time and the third time respectively last for 0.5-1.5 hours; collecting extract, precipitating and filtering; recovering filtrate, and condensing to small volume; standing for devitrification; after the devitrificated crystal is dissolved by alcohol-carbinol mixed liquid at the volume ratio of 8:1-8:3, carrying out hot filtering; and after filtering, standing for devitrification. The method has simple technology, low cost, available raw material and high extraction efficiency and is favorable for industrial production.
Description
Technical field
The invention belongs to the Chemistry for Chinese Traditional Medicine research field, relate in particular to a kind of method of from the Chinese medicinal materials Rodgersia podophylla A. Gray, extracting Bergeninum.
Background technology
Bergeninum (C
14H
10O
9), claim vakerin, bergenit again, the Bergeninum resource is extensive; Be present in five sections, nine platymisciums; The Pharmacopoeia of the People's Republic of China is received to antisussive and expectorant agent, is used for the treatment of chronic bronchitis, is that the multiple compound preparation of raw material has been used for clinical with the Bergeninum; In addition, Bergeninum can also be supplied raw materials for contrast material in the Test on Traditional Chinese Medicine.In addition, there is the bibliographical information Bergeninum to have the effect of anti-inflammatory analgesic.All contain Bergeninum in the multiple medicinal plant, but content differs just.In the prior art; How from medicinal material Japanese Ardisia Herb, Herba astilbes chinensis, Rhizome or herb of Purple Bergenia, to extract; Process for extracting mostly with water extraction and alcohol precipitation method, limewater extraction method, methyl alcohol ultrasonic extraction, also have utilize Alcoholic extraction after; Adopt ammoniacal liquor control potential of hydrogen, the acid strong tannin that molecular weight is big precipitates fully, removes the method for saccharic again with methyl alcohol ether method.Use the methyl alcohol supersound extraction, unsuitable industrial production, this process for extracting of liming is time-consuming.
Summary of the invention
In order to overcome the defective of prior art, the purpose of this invention is to provide a kind of simple to operate, with low cost, productive rate is high, be suitable for the industrial method of from the Chinese medicinal materials Rodgersia podophylla A. Gray, extracting Bergeninum.
To achieve these goals, the technical scheme of the present invention's employing is:
A kind of method of from Chinese medicinal materials ghost lamp is held up, extracting Bergeninum, said method is undertaken by following step:
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) using is the concentration doubly measured of raw material 4-6 as the methyl alcohol of 90-95% or ethanol with raw material refluxing extraction 3 times, and the time is 1-3 hour for the first time, for the second time be 0.5-1.5 hour for the third time,
3) united extraction liquid was placed 8-24 hour,
4) with 3) in place liquid and filter,
5) recovery is filtrated and is concentrated into small volume, puts to separating out crystallization.
6) use volume ratio as ethanol-methanol mixed dissolution with solvents of 8:1-8:5 crystallization after heat filtering, filter the back and place crystallization.
In the aforesaid method the 5th) the step crystallization of separating out carries out the above-mentioned the 6th after with washing with acetone again) step,
With gac with the above-mentioned the 5th) crystallization decolouring in the portion once.
Step and processing parameter are following in the aforesaid method:
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) to use the concentration of 5 times of amounts of raw material be 93% ethanol with raw material refluxing extraction 3 times, and the time is 2 hours for the first time, for the second time be 1 hour for the third time,
3) united extraction liquid was placed 24 hours,,
4) with 3) in place liquid and filter,
5) recovery is filtrated and is concentrated into small volume, puts to separating out crystallization.
6) with the 5th) the step crystallization of separating out uses washing with acetone,
7) use volume ratio as ethanol-methanol mixed dissolution with solvents of 8:3 crystallization after heat filtering, filter the back and place crystallization.
With respect to prior art, advantage of the present invention is: the present invention makes raw material extraction Bergeninum with containing the plain high Rodgersia podophylla A. Gray of Rhizome or herb of Purple Bergenia, and technology is simple; Cost is low, can well be used for industrial production, and the Bergeninum purity that extracts is up to 97%; And extraction yield is high, reaches as high as 80%.
Description of drawings
Fig. 1 is a Bergeninum reference substance mass spectrum molecular ion peak (M-1);
Fig. 2 is a crystallization mass spectrum molecular ion peak (M-1);
Fig. 3 is a reference substance Bergeninum ultraviolet spectrogram;
Fig. 4 crystallization ultraviolet spectrogram;
Fig. 5 Bergeninum reference substance, crystallization high-efficient liquid phase chromatogram.
Embodiment
Below in conjunction with embodiment the present invention is made and to further specify.
Embodiment 1:
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) using is that the concentration of 4 times of amounts of raw material is 90% methyl alcohol with raw material refluxing extraction 3 times, and the time is 1 hour for the first time, for the second time be 0.5 hour for the third time, the Bergeninum extraction yield is 60% as a result,
3) united extraction liquid is placed and is separated out the part crystal after 8 hours,
4) with 3) in place liquid and filter,
5) recovery is filtrated and is concentrated into small volume, puts to separating out crystallization.
6) use volume ratio as ethanol-methanol mixed dissolution with solvents of 8:1 crystallization after heat filtering, filter the back and place crystallization.It is fast that this process is separated out crystallization, and the solvent volume amount is relatively large.
Through above-mentioned steps, get white crystal, to measure through high-performance liquid chromatogram determination and area normalization, purity reaches more than 97%, and whole process extraction yield is 60%.
Embodiment 2:
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) using is that the concentration of 6 times of amounts of raw material is 93% ethanol with raw material refluxing extraction 3 times, and the time is 2 hours for the first time, for the second time be 1 hour for the third time, the Bergeninum extraction yield is 75% as a result,
3) united extraction liquid is placed and is separated out the part crystal after 18 hours,
4) with 3) in place liquid and filter,
5) reclaim filtrating and be concentrated into small volume,
6) with the 5th) the step crystallization of separating out uses washing with acetone,
7) with the 6th) step crystal with activated carbon decolorizing once,
8) use volume ratio as ethanol-methanol mixed dissolution with solvents of 8:3 crystallization after heat filtering, filter the back and place crystallization.It is very fast that this process is separated out crystallization, and the solvent volume amount is suitable.
Through above-mentioned steps, get white crystal, the crystal non-variegation is measured through high-performance liquid chromatogram determination and area normalization, and purity reaches more than 97%, and whole process extraction yield is 75%.
Embodiment 3
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) be the concentration range ethanol of 5 times of amounts of raw material with raw material refluxing extraction 3 times, the preceding time is 3 hours, for the second time be 1.5 hours for the third time, the Bergeninum extraction yield is 80% as a result,
3) collect extracting solution, placed 24 hours,
4) precipitated liquid is filtered,
5) reclaim filtrating and be concentrated into small volume,
6) heat filtering after the deposition that will clean uses concentration as ethanol-methanol mixed dissolution with solvents of 8:5 filters the back and places crystallization.It is slower that this process is separated out crystallization, and the solvent volume amount is less relatively.
Through above-mentioned steps, get white crystal, to measure through high-performance liquid chromatogram determination and area normalization, purity reaches more than 97%, and whole process extraction yield is 80%.
Product among above-mentioned three embodiment is differentiated:
(1) performance liquid chromatography is differentiated
Referring to Fig. 5, chromatographic condition and system suitability test: use octadecylsilane key and silica gel to be weighting agent, moving phase is that methanol-water (25:75) solution is moving phase, and detecting wavelength is 274 nm.Number of theoretical plate calculates by the Bergeninum peak and is not less than 2000.
Need testing solution preparation: get crystallization 5mg, put in the 50ml measuring bottle, with 70% dissolve with methanol solution and be diluted to scale, shake up.
Reference substance solution preparation: precision takes by weighing Bergeninum reference substance 5mg, puts in the 50ml measuring bottle, with 70% dissolve with methanol solution and be diluted to scale, shakes up.
Measure: accurate respectively reference substance solution and each 10ul of need testing solution of drawing, inject liquid chromatograph, measure.The result shows in the trial-product chromatographic peak chromatographic peak that shows identical RT with reference substance.
(2) UV spectrum is differentiated
Referring to Fig. 3-Fig. 4, trial-product and reference substance scan under 400-200nm, show identical UV spectrum.
(3) mass spectrum is differentiated
Referring to Fig. 1-Fig. 2, through negative ion scanning, trial-product shows identical molecular ion peak with reference substance.
(4) fusing point test
Measure fusing point with small amount of crystal, mp:232-240 ℃.
Advanced the detection of above-mentioned four kinds of methods, the crystal that proves gained among the embodiment is a Bergeninum.
Claims (4)
1. the method for an extraction Bergeninum from Chinese medicinal materials ghost lamp is held up, it is characterized in that: said method is undertaken by following step:
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) using is the concentration doubly measured of raw material 4-6 as the methyl alcohol of 90-95% or ethanol with raw material refluxing extraction 3 times, and the time is 1-3 hour for the first time, for the second time be 0.5-1.5 hour for the third time,
3) united extraction liquid was placed 8-24 hour,
4) with 3) in place liquid and filter,
5) reclaim filtrating and be concentrated into small volume, put to separating out crystallization,
6) use volume ratio as ethanol-methanol mixed dissolution with solvents of 8:1-8:5 crystallization after heat filtering, filter the back and place crystallization.
2. the method for from the Chinese medicinal materials Rodgersia podophylla A. Gray, extracting Bergeninum according to claim 1 is characterized in that: in the said method the 5th) the step crystallization of separating out carries out the above-mentioned the 6th after with washing with acetone again) step.
3. the method for from the Chinese medicinal materials Rodgersia podophylla A. Gray, extracting Bergeninum according to claim 2 is characterized in that: with gac with the above-mentioned the 5th) crystallization in the step decolours once.
4. the method for from the Chinese medicinal materials Rodgersia podophylla A. Gray, extracting Bergeninum according to claim 1 and 2 is characterized in that:
1) get Chinese medicinal materials Rodgersia podophylla A. Gray meal and make raw material,
2) using is that the concentration of 5 times of amounts of raw material is 93% ethanol with raw material refluxing extraction 3 times, and the time is 2 hours for the first time, for the second time be 1 hour for the third time,
3) united extraction liquid was placed 24 hours,
4) with 3) in place liquid and filter,
5) reclaim filtrating and be concentrated into small volume, put to separating out crystallization,
6) with the 5th) the step crystallization of separating out uses washing with acetone,
7) use volume ratio as ethanol-methanol mixed dissolution with solvents of 8:3 crystallization after heat filtering, filter the back and place crystallization.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102487629A (en) * | 2011-12-09 | 2012-06-13 | 云南农业大学 | Method for improving germination of featherleaf rodgersflower seeds |
| CN102816169B (en) * | 2012-09-10 | 2014-11-05 | 昭通市骅成制药有限公司 | Extraction method and extraction system for bergenin |
| CN103833765A (en) * | 2014-01-26 | 2014-06-04 | 山西鑫中大生物科技有限公司 | Method for extraction separation of bergenin from Rodgersia podophylla |
| WO2017185276A1 (en) * | 2016-04-28 | 2017-11-02 | 朱小涛 | Method for extracting purple bergenia extractive |
| CN106749298B (en) * | 2016-11-18 | 2019-03-29 | 文县嘉诚农副产品有限公司 | A kind of Bergenin extracts and refining methd |
| KR102243591B1 (en) * | 2019-03-26 | 2021-04-23 | 안동대학교 산학협력단 | Antimicrobial composition comprising the extract of rodgersia podophylla |
| CN111187274B (en) * | 2020-01-15 | 2022-03-15 | 中国科学院西北高原生物研究所 | Method for separating and preparing bergenin chemical reference substance in Saxifraga stolonifera |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712684A (en) * | 2009-11-18 | 2010-05-26 | 陕西白云制药有限公司 | Process for quickly and demicontinuously extracting bergenin |
| CN101817828A (en) * | 2010-03-01 | 2010-09-01 | 山东大学威海分校 | Preparation of bergenin in aruneus dioicus |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101712684A (en) * | 2009-11-18 | 2010-05-26 | 陕西白云制药有限公司 | Process for quickly and demicontinuously extracting bergenin |
| CN101817828A (en) * | 2010-03-01 | 2010-09-01 | 山东大学威海分校 | Preparation of bergenin in aruneus dioicus |
Non-Patent Citations (3)
| Title |
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| 刘海周等.岩白菜中岩白菜素的纯化及提取工艺研究.《云南中医学院学报》.2011,第34卷(第2期),22-25. * |
| 孙敏等.岩白菜素提取工艺制剂及质量标准研究综述.《云南中医中药杂志》.2005,第26卷(第5期),56-58. * |
| 蔡正军等.超声提取鬼灯檠中岩白菜素的最佳工艺研究.《中国现代应用药学杂志》.2009,第26卷(第7期),559-561. * |
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