CN101898938A - Method for preparing bakuchiol - Google Patents
Method for preparing bakuchiol Download PDFInfo
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- CN101898938A CN101898938A CN2009100848325A CN200910084832A CN101898938A CN 101898938 A CN101898938 A CN 101898938A CN 2009100848325 A CN2009100848325 A CN 2009100848325A CN 200910084832 A CN200910084832 A CN 200910084832A CN 101898938 A CN101898938 A CN 101898938A
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- bakuchiol
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Abstract
The invention discloses a method for preparing a natural medicinal effective component, which is characterized by comprising the following steps of: extracting fructus psoraleae with ethanol; precipitating the extract with water; purifying filtrate by a macroporous resin; extracting the filtrate with an organic solvent; abandoning the extract; and washing residues. Technical method comparison experiments prove that the content of the bakuchiol prepared by the method is over 90 percent, which sufficiently proves the advancement of the method.
Description
Technical field
The present invention relates to medical technical field, be specifically related to a kind of Bakuchiol preparation method.
Background technology
The Chinese medicine Psoralea corylifolia is legumes psoraleae (PsoraleacorylifoliaL) fruit, and is warm in nature, and flavor is hot, the effect that tool is tonified the kidney and support yang.Cure mainly cold the rushing down of suffering from a deficiency of the kidney, frequent micturition, impotence, waist knee crymodynia, the cold of insufficiency type is breathed with cough, the external application curing vitiligo.Modern study shows that Bakuchiol is an effective constituent important in the Psoralea corylifolia, though the available technology adopting silica gel column chromatography can make the purity of Bakuchiol reach more than 90%, its method is laboratory method, can not be applied to industrialization; Perhaps adopt the macroporous resin purification method, but follow-up purification process does not carry out deep research, therefore, can only obtain the Bakuchiol of 50%-70% purity, so, a kind of suitable suitability for industrialized production studied, method that purity is high is imperative.
Summary of the invention
For these reasons, our scientific research personnel is by secular experimental study, the creationary preparation method who obtains a kind of Bakuchiol: Bakuchiol is through extraction using alcohol, macroporous resin purification, and the method that organic solvent extraction, gac charcoal take off obtains.This processing method can well be in suitability for industrialized production, and the Bakuchiol purity that obtains surpasses 90%.
The present invention is achieved through the following technical solutions.
A kind of preparation method of Bakuchiol, Psoralea corylifolia is through extraction using alcohol, water precipitation, the filtrate macroporous resin purification, organic solvent extraction, extracting solution discards, and the method for washing residue obtains.
A kind of preparation method of Bakuchiol, wherein method is: get Psoralea corylifolia, pulverize extraction using alcohol, reclaim ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last macroporous adsorbent resin, washing, water lotion is removed, and uses the 30-90% ethanol elution, and elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaim ethanol, concentrate drying, dry thing organic solvent extraction, extracting solution discards, the residue drying, and washing, drying obtains Bakuchiol.
Wherein said macroporous adsorbent resin is a kind of among D101, AB-8, the NKA.
Wherein said organic solvent is a kind of in methyl alcohol, ethanol, propyl alcohol, the propyl carbinol.
Content analysis
According to high effective liquid chromatography for measuring
Chromatographic condition and system suitability experiment are weighting agent with the octadecylsilane chemically bonded silica; With methanol-water=55: 45 was moving phase; The detection wavelength is 246nm, and number of theoretical plate calculates by Bakuchiol should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing Bakuchiol reference substance reference substance, adds methyl alcohol and make the solution that every 1ml contains 20 μ g, promptly.
Effective constituent of the present invention is got in the preparation of need testing solution, and accurate the title decides, and adds dissolve with methanol, is transferred in the 100ml volumetric flask, adds methyl alcohol to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 5-10 μ l of need testing solution of drawing of assay method injects liquid chromatograph, measures, promptly.
Experimental result sees Table 1:
Table 1 active ingredient of akuchiol assay result
Experiment conclusion: analyze experiment and show that preparation method's of the present invention Bakuchiol content is 90%-97%, prove absolutely that processing method of the present invention has scientific meaning.
Processing method relatively
Experimental technique: get Psoralea corylifolia and extract purifying according to the different process method, 1 group is processing method of the present invention, and 2 groups is literature method, obtains Bakuchiol, detects according to above-mentioned check and analysis method, and experimental result sees Table 2.
Table 2 different process methods and results relatively
Conclusion: above-mentioned experiment shows that processing method of the present invention obtains Bakuchiol content greater than more than 90%, and document literature and art method Psoralea corylifolia uses content less than 80%, proves absolutely that processing method of the present invention is creative.
Preparation embodiment
Embodiment 1
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last NKA macroporous adsorbent resin, and washing, water lotion is removed, use 30% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent propanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 2
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last D101 macroporous adsorbent resin, and washing, water lotion is removed, use 90% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent n-butanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 3
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 35% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent methanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 4
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last NKA macroporous adsorbent resin, and washing, water lotion is removed, use 40% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, the organic solvent ethanol ethanol-extracted of dry thing, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 5
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last D101 macroporous adsorbent resin, and washing, water lotion is removed, use 45% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent n-butanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 6
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 45% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent propanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 7
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last D101 macroporous adsorbent resin, and washing, water lotion is removed, use 50% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent methanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 8
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last NKA macroporous adsorbent resin, and washing, water lotion is removed, use 55% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent propanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 9
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 60% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent n-butanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 10
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last D101 macroporous adsorbent resin, and washing, water lotion is removed, use 65% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent propanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 11
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 70% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent methanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 12
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last NKA macroporous adsorbent resin, and washing, water lotion is removed, use 75% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent n-butanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 13
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 80% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent extraction using alcohol, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 14
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last D101 macroporous adsorbent resin, and washing, water lotion is removed, use 85% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent n-butanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 15
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 90% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent propanol extraction, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
Embodiment 16
Get Psoralea corylifolia, pulverize, extraction using alcohol reclaims ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last AB-8 macroporous adsorbent resin, and washing, water lotion is removed, use 60% ethanol elution, elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaims ethanol, concentrate, drying, dry thing organic solvent extraction using alcohol, extracting solution discards, the residue drying, washing, drying obtains Bakuchiol.
The application of Bakuchiol in preparation treatment erectile disfunction medicine in the foregoing description.
Claims (4)
1. the preparation method of a Bakuchiol is characterized in that Psoralea corylifolia through extraction using alcohol, water precipitation, and the filtrate macroporous resin purification, organic solvent extraction, extracting solution discards, and the method for washing residue obtains.
2. the preparation method of a kind of Bakuchiol according to claim 1, wherein method is: get Psoralea corylifolia, pulverize extraction using alcohol, reclaim ethanol, concentrate, be dissolved in water fully, leave standstill, filter, filtrate concentrates, last macroporous adsorbent resin, washing, water lotion is removed, and uses the 30-90% ethanol elution, and elutriant discards, and uses 95% or the dehydrated alcohol wash-out again, reclaim ethanol, concentrate drying, dry thing organic solvent extraction, extracting solution discards, the residue drying, and washing, drying obtains Bakuchiol.
3. the preparation method of Bakuchiol according to claim 1 and 2, wherein said macroporous adsorbent resin is a kind of among D101, AB-8, the NKA.
4. the preparation method that Psoralea corylifolia according to claim 1 and 2 divides, wherein said organic solvent is a kind of in methyl alcohol, ethanol, propyl alcohol, the propyl carbinol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100848325A CN101898938A (en) | 2009-05-25 | 2009-05-25 | Method for preparing bakuchiol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100848325A CN101898938A (en) | 2009-05-25 | 2009-05-25 | Method for preparing bakuchiol |
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| CN101898938A true CN101898938A (en) | 2010-12-01 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104418707A (en) * | 2013-09-05 | 2015-03-18 | 复旦大学 | Natural product fructus psoraleae phenol and asymmetric synthesis method of enantiomer thereof |
| CN108653379A (en) * | 2018-06-15 | 2018-10-16 | 上海中医药大学 | A kind of psoralea corylifolia active component and its preparation method and application |
| CN114478196A (en) * | 2021-01-27 | 2022-05-13 | 江苏巴帝恩生物科技有限公司 | Method for extracting and purifying bakuchiol from radix Ulmi Pumilae and its application in cosmetics |
-
2009
- 2009-05-25 CN CN2009100848325A patent/CN101898938A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104418707A (en) * | 2013-09-05 | 2015-03-18 | 复旦大学 | Natural product fructus psoraleae phenol and asymmetric synthesis method of enantiomer thereof |
| CN104418707B (en) * | 2013-09-05 | 2017-10-10 | 复旦大学 | A kind of method of asymmetric synthesis of natural products Bakuchiol and its enantiomer |
| CN108653379A (en) * | 2018-06-15 | 2018-10-16 | 上海中医药大学 | A kind of psoralea corylifolia active component and its preparation method and application |
| CN114478196A (en) * | 2021-01-27 | 2022-05-13 | 江苏巴帝恩生物科技有限公司 | Method for extracting and purifying bakuchiol from radix Ulmi Pumilae and its application in cosmetics |
| CN114478196B (en) * | 2021-01-27 | 2023-11-10 | 江苏巴帝恩生物科技有限公司 | Method for extracting and purifying bakuchiol from Ulmus pumila root and application of bakuchiol in cosmetics |
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Application publication date: 20101201 |