CN101168556A - Method for purifying esgoside and extracting biological active compound - Google Patents
Method for purifying esgoside and extracting biological active compound Download PDFInfo
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- CN101168556A CN101168556A CNA2006100512560A CN200610051256A CN101168556A CN 101168556 A CN101168556 A CN 101168556A CN A2006100512560 A CNA2006100512560 A CN A2006100512560A CN 200610051256 A CN200610051256 A CN 200610051256A CN 101168556 A CN101168556 A CN 101168556A
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Abstract
The invention discloses purification momordica grosvenori glucoside and a method for withdrawing the biological activity material, the method uses the solvent-extraction process to purify momordica grosvenori glucoside, simultaneously withdraws the momordica grosvenori element, and includes the steps that the fluid is prepared, the extract is carried on with moderate nonpolar resolver, the withdrawing is carried on with medium polar organic solvent, and the spraying and the drying are performed. The method of the invention can eliminate the return bitter taste in the momordica grosvenori, the momordica grosvenori sweet material, the extraction of the momordica grosvenori, the momordica grosvenori concentration fruit juice, the momordica grosvenori sweetening agent, and the product, thereby improving momordica grosvenori sweet material taste, purifying momordica grosvenori glucoside, and simultaneously withdrawing the active material, namely, the momordica grosvenori element having anti-microorganism. The momordica grosvenori element has the activeness suppressing microorganism, such as Gram-negative bacteria, Gelanshi masculine fungus and fungus and so on. The anti-microorganism activeness of the momordica grosvenori element extracted with the invention can be used to prepare the anti-microorganism medicine and daily necessities like cough syrup, throat piece, toothpaste, rinses mouth fluid and so on, and the invention can have very great use value and economic value.
Description
Technical field
The present invention relates to the purifying of atural spice thing, also extract the method for biologically active material in particular to the purifying of Momordia grosvenori aglycone simultaneously.
Background technology
Grosvenor Momordica is the fruit that the perennial perennial root of Curcurbitaceae is climbed up by holding on to vine Grosvenor Momordica (Siraitiagrosvenorii).Grosvenor Momordica typically refers to the fruit of plant (Siraitia grosvenorii), but also comprise relevant similar floristics: S.siamensis, S.silomaradjae, S.sikkimensis, S.siraitia, S.borneensis and S.taiwaniana.Sweet ingredient Momordia grosvenori aglycone in the Grosvenor Momordica is a triterpene compound, and its glucose ring links to each other with the mogrol base.Fructus Monordicae extract is a kind of powder, and the content of its Momordia grosvenori aglycone is 60%～99%, has been widely used as sweeting agent at present.Yet the Fructus Monordicae extract of producing still contains the bitter taste that returns to a certain degree at present, and this has influenced the mouthfeel of Fructus Monordicae extract and has limited its application as natural sweeteners.The Grosvenor Momordica fruit juice concentrate that the crushing of Grosvenor Momordica fresh fruit is made is the product that just develops in recent years, is documented among the U.S. Pat Patent 20060003053, equally also contains the bitter taste that returns to a certain degree, also can influence beverage quality.For a long time, it is believed that back that bitter taste may be a kind of ins and outs of Momordia grosvenori aglycone.The contriver is by discovering Grosvenor Momordica, the chemical substance of returning bitter taste in Fructus Monordicae extract and the fruit juice concentrate has the chemical structure similar with Momordia grosvenori aglycone, therefore they often be mixed together and be difficult for separated so that former laboratory and industrially all fail to detect and isolate back bitter substance; Thereby proved that time bitter taste is not a kind of ins and outs of Momordia grosvenori aglycone.Before this, the contriver has invented the method for removing bitter taste of momordica grosvenori extract, and employment application patent, application number is CN200610051186.9.The contriver finds also that simultaneously bitter substance has antimicrobial activity.Yet up to now, also nobody proposes the purifying Momordica grosvenori glycosides, extraction simultaneously has the method for antimicrobial active substance.
Summary of the invention
The method that purpose of the present invention just is to provide a kind of purifying Momordica grosvenori glycosides and extracts the tool biologically active substance, the Momordia grosvenori aglycone that purifying is crossed become that a kind of application is wider, sweet taste is denseer, and the sweeting agent that mouthfeel is purer obtains having the material of antimicrobial acivity simultaneously.
The contriver discovers can be with Grosvenor Momordica, and the bitter substance that returns in Fructus Monordicae extract and the fruit juice concentrate is separated, and finds back also that simultaneously bitter substance has good antimicrobial acivity.After tested, learn that the Fructus Monordicae extract that contains 80% sweet glycosides approximately contains 7% the bitter substance that returns; The contriver is through research, find and assert that the bitter taste that returns in the Fructus Monordicae extract mainly is spontaneous one or more times bitter substance or the material of the similar bitters of chemical structure produces in the similar cucurbitaceous plant process of growth that the contriver is temporarily with these material called afters " Grosvenor Momordica element "; And find that " Grosvenor Momordica element " is present in whole Momordica grosvenori plant is in Leaf of Grosvenor Momordica, rattan, root, stem and the fruit, it has the inhibition microbic activity, as part Gram-negative bacteria, gram-positive microorganism and fungi etc. are had restraining effect.
The contriver discovers and utilizes polarity and deliquescent difference, " Grosvenor Momordica element " and Momordia grosvenori aglycone can be separated; Like this, can in the purifying Momordica grosvenori glycosides, extract biologically active material " Grosvenor Momordica element ".Therefore, solution provided by the invention is to adopt solvent-extraction process purifying Momordica grosvenori glycosides, extraction " Grosvenor Momordica element " simultaneously, promptly removes and collects bitter substance and carry out simultaneously.
Method provided by the invention is following realization:
1. carrying out mechanical disintegration obtains meal in fact with the Grosvenor Momordica dry fruit, or the fragment that the crushing of fresh Lo Han Guo fruit is obtained wetting, the alcoholic solution of water or different concns soaks described meal and fragment, and is heated at least 80 ℃, carry out the above extraction of 60min, obtain extract liquid; Repeat to extract 3 times, the Grosvenor Momordica extracting liquid filtering is obtained filtrate, ethanol evaporation and obtain the aqueous solution; Or with the water-soluble aqueous solution that directly obtains of Fructus Monordicae extract;
2. with nonpolar solvent extraction at least 1 time to remove lipid acid, protein and some other impurity, separate organic layer and water layer;
3. combining water layer washes with water to remove the not material of absorption also by isorrheic nonpolar macroporous adsorbent resin; 10%～95% ethanol with 3 times of column volumes carries out gradient elution again; Ethanol is removed in 40%～70% elutriant merging obtained the Grosvenor Momordica aqueous solution; Elutriant with 80%～95% merges removes ethanol, and drying obtains " Grosvenor Momordica element ";
4. obtain organic layer three times with the polar solvent extraction Grosvenor Momordica aqueous solution, this organic layer promptly contains " Grosvenor Momordica element ", and water layer contains Momordia grosvenori aglycone; Separate organic layer and water layer, dry organic layer obtains " Grosvenor Momordica element ", and the spraying drying water layer obtains Momordia grosvenori aglycone.
1.～3. step is used for from Grosvenor Momordica dry fruit or the fresh Lo Han Guo fruit Momordia grosvenori aglycone of purifying; If Grosvenor Momordica dry fruit mechanical disintegration is become the Grosvenor Momordica meal, 4. handle with step, can directly obtain " Grosvenor Momordica element " and contain the mangosteen powder of Momordia grosvenori aglycone.
If raw material is the aqueous solution made from Fructus Monordicae extract or uses the Grosvenor Momordica fruit juice concentrate, then directly enter step 4., obtain Momordia grosvenori aglycone and " the Grosvenor Momordica element " of purifying.
The contriver points out, because wax, pigment (as chlorophyll, xenthophylls etc.), high boiling terpene, nonpolar lipid acid and fat etc. may disturb the purifying of " Grosvenor Momordica element ", so at first remove them with nonpolar solvent extraction, solvent be normal hexane and, sherwood oil and tetracol phenixin etc., also can use their mixture.
The contriver also points out, moderate polar solvent refers to anyly has some polarity, but not miscible with water organic solvent as methylene dichloride and ethyl acetate etc., also can be their mixed solvent.These solvents have very strong avidity for " Grosvenor Momordica element ".Through the organic solvent extraction of middle polarity, the aqueous solution that contains Momordia grosvenori aglycone of resulting light color has been sloughed bitter substance most time.
The 3rd step of aforesaid method is used for carrying out isolating macroporous resin and comprises Amberlite and commercially available macroporous adsorbent resin.With macroporous adsorbent resin separate with can exchange sequence with the leaching process of moderate polar solvent, promptly can be before by macroporous adsorbent resin or by carrying out after the macroporous adsorbent resin with the leaching process of moderate polar solvent.
Method of the present invention can be removed Grosvenor Momordica, Grosvenor Momordica sweetener, the extract of Grosvenor Momordica and Grosvenor Momordica fruit juice concentrate, time bitter taste in momordica grosvenori sweetening agent and the goods, improve the taste of Grosvenor Momordica sweetener, be further purified Momordia grosvenori aglycone and extract simultaneously and have antimicrobial active substance " Grosvenor Momordica element ", can also be from Lo Han Guo fruit the direct purer Momordia grosvenori aglycone of extraction." Grosvenor Momordica element " has the inhibition microbic activity, as Gram-negative bacteria, gram-positive microorganism and fungi etc.The antimicrobial acivity of contriver's prediction " Grosvenor Momordica element " can be used to prepare antimicrobial medicine and daily necessities such as cough syrup, lozenge, and toothpaste and collutory etc. will have very big practical value and economic worth.
Embodiment
Following examples can illustrate the present invention better:
Embodiment 1: for Grosvenor Momordica
10g arhat fruit is carried out mechanical disintegration obtain the Grosvenor Momordica meal, or the fragment that the crushing of fresh 10g arhat fruit is obtained wetting, carry out extraction more than the 120min, obtain organic layer with the ethyl acetate of 100ml; The organic layer extraction is repeated 3 times, separate organic layer and Grosvenor Momordica meal; Merge organic layer, be dried and obtain about 0.4g " the Grosvenor Momordica element "; Spraying drying obtains the purer Momordia grosvenori aglycone of about 9.4g.
Embodiment 2: for Grosvenor Momordica
100g Grosvenor Momordica dry fruit is carried out mechanical disintegration obtain meal, or the fragment that the crushing of fresh 100g arhat fruit is obtained wetting, soak described meal and fragment with the aqueous ethanolic solution of 500ml water or 50% or 50% methanol aqueous solution, and be heated at least 80 ℃, carry out the above extraction of 60min at least, obtain extract liquid; Extract and repeat 3 times, extracting liquid filtering is obtained filtrate 1200ml; Ethanol evaporation and obtain the aqueous solution.With nonpolar solvent such as normal hexane extraction at least once to remove lipid acid, protein and some other impurity; Separate organic layer and water layer, keep water layer.Obtain organic layer at least 3 times with moderate polar solvent ethyl acetate 1000ml aqueous layer extracted, this organic layer promptly contains " Grosvenor Momordica element ", and water layer contains Momordia grosvenori aglycone; Separate organic layer and water layer, dry organic layer obtains 0.5g " the Grosvenor Momordica element ".Water layer is passed through isorrheic nonpolar 100ml macroporous adsorbent resin, for example Amberlite XAD16 post.Wash with water to remove the not material of absorption; 10% to 95% ethanol with 3 times of column volumes carries out gradient elution up to there not being sweet taste substance again; Contain our desirable ingredients in 40% to 95% the elutriant, collect 40% to 95% elutriant, 40% to 70% elutriant merging spraying drying is removed ethanol obtain the purer Momordia grosvenori aglycone powder of 1.5g.80% to 95% elutriant merging spraying drying is removed ethanol obtain purer 0.2g " Grosvenor Momordica element ".
Embodiment 3: for Grosvenor Momordica
Drying in the sun 100g Lo Han Guo fruit is carried out mechanical disintegration obtain meal, or,, be heated at least 80 ℃ and carry out the above extraction of 60min, obtain extract liquid with 500ml water or 50% aqueous ethanolic solution with the fragment that fresh Lo Han Guo fruit crushing obtains wetting; Centrifugation also keeps supernatant liquor and solid, solid matter is extracted repeat 3 times, and the Grosvenor Momordica extracting liquid filtering is obtained filtrate; Ethanol evaporation obtains the aqueous solution; Extracting liquid filtering is obtained the about 1200ml of filtrate; Filtrate had been carried out isorrheic nonpolar Amberlite XAD post by 100ml; Wash to remove the not material of absorption with 1200ml; Carry out gradient elution with each 300ml of ethanol of 10% to 95% again, contain Momordia grosvenori aglycone in 40% to 60% the elutriant, collect 40% to 95% elutriant respectively, 40% to 70% elutriant merging drying is removed ethanol obtain the Grosvenor Momordica extracting solution aqueous solution.With the 500ml moderate polar solvent ethyl acetate extraction Grosvenor Momordica extracting solution aqueous solution, obtain organic layer, this organic layer contains " the Grosvenor Momordica element ", and water layer contains Momordia grosvenori aglycone; Extract and repeat 3 times; Separate organic layer and water layer, dry water layer obtains the 1.5g Momordia grosvenori aglycone.80% to 95% elutriant drying is removed ethanol obtain, dry organic layer obtains 0.5g " Grosvenor Momordica element ".
Embodiment 4: for Fructus Monordicae extract
10g is contained 80% Momordia grosvenori aglycone Fructus Monordicae extract powder make the 100ml aqueous solution and carry out extraction more than the 30min, obtain organic layer and water layer with isopyknic ethyl acetate; The water layer extraction is repeated 3 times, separate organic layer and water layer; Merge organic layer, be dried and obtain about 0.7g " Grosvenor Momordica element "; Merge the water layer and the spraying drying that contain Momordia grosvenori aglycone and obtain the purer Momordia grosvenori aglycone of about 9g.
Embodiment 5: for the Grosvenor Momordica fruit juice concentrate
With 100ml Grosvenor Momordica fruit juice concentrate, carry out extraction more than the 30min with isopyknic ethyl acetate, obtain organic layer and water layer; Water layer is extracted repetition 3 times, separate organic layer and water layer; Merge organic layer, be dried and obtain about 0.67g " Grosvenor Momordica element "; Merging the water layer contain Momordia grosvenori aglycone obtains purifying and crosses the about 100ml of Grosvenor Momordica fruit juice concentrate.
Claims (8)
1. purifying Momordica grosvenori glycosides and extract the method for biologically active substance is characterized in that this method adopts solvent-extraction process purifying Momordica grosvenori glycosides, extracts " Grosvenor Momordica element " simultaneously, may further comprise the steps:
1. carrying out mechanical disintegration obtains meal in fact with the Grosvenor Momordica dry fruit, or the fragment that the crushing of fresh Lo Han Guo fruit is obtained wetting, the alcoholic solution of water or different concns soaks described meal and fragment, and is heated at least 80 ℃, carry out the above extraction of 60min, obtain extract liquid; Extract to repeat 3 times, the Grosvenor Momordica extracting liquid filtering is obtained filtrate, ethanol evaporation and obtain the aqueous solution; Or with the water-soluble aqueous solution that directly obtains of Fructus Monordicae extract;
2. with nonpolar solvent extraction at least 1 time to remove lipid acid, protein and some other impurity, separate organic layer and water layer;
3. combining water layer washes with water to remove the not material of absorption also by isorrheic nonpolar macroporous adsorbent resin; 10%～95% ethanol with 3 times of column volumes carries out gradient elution again; Ethanol is removed in 40%～70% elutriant merging obtained the Grosvenor Momordica aqueous solution; Elutriant with 80%～95% merges removes ethanol, and drying obtains " Grosvenor Momordica element ";
4. obtain organic layer 3 times with the polar solvent extraction Grosvenor Momordica aqueous solution, this organic layer promptly contains
" Grosvenor Momordica element ", and water layer contains Momordia grosvenori aglycone; Separate organic layer and water layer, dry organic layer obtains " Grosvenor Momordica element ", and the spraying drying water layer obtains Momordia grosvenori aglycone.
2. the method for claim 1 is characterized in that the Grosvenor Momordica meal that becomes with Grosvenor Momordica dry fruit mechanical disintegration is a raw material, 4. handles promptly the mangosteen powder that directly obtains " Grosvenor Momordica element " and contain Momordia grosvenori aglycone with step.
3. the method for claim 1 is characterized in that the aqueous solution made with Fructus Monordicae extract or is raw material with the Grosvenor Momordica fruit juice concentrate, then directly enters step 4., obtains Momordia grosvenori aglycone and " the Grosvenor Momordica element " of purifying
4. the method for claim 1 is characterized in that described non-polar solvent is normal hexane or sherwood oil or tetracol phenixin or their mixture.
5. the method for claim 1 is characterized in that described moderate polar solvent is chloroform or methylene dichloride or ethyl acetate or their mixture.
6. the method for claim 1 is characterized in that describedly being used for carrying out isolating macroporous resin and comprising commercially available anionite-exchange resin, Zeo-karb and mixed type ion exchange resin.
7. the method for claim 1, it is characterized in that the sepn process carried out with macroporous adsorbent resin with can exchange sequence with the leaching process of moderate polar solvent, promptly can be before by macroporous adsorbent resin or by carrying out after the macroporous adsorbent resin with the leaching process of moderate polar solvent.
8. the method for claim 1 is characterized in that described Grosvenor Momordica is meant fruit and the plant S.siamensis of plant Siraitia grosvenorii, S.silomaradjae, S.sikkimensis, S.siraitia, the fruit of S.borneensis and Taiwan Grosvenor Momordica.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2006100512560A CN101168556A (en) | 2006-10-27 | 2006-10-27 | Method for purifying esgoside and extracting biological active compound |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059959A (en) * | 2013-03-20 | 2014-09-24 | 广西壮族自治区中国科学院广西植物研究所 | Method for synthesizing sweet saponin with bitter and fallen grosvenor momordica fruit as raw material |
| CN107397103A (en) * | 2017-08-25 | 2017-11-28 | 湖南华诚生物资源股份有限公司 | A kind of preparation method of Momordica grosvenori decolouring flavor inspissated juice |
| CN110214886A (en) * | 2012-08-07 | 2019-09-10 | 桂林吉福思罗汉果有限公司 | The preparation method of sweet juice composition |
-
2006
- 2006-10-27 CN CNA2006100512560A patent/CN101168556A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110214886A (en) * | 2012-08-07 | 2019-09-10 | 桂林吉福思罗汉果有限公司 | The preparation method of sweet juice composition |
| CN110214885A (en) * | 2012-08-07 | 2019-09-10 | 桂林吉福思罗汉果有限公司 | The preparation method of sweet juice composition |
| CN110214886B (en) * | 2012-08-07 | 2021-10-26 | 桂林吉福思罗汉果生物技术股份有限公司 | Process for preparing sweet juice composition |
| CN104059959A (en) * | 2013-03-20 | 2014-09-24 | 广西壮族自治区中国科学院广西植物研究所 | Method for synthesizing sweet saponin with bitter and fallen grosvenor momordica fruit as raw material |
| CN107397103A (en) * | 2017-08-25 | 2017-11-28 | 湖南华诚生物资源股份有限公司 | A kind of preparation method of Momordica grosvenori decolouring flavor inspissated juice |
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Effective date of registration: 20090327 Address after: 89, West Hangzhou Road, Hubei, Huangshi Province, China: 550001 Applicant after: Department of Hubei special biomedical Technology Co., Ltd. Address before: School of life science, Southern District of Guizhou University, Guizhou, Guiyang: 550025 Applicant before: Zhou Ying |
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