CN104193594A - Preparation method of piceatannol - Google Patents
Preparation method of piceatannol Download PDFInfo
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- CN104193594A CN104193594A CN201410450543.3A CN201410450543A CN104193594A CN 104193594 A CN104193594 A CN 104193594A CN 201410450543 A CN201410450543 A CN 201410450543A CN 104193594 A CN104193594 A CN 104193594A
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- piceatannol
- ethanol
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- Life Sciences & Earth Sciences (AREA)
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparation method of piceatannol. The preparation method comprises the following steps: (1) crushing passion fruit seeds, adding 50-60 DEG C aqueous solution the amount of which is twice that of the passion fruit seeds, adding 0.1-0.5% of biological enzyme for enzymolysis, adding 50-90% ethanol solution for reflux extraction for 2-3 times, recovering the reagent from the extract and then adding the extract to a macroporous resin for adsorption, performing gradient elution by use of the ethanol solution, concentrating, standing and precipitating the eluate, and filtering to obtain the precipitate; (2) dissolving the precipitate by use of 95% ethanol, putting the solution through an aluminum oxide short column, collecting the column passing solution, adding 1-2 times of water by volume, stirring thoroughly and standing for crystallization, filtering out the crystals, performing reflux dissolution on the crystals by use of 95% ethanol for recrystallization, and drying the crystals to obtain the piceatannol. As the method is used for producing the piceatannol, the obtained piceatannol is high in purity, and the process is simple and easy to operate, high in extraction efficiency and easy for industrial production.
Description
Technical field
The invention belongs to biological technical field, relate in particular to a kind of preparation method of piceatannol.
Background technology
Piceatannol, CAS accession number 10083-24-6, molecular formula C14H12O4, molecular weight 244.24, molecular structure:
Piceatannol has superpower antioxygenation, suppresses non-receptor activation enzyme, spleen butyric acid kinases and lymphocyte specific protein tyrosine kinase.Herba Passiflorae Caeruleae is Passifloraceae, and fruit is rich in 17 seed amino acids, multivitamin and carotenoid and the various trace element of needed by human body, soluble solid 15-16%, and total acid content 3.8-4%, sweet acid is moderate.Normal edible Purple Granadilla and processed goods thereof, to human body have aid digestion, can reduce phlegm, control deficiency of the kidney, produce refreshing effect to the mind, invigorate blood circulation keep fit, the effect such as sedation-analgesia, decompression lipopenicillinase.Seed Herba Passiflorae Caeruleae seed weight account for whole fruit heavy 8%～15%, and in seed containing rich in protein and fat, also contain a kind of antioxidant piceatannol.
By searching document, the document of preparing at present piceatannol from plant discloses less, and the method disclosing as patent " containing piceatannol composition and containing the preparation method of piceatannol composition " is that organic reagent extracts and is drying to obtain, and piceatannol purity is lower.
Summary of the invention
The present invention will address the deficiencies of the prior art and deficiency, and a kind of industrialized process for preparing of highly purified piceatannol is provided.
The present invention realizes by the following technical solutions:
A preparation method for piceatannol, is characterized in that comprising following steps:
(1) getting passion fruit seed pulverizes, add 50 ~ 60 DEG C of aqueous solution of 2 times of amounts, add again 0.1 ~ 0.5% biological enzyme enzymolysis, add again 50 ~ 90% ethanolic soln refluxing extraction 2 ~ 3 times, after extracting solution recovery reagent, add in macroporous resin and adsorb, use ethanolic soln gradient elution, the concentrated precipitation of placing of elutriant, filters to obtain throw out;
(2) above-mentioned throw out 95% dissolve with ethanol, peroxidation aluminium short column, collected post liquid and added 1 ~ 2 times of volume water, fully stirred and placed crystallization, and crystallisate leaches with 95% alcohol reflux dissolving-recrystallization, and crystallisate is drying to obtain.
One in step (1) in the optional cellulase of biological enzyme, amylase and polygalacturonase.
One in step (1) in the optional D101 of macroporous resin model, HZ816, AB-8 and HPD100.
In step (1), ethanol gradient elution is: first use 5 ~ 10 times of column volumes, 20 ~ 50% ethanol elution impurity, then use 5 ~ 10 times of cylinders, 60 ~ 90% ethanol elution effective constituents.
Adopt the present invention to produce piceatannol, method is simple to operate, and product yield is high, is easy to suitability for industrialized production.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to the following example.
Embodiment
Embodiment 1:
Getting Herba Passiflorae Caeruleae seed 10kg pulverizes, add 60 DEG C of aqueous solution of 2 times of amounts, add again 0.1% cellulase degradation 3 hours, 8 times of amount ethanolic soln refluxing extraction of 60% 3 times again, the concentrated dilute with water of extracting solution adds in D101 macroporous resin column and adsorbs, first use 6 times of column volumes, 40% ethanolic soln wash-out impurity, use again 10 times of cylinders, 70% ethanol elution effective constituent, elutriant is concentrated places precipitation without alcohol, collecting precipitation thing adds alumina with 95% dissolve with ethanol, collected the water that post liquid adds two volumes, place crystallization, crystallisate leaches, use again 95% alcohol reflux dissolving-recrystallization, be dried to obtain piceatannol 9.5g, content 94.3% after testing.
Embodiment 2:
Getting Herba Passiflorae Caeruleae seed 10kg pulverizes, add 60 DEG C of aqueous solution of 2 times of amounts, add again 0.2% amylase enzymolysis 3 hours, 8 times of amount ethanolic soln refluxing extraction of 60% 3 times again, the concentrated dilute with water of extracting solution adds in HZ816 macroporous resin column and adsorbs, first use 6 times of column volumes, 40% ethanolic soln wash-out impurity, use again 10 times of cylinders, 70% ethanol elution effective constituent, elutriant is concentrated places precipitation without alcohol, collecting precipitation thing adds alumina with 95% dissolve with ethanol, collected the water that post liquid adds two volumes, place crystallization, crystallisate leaches, use again 95% alcohol reflux dissolving-recrystallization, be dried to obtain piceatannol 10.2g, content 95.4% after testing.
Embodiment 3:
Getting Herba Passiflorae Caeruleae seed 10kg pulverizes, add 50 DEG C of aqueous solution of 2 times of amounts, add again 0.3% pectinase enzymatic hydrolysis 2 hours, 5 times of amount ethanolic soln refluxing extraction of 90% 3 times again, the concentrated dilute with water of extracting solution adds in AB-8 macroporous resin column and adsorbs, first use 6 times of column volumes, 50% ethanolic soln wash-out impurity, use again 7 times of cylinders, 80% ethanol elution effective constituent, elutriant is concentrated places precipitation without alcohol, collecting precipitation thing adds alumina with 95% dissolve with ethanol, collected the water that post liquid adds two volumes, place crystallization, crystallisate leaches, use again 95% alcohol reflux dissolving-recrystallization, be dried to obtain piceatannol 8.9g, content 93.1% after testing.
Embodiment 4:
Getting Herba Passiflorae Caeruleae seed 10kg pulverizes, add 50 DEG C of aqueous solution of 2 times of amounts, add again 0.2% amylase enzymolysis 3 hours, 7 times of amount ethanolic soln refluxing extraction of 80% 3 times again, the concentrated dilute with water of extracting solution adds in HPD100 macroporous resin column and adsorbs, first use 6 times of column volumes, 40% ethanolic soln wash-out impurity, use again 8 times of cylinders, 80% ethanol elution effective constituent, elutriant is concentrated places precipitation without alcohol, collecting precipitation thing adds alumina with 95% dissolve with ethanol, collected the water that post liquid adds two volumes, place crystallization, crystallisate leaches, use again 95% alcohol reflux dissolving-recrystallization, be dried to obtain piceatannol 9.2g, content 94.1% after testing.
Claims (4)
1. a preparation method for piceatannol, is characterized in that comprising following steps:
(1) getting passion fruit seed pulverizes, add 50 ~ 60 DEG C of aqueous solution of 2 times of amounts, add again 0.1 ~ 0.5% biological enzyme enzymolysis, add again 50 ~ 90% ethanolic soln refluxing extraction 2 ~ 3 times, after extracting solution recovery reagent, add in macroporous resin and adsorb, use ethanolic soln gradient elution, the concentrated precipitation of placing of elutriant, filters to obtain throw out;
(2) above-mentioned throw out 95% dissolve with ethanol, peroxidation aluminium short column, collected post liquid and added 1 ~ 2 times of volume water, fully stirred and placed crystallization, and crystallisate leaches with 95% alcohol reflux dissolving-recrystallization, and crystallisate is drying to obtain.
2. the preparation method of piceatannol as claimed in claim 1, is characterized in that the one in the optional cellulase of biological enzyme, amylase and polygalacturonase in described step (1).
3. the preparation method of piceatannol as claimed in claim 1, is characterized in that the one in the optional D101 of macroporous resin model, HZ816, AB-8 and HPD100 in described step (1).
4. the preparation method of piceatannol as claimed in claim 1, is characterized in that in described step (1), ethanol gradient elution is: first use 5 ~ 10 times of column volumes, 20 ~ 50% ethanol elution impurity, then use 5 ~ 10 times of cylinders, 60 ~ 90% ethanol elution effective constituents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410450543.3A CN104193594A (en) | 2014-09-05 | 2014-09-05 | Preparation method of piceatannol |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410450543.3A CN104193594A (en) | 2014-09-05 | 2014-09-05 | Preparation method of piceatannol |
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| CN104193594A true CN104193594A (en) | 2014-12-10 |
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| CN201410450543.3A Pending CN104193594A (en) | 2014-09-05 | 2014-09-05 | Preparation method of piceatannol |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439824A (en) * | 2015-11-06 | 2016-03-30 | 陕西嘉禾生物科技股份有限公司 | Synthesis method of piceatannol |
| CN110655452A (en) * | 2019-09-29 | 2020-01-07 | 钟华 | Method for extracting piceatannol from mixture of passion fruit, grape and blueberry and application of piceatannol |
| CN111704530A (en) * | 2020-07-07 | 2020-09-25 | 昆明翔昊科技有限公司 | Method for extracting piceatannol from rheum officinale, microcapsule molecule embedding method and application of piceatannol in cosmetics |
| CN111763141A (en) * | 2020-07-07 | 2020-10-13 | 昆明翔昊科技有限公司 | Method for extracting piceatannol from rhubarb medicinal materials, microcapsule molecule embedding method and application of microcapsule molecule embedding method in food and health care products |
-
2014
- 2014-09-05 CN CN201410450543.3A patent/CN104193594A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105439824A (en) * | 2015-11-06 | 2016-03-30 | 陕西嘉禾生物科技股份有限公司 | Synthesis method of piceatannol |
| CN110655452A (en) * | 2019-09-29 | 2020-01-07 | 钟华 | Method for extracting piceatannol from mixture of passion fruit, grape and blueberry and application of piceatannol |
| CN111704530A (en) * | 2020-07-07 | 2020-09-25 | 昆明翔昊科技有限公司 | Method for extracting piceatannol from rheum officinale, microcapsule molecule embedding method and application of piceatannol in cosmetics |
| CN111763141A (en) * | 2020-07-07 | 2020-10-13 | 昆明翔昊科技有限公司 | Method for extracting piceatannol from rhubarb medicinal materials, microcapsule molecule embedding method and application of microcapsule molecule embedding method in food and health care products |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20141210 |
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| WD01 | Invention patent application deemed withdrawn after publication |