CN102232994A - Method for preparing total phenols of Lignum Sappan - Google Patents
Method for preparing total phenols of Lignum Sappan Download PDFInfo
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- CN102232994A CN102232994A CN2011101178703A CN201110117870A CN102232994A CN 102232994 A CN102232994 A CN 102232994A CN 2011101178703 A CN2011101178703 A CN 2011101178703A CN 201110117870 A CN201110117870 A CN 201110117870A CN 102232994 A CN102232994 A CN 102232994A
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- lignum sappan
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Abstract
The invention relates to a method for preparing total phenols of Lignum Sappan, which comprises: crushing Lignum Sappan serving as a raw material; adding into an extraction kettle; performing supercritical CO2 extraction, and collecting Lignum Sappan extract; adding water for dispersion, adding into macroporous resin for absorption, performing gradient elution by alcohol solution, and collecting and combining eluent; and concentrating to a small volume, standing, precipitating, filtering out crystals, drying and obtaining the products of total phenols of Lignum Sappan. The method has the advantages of low energy consumption, short preparation period and high product purity.
Description
Technical field:
The invention belongs to the Separation of Natural Products field, especially relate to a kind of employing supercritical CO
2Abstraction technique prepares the method for Lignum Sappan total phenols.
Background technology:
Lignum Sappan Caesalpinia sappan L. is a pulse family Semen Caesalpiniae platymiscium, has another name called lignum sappan, Soviet Union's a tree, used in making timber for boats, Ramulus et Folium Bischofiae Javanicae, brown wood, red bavin etc., and its dry duramen is Chinese Chinese medicine.Nature and flavor: sweet, salty, flat.GUIXIN, liver, spleen channel.Function cures mainly: activating blood circulation to dissipate blood stasis, reducing swelling and alleviating pain, anti-inflammation, function of gallbladder promoting Sal Nitri.Being used for amenorrhea dysmenorrhea, tired resistance in puerperal, breast ventral spine pain, wound swells and ache etc.The Japan scholar is more to the chemical constitution study of Lignum Sappan, finds that phenolic compound is its active ingredient, comprises homoisoflavone class and derivant thereof, brazilin class, former brazilin and chalcone.
Modern pharmacological research shows, Lignum Sappan has immunosuppressive action, antitumor action, to blood circulation effect, sedation and analgesia effect, hypoglycemic activity, antibacterial and anti-inflammation functions, diuresis etc.
Shen Jia etc. studies show that brazilin class material has effects such as vasodilative effect, hypoglycemic activity, anticoagulant.Brazilin can also suppress the inductive macrophage of LPS synthetic to NO in addition, and brazilin and the complex of copper ion formation can destroy superhelix and the antibacterial activity of DNA; Brasilein has the certain protection effect to the Neuro-2 cell that lacks sugared anoxia-induced apoptosis, can improve the survival rate of cell and reduce the escape rate of cell lactic acid dehydrogenase.
Disclosed document such as Wu Jian " Lignum Sappan ethanol extract Chinese People's Anti-Japanese Military and Political College rat heart graft-rejection analysis of effective component ", this studies show that protosappanin A can alleviate graft-rejection, prolonging the survival natural law of graft, is the effective monomer of the anti-heart transplant rejection of Lignum Sappan ethanol extract.
Lai Zhenyuan etc. studies show that Lignum Sappan chalcone, oxidation haematoxylin and 3-deoxidation Lignum Sappan chalcone all have certain inhibition activity to HL-60 and SWO-38 tumor cell.
Prior art is more deep to the pharmacological research of various compositions in the Lignum Sappan, relates to few to the extraction of Lignum Sappan total phenols research.In the disclosed document of Solenognathus " Lignum Sappan total phenols quantitative approach, stability and Study on extraction ", the document finally determines to adopt 15 times of amount 70% ethanol by quantitative study, heating and refluxing extraction twice, and each 1 hour method obtains the Lignum Sappan total phenols.This method only obtains the crude extract of Lignum Sappan total phenols, it is not further purified, and adopts the reflux, extract, energy consumption bigger.
Summary of the invention:
The preparation method that the purpose of this invention is to provide a kind of Lignum Sappan total phenols, this method is easy and simple to handle, environmentally safe, energy consumption is relatively little, and the purity of the Lignum Sappan total phenols that makes is higher.
A kind of preparation method of Lignum Sappan total phenols is characterized in that comprising following steps: be raw material with the Lignum Sappan, pulverized 20 mesh sieves, add in the extraction kettle, adopt supercritical CO
2Extraction adds entrainer and participates in extraction, collects the Lignum Sappan extract, adds aqueous dispersion, is added in the macroporous resin and adsorbs, and with ethanol liquid gradient elution, collects eluent and merges, and is concentrated into small size, places crystallize, leaches crystal and is drying to obtain the total phenolic product of Lignum Sappan.
Described supercritical CO
2The extraction parameter setting is: extraction temperature is 30-45 ℃, and extracting pressure is 18-30MPa, and the extraction time is 1.5-3h, and the separation reactor I temperature is 15-22 ℃, and pressure is 8-12MPa, and separation reactor I I temperature is 8-15 ℃, and pressure is 6-8MPa.
Described entrainer is 85～95% ethanol or methanol, and consumption is a medical material amount 20～50%.
Described macroporous resin can be selected a kind of among XAD-1, AB-8, XSD-3 or the SP825 for use.
Described ethanol liquid gradient is: 2-4BV20-30% alcoholic solution → 3-5BV30～50% alcoholic solution → 4-6BV50-70% alcoholic solution.
This method good effect is:
1) this method adopts supercritical CO
2Extraction, energy consumption is low, extractant CO
2Cleanliness without any pollution;
2) this method adopts purification by macroporous resin Lignum Sappan total phenols, and treating capacity is big, and eluting solvent is simple.
3) this method processing step is simple to operate, and fast, whole technology all adopts nontoxic reagent, and products obtained therefrom can be used for medicine, field of health care products.
The invention will be further described below in conjunction with specific embodiment, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment:
Embodiment 1:
Get Lignum Sappan medical material 1kg, pulverized 20 mesh sieves, add in the extraction kettle, adopt supercritical CO
2Extraction, setting extraction kettle condition is: extraction temperature is 30 ℃, and extracting pressure is 30MPa, CO
2Flow is 15L/h, and the extraction time is 1.5h, adds 500ml85% methanol and participates in extraction as entrainer, setting the separating still condition is: the separation reactor I temperature is 22 ℃, and pressure is 12MPa, and separation reactor I I temperature is 12 ℃, pressure is 8MPa, collects the Lignum Sappan extract in separation reactor I I; Get XAD-1 type macroporous resin dress post, after the washing balance, the Lignum Sappan extract is added aqueous dispersion, feed in the resin column and adsorb, use 2BV30% alcoholic solution → 5BV50% alcoholic solution → 4BV70% alcoholic solution gradient elution successively, collect eluent and merge, be concentrated into small size, place crystallize, leach crystal and be drying to obtain the total phenolic product 52.3g of Lignum Sappan, Folin-phenol method detection level is 89.3%.
Embodiment 2:
Get Lignum Sappan medical material 5kg, pulverized 20 mesh sieves, add in the extraction kettle, adopt supercritical CO
2Extraction, setting extraction kettle condition is: extraction temperature is 40 ℃, and extracting pressure is 20MPa, CO
2Flow is 18L/h, and the extraction time is 2.5h, adds 1kg80% ethanol and participates in extraction as entrainer, setting the separating still condition is: the separation reactor I temperature is 20 ℃, and pressure is 10MPa, and separation reactor I I temperature is 15 ℃, pressure is 6MPa, collects the Lignum Sappan extract in separation reactor I I; Get AB-8 type macroporous resin dress post, after the washing balance, the Lignum Sappan extract is added aqueous dispersion, feed in the resin column and adsorb, use 3BV20% alcoholic solution → 4BV40% alcoholic solution → 5BV60% alcoholic solution gradient elution successively, collect eluent and merge, be concentrated into small size, place crystallize, leach crystal and be drying to obtain the total phenolic product 271.3g of Lignum Sappan, Folin-phenol method detection level is 84.7%.
Embodiment 3:
Get Lignum Sappan medical material 10kg, pulverized 20 mesh sieves, add in the extraction kettle, adopt supercritical CO
2Extraction, setting extraction kettle condition is: extraction temperature is 45 ℃, and extracting pressure is 22MPa, CO
2Flow is 25L/h, and the extraction time is 3h, adds 3kg95% ethanol and participates in extraction as entrainer, setting the separating still condition is: the separation reactor I temperature is 18 ℃, and pressure is 11MPa, and separation reactor I I temperature is 12 ℃, pressure is 6MPa, collects the Lignum Sappan extract in separation reactor I I; Get SP825 type macroporous resin dress post, after the washing balance, the Lignum Sappan extract is added aqueous dispersion, feed in the resin column and adsorb, use 3BV30% alcoholic solution → 4BV45% alcoholic solution → 6BV65% alcoholic solution gradient elution successively, collect eluent and merge, be concentrated into small size, place crystallize, leach crystal and be drying to obtain the total phenolic product 437.9g of Lignum Sappan, Folin-phenol method detection level is 87.1%.
Claims (4)
1. the preparation method of a Lignum Sappan total phenols is characterized in that comprising following steps: be raw material with the Lignum Sappan, pulverize, add in the extraction kettle, adopt supercritical CO
2Extraction adds entrainer and participates in extraction, collects the Lignum Sappan extract, adds aqueous dispersion, is added in the macroporous resin and adsorbs, and with ethanol liquid gradient elution, collects eluent and merges, and is concentrated into small size, places crystallize, leaches crystal and is drying to obtain the total phenolic product of Lignum Sappan.
2. the preparation method of a kind of Lignum Sappan total phenols as claimed in claim 1 is characterized in that described supercritical CO
2The extraction parameter setting is: extraction temperature is 30-45 ℃, and extracting pressure is 18-30MPa, and the extraction time is 1.5-3h, and the separation reactor I temperature is 15-22 ℃, and pressure is 8-12MPa, and separation reactor I I temperature is 8-15 ℃, and pressure is 6-8MPa.
3. the preparation method of a kind of Lignum Sappan total phenols as claimed in claim 1 is characterized in that described entrainer is 85～95% ethanol or methanol, and consumption is a medical material amount 20～50%.
4. the preparation method of a kind of Lignum Sappan total phenols as claimed in claim 1 is characterized in that described ethanol liquid gradient is: 2-4BV20-30% alcoholic solution → 3-5BV30～50% alcoholic solution → 4-6BV50-70% alcoholic solution.
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| CN2011101178703A CN102232994A (en) | 2011-05-06 | 2011-05-06 | Method for preparing total phenols of Lignum Sappan |
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| CN2011101178703A CN102232994A (en) | 2011-05-06 | 2011-05-06 | Method for preparing total phenols of Lignum Sappan |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622353A (en) * | 2015-12-22 | 2016-06-01 | 广州市娇兰化妆品有限公司 | Method for extracting Cakile Maritima phenolic substance from supercritical carbon dioxide |
| CN108703910A (en) * | 2018-08-08 | 2018-10-26 | 东莞市白天鹅纸业有限公司 | A kind of paper handkerchief and manufacturing method comprising lotion |
| CN109054432A (en) * | 2018-07-05 | 2018-12-21 | 佛山市衣香蒂丝服装设计有限公司 | A kind of brazilwood vegetable dye and its textile fabric coloring composition |
| CN109082905A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of dyeing of textile |
-
2011
- 2011-05-06 CN CN2011101178703A patent/CN102232994A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622353A (en) * | 2015-12-22 | 2016-06-01 | 广州市娇兰化妆品有限公司 | Method for extracting Cakile Maritima phenolic substance from supercritical carbon dioxide |
| CN109054432A (en) * | 2018-07-05 | 2018-12-21 | 佛山市衣香蒂丝服装设计有限公司 | A kind of brazilwood vegetable dye and its textile fabric coloring composition |
| CN109082905A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of dyeing of textile |
| CN108703910A (en) * | 2018-08-08 | 2018-10-26 | 东莞市白天鹅纸业有限公司 | A kind of paper handkerchief and manufacturing method comprising lotion |
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Application publication date: 20111109 |