CN101875685A - Lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin and extraction process thereof - Google Patents
Lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin and extraction process thereof Download PDFInfo
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- CN101875685A CN101875685A CN 201010210917 CN201010210917A CN101875685A CN 101875685 A CN101875685 A CN 101875685A CN 201010210917 CN201010210917 CN 201010210917 CN 201010210917 A CN201010210917 A CN 201010210917A CN 101875685 A CN101875685 A CN 101875685A
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Abstract
The invention provides a white crystalline powdered lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin, and discloses an extraction process of the extract. By taking lysimachia foenum-graecum hance as a raw material, the extraction process comprises the following steps of: extracting solvent, concentrating, performing resin absorption, performing resin decoloring by washing, eluting with alcoholic solution, collecting eluent, drying, obtaining a crude lysimachia foenum-graecum hance saponin product, heating to dissolve the crude lysimachia foenum-graecum hance saponin product by using alcohol, concentrating, drying and obtaining the white crystalline powdered lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin. The extraction process has the advantages of simple process, low production cost, high saponin yield, sufficient and reasonable utilization of the big polar part of the lysimachia foenum-graecum hance, and expanded sources of triterpenoid saponis.
Description
Technical field
The present invention relates to chemical industry, especially the Lysimachia foenum-graecum saponin extract and the extraction process thereof of saponin content 〉=30%.
Background technology
Lysimachia foenum-graecum (Lysimachia foenum-graecum Hance) is a Primulaceae Lysimachia plant, and the Dayao Mountain of Guangxi Gold show is the important place of production of Lysimachia foenum-graecum.Lysimachia foenum-graecum has the special fragrance breath, have " fragrant king's title ", is a kind of famous and precious natural perfume, and its essential oil is described as " liquid golden ", is widely used in industries such as medicine, spices, food, tobacco, weaving, daily-use chemical industry.In addition, Lysimachia foenum-graecum still is a kind of rare Chinese herbal medicine, its stem and Ye Douke are used as medicine, hot, sweet, the warm in nature characteristic of distinguishing the flavor of, have be good for the stomach, effects such as heat-clearing, sweating, promoting the circulation of qi, pain relieving, expelling parasite, remarkable to effects such as treatment Common Cold, stomachache, eczema, impotence, dysmenorrhoea, the disturbance of lower legs due to pathogenic cold and dampness, wound abscess, mountain sickness diseases.Therefore, Lysimachia foenum-graecum has boundless application prospect and value of exploiting and utilizing.
In former study work, more for the essential oil part Study of Lysimachia foenum-graecum, and water-soluble portion especially the development research of saponin is less.Once there are some researches show, contained the triterpenoid saponin compounds of serial oleanane type in the Lysimachia foenum-graecum.The triterpenoid saponin compounds extensively exists in the Lysimachia plant, has immunomodulatory, physiologically active such as antitumor, antiviral, antimycotic, anticancer, is a compounds that has application prospect.Yet the application for Lysimachia foenum-graecum at present only is confined to the essential oil part, and the effective constituent of a large amount of high polarity parts is left in the basket.Have not yet to see the extraction process of Lysimachia foenum-graecum saponin.How reasonably developing the high polarity part of Lysimachia foenum-graecum, give full play to the pharmaceutical use of Lysimachia foenum-graecum, utilize the Lysimachia foenum-graecum resources advantage, enlarge the application prospect of Lysimachia foenum-graecum, promote the economic value added of Lysimachia foenum-graecum, is urgent problem.
Summary of the invention
Purpose of the present invention aims to provide the Lysimachia foenum-graecum saponin extract and the extraction process thereof of a kind of saponin content 〉=30%.
The Lysimachia foenum-graecum saponin (extract) of a kind of saponin content 〉=30%, with the Lysimachia foenum-graecum is raw material, through solvent extraction → concentrated → resin absorption → washed resin decolouring → alcoholic solution wash-out → collection elutriant → drying, the Lysimachia foenum-graecum saponin crude product → crude product of content 〉=15% with pure heating for dissolving → concentrated → drying, make the extract of the white crystalline powder shape of Lysimachia foenum-graecum saponin content 〉=30%.
Product after tested, the saponin of extract is a triterpenoid saponin, content 〉=30%.
The extraction process of the Lysimachia foenum-graecum saponin (extract) of a kind of saponin content 〉=30% comprises the steps:
(1) Lysimachia foenum-graecum herb flush away sand, air-dry after, pulverize;
(2) add raw material 5-12 single or mixed solvent doubly, refluxing extraction, ultrasonic wave or microwave-assisted extract;
(3) united extraction liquid, concentrating under reduced pressure reclaims alcohol to there not being the alcohol flavor, and concentrated solution adds the suitable quantity of water dilution;
(4) extracting solution after the processing is used resin absorption;
(5) resin after the washing absorption near colourless, is the alcoholic solution wash-out of 50-100% until effluent liquid with concentration again, collects elutriant;
(6) elutriant drying obtains the Lysimachia foenum-graecum saponin extract crude product of saponin content 〉=15%;
(7) Lysimachia foenum-graecum saponin crude product 90%-100% alcohol heating for dissolving, cooled and filtered is got clear liquid;
(8) filtrate is concentrated, reclaim alcohol;
(9) concentrated solution drying obtains the Lysimachia foenum-graecum saponin of saponin content 〉=30%.
Single or mixed solvent described in the said extracted technology is single or several mixed solvents of methyl alcohol, ethanol, propyl carbinol, amylalcohol, water;
Described resin absorption can be selected styrene type interpolymer macroporous resin adsorption for use, and as using D type resin, D101, D201, D301 etc. are arbitrary all can;
Described wash-out is alcohol-water or methanol-water solution with the alcoholic solution of 50-100%; Described saponin crude product refining can be selected methyl alcohol, ethanol for use.
The invention has the advantages that:
1, finds the extraction process of from Lysimachia foenum-graecum, extracting the Lysimachia foenum-graecum saponin, particularly found the extraction process of extracting high-content Lysimachia foenum-graecum saponin;
2, present method technology is simple, and production cost is low, saponin yield height, after tested, extract saponin content 〉=30%;
3, the high polarity of Lysimachia foenum-graecum partly is fully used, has expanded the source of triterpenoid saponin.
Embodiment
The present invention will be described to enumerate a part of specific embodiment below, is necessary to be pointed out that at this following specific embodiment only is used for that the present invention is described further, does not represent limiting the scope of the invention.Some nonessential modifications that other people make according to the present invention and adjustment still belong to protection scope of the present invention.
Embodiment 1
Get Lysimachia foenum-graecum 100 grams, wash shakeout soil with water, pulverize air-dry back; Each 1 liter of 70% ethanolic soln, heating and refluxing extraction 3 times, each 1 hour of adding; Merge extracting solution according to a conventional method No. three times, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, concentrated solution and water with 1: 1 to 1: 5 dilution proportion after, fully adsorb with D101 or D201 or D301 macroporous adsorbent resin; Resin after the washing absorption near colourless, is 70% ethanolic soln wash-out until effluent liquid with concentration again, collects elutriant; Elutriant obtains Lysimachia foenum-graecum saponin crude product 8.2 grams after drying, and with Oleanolic Acid in contrast, adopting Vanillin-Glacial acetic acid-perchloric acid system colour developing and measuring saponin content is 28.3%; With the saponin crude product with 80 milliliter of 100% methyl alcohol heating for dissolving, cooled and filtered, concentrating filter liquor reclaims methyl alcohol; The concentrated solution drying obtains purified Lysimachia foenum-graecum saponin 5.4 grams, and saponin content is 43% after measured.
Embodiment 2
Get Lysimachia foenum-graecum 100 grams, wash shakeout soil with water, pulverize air-dry back; Add 1 liter of entry at every turn, heating and refluxing extraction 3 times, the time was followed successively by 2 hours, 1 hour, 1 hour; Merge No. three times extracting solution, concentrating under reduced pressure, concentrated solution fully adsorbs with macroporous adsorbent resin; Resin after the washing absorption near colourless, is 60% ethanolic soln wash-out until effluent liquid with concentration again, collects elutriant; Elutriant obtains Lysimachia foenum-graecum saponin crude product 5.0 grams after drying, and with Oleanolic Acid in contrast, adopting Vanillin-Glacial acetic acid-perchloric acid system colour developing and measuring saponin content is 20.8%; With the saponin crude product with 80 milliliter of 100% methyl alcohol heating for dissolving, cooled and filtered, concentrating filter liquor reclaims methyl alcohol; The concentrated solution drying obtains purified Lysimachia foenum-graecum saponin 3.2 grams, and saponin content is 32.5% after measured, and all the other are with embodiment 1.
Embodiment 3
Get Lysimachia foenum-graecum 100 grams, wash shakeout soil with water, pulverize air-dry back; Each 1 liter of 50% ethanolic soln that adds, ultrasonic-assisted extraction 3 times, each time is 0.5 hour; Merge No. three times extracting solution, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, and concentrated solution fully adsorbs with macroporous adsorbent resin after adding the suitable quantity of water dilution; Resin after the washing absorption near colourless, is 70% ethanolic soln wash-out until effluent liquid with concentration again, collects elutriant; Elutriant obtains Lysimachia foenum-graecum saponin crude product 7.0 grams after drying, and with Oleanolic Acid in contrast, adopting Vanillin-Glacial acetic acid-perchloric acid system colour developing and measuring saponin content is 25.2%; With the saponin crude product with 80 milliliter of 95% ethanol heating for dissolving, cooled and filtered, concentrating filter liquor reclaims ethanol; The concentrated solution drying obtains purified Lysimachia foenum-graecum saponin 4.1 grams, and saponin content is 36.3% after measured, and all the other are with embodiment 1.
Embodiment 4
Get 2 kilograms of Lysimachia foenum-graecums, wash shakeout soil with water, pulverize air-dry back; Each 10 liters of 60% ethanolic solns that add, microwave-assisted extracts 3 times, and each time is 0.5 hour; Merge No. three times extracting solution, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, and concentrated solution fully adsorbs with macroporous adsorbent resin after adding the suitable quantity of water dilution; Resin after the washing absorption near colourless, is 70% ethanolic soln wash-out until effluent liquid with concentration again, collects elutriant; Elutriant obtains Lysimachia foenum-graecum saponin crude product 135 grams after drying, and with Oleanolic Acid in contrast, adopting Vanillin-Glacial acetic acid-perchloric acid system colour developing and measuring saponin content is 25.1%; With the saponin crude product with 1 liter of 95% ethanol heating for dissolving, cooled and filtered, concentrating filter liquor reclaims ethanol; The concentrated solution drying obtains purified Lysimachia foenum-graecum saponin 75 grams, and saponin content is 35.5% after measured, and all the other are with embodiment 1.
Claims (6)
1. the extraction process of the Lysimachia foenum-graecum saponin extract of saponin content 〉=30% comprises the steps:
(1) Lysimachia foenum-graecum herb flush away sand, air-dry after, pulverize;
(2) add raw material 5-12 single or mixed solvent doubly, refluxing extraction, ultrasonic wave or microwave-assisted extract;
(3) united extraction liquid, concentrating under reduced pressure reclaims alcohol to there not being the alcohol flavor, and concentrated solution adds the suitable quantity of water dilution;
(4) extracting solution after the processing is used resin absorption;
(5) resin after the washing absorption near colourless, is the alcoholic solution wash-out of 50-100% until effluent liquid with concentration again, collects elutriant;
(6) elutriant drying obtains the Lysimachia foenum-graecum saponin extract crude product of saponin content 〉=15%;
(7) Lysimachia foenum-graecum saponin crude product 90%-100% alcohol heating for dissolving, cooled and filtered is got clear liquid;
(8) filtrate is concentrated, reclaim alcohol;
(9) concentrated solution drying obtains the Lysimachia foenum-graecum saponin of saponin content 〉=30%.
2. extraction process according to claim 1 is characterized in that: the described single or mixed solvent of step (2) is single or several mixed solvents of methyl alcohol, ethanol, propyl carbinol, amylalcohol, water.
3. extraction process according to claim 1 is characterized in that: the described resin of step (4) is a styrene type interpolymer macroporous adsorbent resin.
4. extraction process according to claim 1 is characterized in that: the described wash-out of step (5) is alcohol-water or methanol-water solution with the alcoholic solution of 50-100%.
5. extraction process according to claim 1 is characterized in that: the described alcohol of step (7) is methyl alcohol or ethanol.
6. the Lysimachia foenum-graecum saponin extract of the white crystalline powder shape of saponin 〉=30% that extracts with the described extraction process of claim 1.
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| CN 201010210917 CN101875685A (en) | 2010-06-25 | 2010-06-25 | Lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin and extraction process thereof |
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| CN 201010210917 CN101875685A (en) | 2010-06-25 | 2010-06-25 | Lysimachia foenum-graecum hance saponin extract having more than or equal to 30 percent of saponin and extraction process thereof |
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Cited By (3)
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| CN103421611A (en) * | 2013-09-10 | 2013-12-04 | 文笃祥 | Method for extracting effective constituents from holy basil |
| CN105462287A (en) * | 2016-01-26 | 2016-04-06 | 青岛百草纤维科技股份有限公司 | Method for extracting lavender dye and application of method to regenerated cellulose fiber dyeing |
| CN107231788A (en) * | 2015-07-31 | 2017-10-03 | 南部大学产学协力团 | Contain holy basil extract as the composition for preventing and treating citrus diplostomiasis of active ingredient, microcapsules and utilize its citrus diplostomiasis prevention and controls |
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| CN1414077A (en) * | 2002-09-27 | 2003-04-30 | 广西壮族自治区中国科学院广西植物研究所 | Extraction method of high quality lingxiang grass purified oil |
| CN101457178A (en) * | 2008-12-10 | 2009-06-17 | 广西中烟工业有限责任公司 | Method for extracting water-soluble volatilization component from lysimachia foenum-graecum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103421611A (en) * | 2013-09-10 | 2013-12-04 | 文笃祥 | Method for extracting effective constituents from holy basil |
| CN107231788A (en) * | 2015-07-31 | 2017-10-03 | 南部大学产学协力团 | Contain holy basil extract as the composition for preventing and treating citrus diplostomiasis of active ingredient, microcapsules and utilize its citrus diplostomiasis prevention and controls |
| CN105462287A (en) * | 2016-01-26 | 2016-04-06 | 青岛百草纤维科技股份有限公司 | Method for extracting lavender dye and application of method to regenerated cellulose fiber dyeing |
| CN105462287B (en) * | 2016-01-26 | 2017-08-25 | 青岛百草新材料股份有限公司 | A kind of extracting method of lavender dyestuff and its application in regenerated celulose fibre dyeing |
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Application publication date: 20101103 |