CN104069152A - Preparation method of extract with high mogroside IV content - Google Patents
Preparation method of extract with high mogroside IV content Download PDFInfo
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- CN104069152A CN104069152A CN201410245164.0A CN201410245164A CN104069152A CN 104069152 A CN104069152 A CN 104069152A CN 201410245164 A CN201410245164 A CN 201410245164A CN 104069152 A CN104069152 A CN 104069152A
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Abstract
The invention provides a preparation method of an extract with high mogroside IV content. The preparation method is characterized by using fresh momordica grosvenori as the raw material and adopts the following processing steps: momordica grosvenori grinding, extraction, filtration, filtrate obtainment, membrane separation, adsorption separation, elution 1, ethanol recovery 1, decoloration with resin, drying, obtainment of coarse products of momordica glycosides, dilution with water, adsorption with macroporous resin, elution 2, ethanol recovery 2, drying under reduced pressure and obtainment of the momordica grosvenori extract, wherein the fresh momordica grosvenori with fruit age of 30-50 days is adopted and is subjected to grinding, extraction, filtration, membrane separation, adsorption separation, elution, ethanol recovery, decoloration with resin and drying, thus obtaining the coarse products of momordica glycosides; the coarse products of momordica glycosides are further adsorbed by adopting macroporous resin, a 70% ethanol solution is used for selective elution for 100 minutes, ethanol is recovered and drying is carried out, thus obtaining the momordica grosvenori extract with mogroside IV content of 15-55%.
Description
Technical field
The present invention relates to field of plant extraction, especially a kind of preparation method of Fructus Momordicae extract.
Background technology
Fructus Momordicae is Cucurbitaceae herbaceous perennial vine plant, is the first batch of medicine-food two-purpose rare Chinese medicine of announcing of Ministry of Public Health, is described as " angle fruit " by people.Fructus Momordicae nutritive value is very high, and containing Fructus Momordicae glycoside, wherein mogroside V is the main component of Fructus Momordicae dry fruit, accounts for 0.5% of dry fruit.Mogroside IV content is little, within 30-50 in age days, is that content is higher fruit, in maturation process, fades away, and does not substantially contain mogroside IV in mellow fruit.Contain in addition glucose, fructose, polysaccharide, protein, aminoacid, flavonoid glycosides, vitamin C and multiple mineral element, there is sweet in the mouth cool in nature, return lung, large intestine channel, there is nourishing the lung to arrest cough, effect of promoting the production of body fluid to quench thirst, be applicable to lung-heat or xeropulmonary cough, pertussis and summer-heat impairment of body fluid are thirsty etc., also have in addition effect of loosening bowel to relieve constipation.Fructus Momordicae deep processing is mainly to extract Fructus Momordicae glycoside.Chinese invention patent application publication number is CN101007042A, discloses a kind of decolouring, debitterize, containing the method for preparing extractive of Fructus Momordicae glycoside, but does not mention mogroside IV content.
Summary of the invention
Technical problem to be solved by this invention is to provide the high method for preparing extractive of a kind of mogroside IV content, can obtain one by the method has obvious inhibiting Fructus Momordicae extract to hepatitis C virus (HCV), can be used as the medicine material of prophylactic treatment hepatitis C.
In order to solve this technical problem, the technical scheme that the present invention takes is:
Taking the new fresh Fructus Momordicae in 30-50 days fruit ages as raw material, adopt and extract, membrance separation, chromatographic column, the technology such as dry, obtain the Fructus Momordicae extract that mogroside IV content is 15-55%.Concrete technology flow process is as follows:
Fructus Momordicae → grinding → extraction → filtration → filtrate → membrance separation → adsorbing separation → eluting 1 → ethanol reclaims 1 → resin decolorization → dry → Momordica-Glycosides crude product → water dilution → macroporous resin adsorption → eluting 2 → ethanol and reclaims the Fructus Momordicae extract that 2 → drying under reduced pressure → mogroside IV content is 15%-55%.
Described Fructus Momordicae is that to adopt fruit age be the fresh Fructus Momordicae of 30-50 days;
Described grinding is the water that adds 2 times of Fructus Momordicae weight, grinds with grater;
Described extraction is 20% alcoholic solution that adds again 6 times of Fructus Momordicae weight, carries out ultrasound wave reflux, extract, 1-2 hour; Filter, then repeat 2 times, merge to obtain extracting solution;
The ultrafilter membrane that described membrance separation is 1000 by extracting solution with molecular cut off is tentatively concentrated, obtains concentrated solution 1,
Described adsorbing separation is that concentrated solution 1 is injected to AB-8 adsorption resin column, discards post effluent; After having adsorbed, be eluted to post effluent as colourless taking 20% alcoholic solution of 2 times of bed volumes;
Described eluting 1 is the 75% alcoholic solution eluting with 3.5 times of bed volumes, collects eluent 1.
It is that the ethanol reduction vaporization in eluent 1 is reclaimed and obtains extractum that described ethanol reclaims 1;
Described resin decolorization is to add water by reclaiming the later extractum of ethanol, through D-280 ion-exchange resin decolorization;
Described being dried is by post effluent drying under reduced pressure, obtains light yellow product, i.e. Momordica-Glycosides crude product.
Described macroporous resin adsorption is by dilute with water 10-20 times again of Momordica-Glycosides crude product, again adopts macroporous resin adsorption to separate, and resin is selected D201, or HPD100;
Described eluting 2 is selective elution; With 70% alcoholic solution eluting, elution time is 100 minutes, collects eluent 2; Ethanol in eluent 2, after reduction vaporization reclaims, is obtained to concentrated solution 2; Also can be after absorption finishes, first control is 80 minutes by 70% alcoholic solution elution time, eluent is separately used as him, use again 70% alcoholic solution eluting, the elution time of controlling eluent is 100 minutes, collect this eluent, the ethanol in this eluent, after reduction vaporization reclaims, is obtained to concentrated solution 2; This time can also be with 70% alcoholic solution eluting after eluting, the material such as elution time is 120 minutes, collects eluent, recovery mogroside V;
Described drying under reduced pressure is that concentrated solution 2 is carried out to drying under reduced pressure, obtains white or light yellow product, obtains the Fructus Momordicae extract that mogroside IV content is 15%-55%.
Described grind, extract, filtration, membrance separation, adsorbing separation, resin decolorization, eluting, ethanol are reclaimed, dry be all known technology.
The present invention has following advantages and characteristic:
1, mogroside IV content is high.
Mogroside IV content in fresh fruit is extremely low, and by technical solution of the present invention, mogroside IV content can reach 15-55%.
2, combination technique novelty, creative.
Taking 30-50 days, really the new fresh Fructus Momordicae in age, as raw material, ensured mogroside IV content in raw material; Adopt extraction, filtration, membrance separation, adsorbing separation, by separating substances such as Fructus Momordicae glycoside material and saccharides, preliminary purification, obtains Momordica-Glycosides crude product; By Momordica-Glycosides crude product dilute with water, adopt macroporous resin adsorption, with 70% alcoholic solution selective elution, elution time is 100 minutes; Or first control is 80 minutes by 70% alcoholic solution elution time, and eluent is separately used as him, then uses 70% alcoholic solution eluting, the elution time of controlling eluent is 100 minutes, collects this eluent; This eluting be for mogroside IV is separated with other Fructus Momordicae glycoside materials, purification; Eluent 2 is carried out to ethanol recovery, dry, obtain the Fructus Momordicae extract that mogroside IV content is 15-55%.Visible, after these technical combinations, support mutually, indispensable, combined effect, just can obtain the Fructus Momordicae extract that mogroside IV content is 15-55%, Welded joint is not known technology, is not simple stack, has outstanding substantive distinguishing features and significant progressive.
Detailed description of the invention
The following stated example understands the present invention in detail.
Embodiment 1
The new fresh Fructus Momordicae 100kg that takes 50 days fruit ages, adds 200kg water, Fructus Momordicae and water one is reinstated to grater and grind; Proceed in the ultrasonic extraction tank of 1 ton, and then add 20% alcoholic solution of 600kg, carry out ultrasound wave reflux, extract, 1 hour; Extraction finishes rear filtration, obtains filtrate; Fructus Momordicae filtering residue is added to 20% alcoholic solution of 600kg again, repeat to extract 3 times, merge the filtrate of gained, obtain extracting solution 1; By the ceramic membrane filter of extracting solution 1 use 0.45 μ m, obtain micro-filtrate, the ultrafilter membrane that is 1000 with molecular cut off by micro-filtrate carries out ultrafiltration, collects ultrafiltration trapped fluid, obtains concentrated solution 1; Concentrated solution 1 is injected to AB-8 adsorption resin column, discard post effluent; After having adsorbed, be eluted to post effluent as colourless taking 20% alcoholic solution of 2 times of bed volumes; By 75% alcoholic solution eluting of 3.5 times of bed volumes, collect eluent 1 again; Ethanol reduction vaporization in eluent 1 is reclaimed and obtains extractum; The water that the later extractum of recovery ethanol is added to 10 times of weight, through D-280 ion-exchange resin decolorization, by post effluent drying under reduced pressure, obtains light yellow product, i.e. Momordica-Glycosides crude product.Momordica-Glycosides crude product 20 times of dilute with waters again; Use D201 macroporous resin adsorption; After absorption finishes, with 70% alcoholic solution eluting, the elution time of controlling eluent is 100 minutes, collects eluent 2; Ethanol in eluent 2, after reduction vaporization reclaims, is obtained to concentrated solution 2; Concentrated solution 2 is carried out to drying under reduced pressure, obtain light yellow product, will detect.Mogroside IV content is 15.5%.
Embodiment 2
The new fresh Fructus Momordicae 100kg that takes 40 days fruit ages, adds 200kg water, Fructus Momordicae and water one is reinstated to grater and grind; Proceed in the ultrasonic extraction tank of 1 ton, and then add 20% alcoholic solution of 600kg, carry out ultrasound wave reflux, extract, 2 hours; Extraction finishes rear filtration, obtains filtrate; Fructus Momordicae filtering residue is added to 20% alcoholic solution of 600kg again, then repeat to extract 2 times, merge the filtrate of gained, obtain extracting solution 1; By the ceramic membrane filter of extracting solution 1 use 0.22 μ m, obtain micro-filtrate, the ultrafilter membrane that is 1000 with molecular cut off by micro-filtrate carries out ultrafiltration, collects ultrafiltration trapped fluid, obtains concentrated solution 1; Concentrated solution 1 is injected to AB-8 adsorption resin column, discard post effluent; After having adsorbed, be eluted to post effluent as colourless taking 20% alcoholic solution of 2 times of bed volumes; By 75% alcoholic solution eluting of 3.5 times of bed volumes, collect eluent 1 again; Ethanol reduction vaporization in eluent 1 is reclaimed and obtains extractum; The later extractum of recovery ethanol is added to the water of 10 times of weight, through D-280 ion-exchange resin decolorization, by 2 times of post effluent dilute with waters; Use HPD100 macroporous resin adsorption; After absorption finishes, with 70% alcoholic solution eluting, the elution time of controlling eluent is 100 minutes, collects eluent 2; Ethanol in eluent 2, after reduction vaporization reclaims, is obtained to concentrated solution 2; Concentrated solution 2 is carried out to drying under reduced pressure, obtain light yellow product, will detect.Mogroside IV content is 40.2%.
Embodiment 3
The new fresh Fructus Momordicae 100kg that takes 30 days fruit ages, adds 200kg water, Fructus Momordicae and water one is reinstated to grater and grind; Proceed in the ultrasonic extraction tank of 1 ton, and then add 20% alcoholic solution of 600kg, carry out ultrasound wave reflux, extract, 1 hour; Extraction finishes rear filtration, obtains filtrate; Fructus Momordicae filtering residue is added to 20% alcoholic solution of 600kg again, then repeat to extract 2 times, merge the filtrate of gained, obtain extracting solution 1; By the ceramic membrane filter of extracting solution 1 use 0.45 μ m, obtain micro-filtrate, the ultrafilter membrane that is 1000 with molecular cut off by micro-filtrate carries out ultrafiltration, collects ultrafiltration trapped fluid, obtains concentrated solution 1; Concentrated solution 1 is injected to AB-8 adsorption resin column, discard post effluent; After having adsorbed, be eluted to post effluent as colourless taking 20% alcoholic solution of 2 times of bed volumes; By 75% alcoholic solution eluting of 3.5 times of bed volumes, collect eluent 1 again; Ethanol reduction vaporization in eluent 1 is reclaimed and obtains extractum; The later extractum of recovery ethanol is added to the water of 10 times of weight, through D-280 ion-exchange resin decolorization.Extractum also can obtain Momordica-Glycosides crude product by convection drying, after 20 times of Momordica-Glycosides crude product thin ups, carries out D-280 ion-exchange resin decolorization.By 2 times of post effluent dilute with waters; Use HPD100 macroporous resin adsorption; After absorption finishes, with 70% alcoholic solution eluting, first control is 80 minutes by 70% alcoholic solution elution time, and eluent is separately used as him, then uses 70% alcoholic solution eluting, and the elution time of controlling eluent is 100 minutes, collects this eluent 3; Ethanol in eluent 3, after reduction vaporization reclaims, is obtained to concentrated solution 2; Concentrated solution 2 is carried out to drying under reduced pressure, obtain light yellow product, will detect.Mogroside IV content is 55.0%.Can also control the alcoholic solution eluting with 70%, the elution time of controlling eluent is 120 minutes, collects this eluent, reclaims mogroside V.
Claims (3)
1. the high method for preparing extractive of mogroside IV content, taking fresh Fructus Momordicae as raw material, is characterized in that: adopt following processing step:
Fructus Momordicae → grinding → extraction → filtration → filtrate → membrance separation → adsorbing separation → eluting 1 → ethanol reclaims 1 → resin decolorization → dry → Momordica-Glycosides crude product → water dilution → macroporous resin adsorption → eluting 2 → ethanol and reclaims 2 → drying under reduced pressure → Fructus Momordicae extract;
Described Fructus Momordicae is that to adopt fruit be 30-50 days age;
Described grinding is the water that adds 2 times of Fructus Momordicae weight, grinds with grater;
Described extraction refers to 20% alcoholic solution that adds again 6 times of Fructus Momordicae weight, carries out ultrasound wave reflux, extract, 1-2 hour; Filter, repeat 3 times, merge to obtain extracting solution;
Extracting solution is first used microfiltration of ceramic membrane by described membrance separation, obtains micro-filtrate, then the ultrafilter membrane that is 1000 with molecular cut off is tentatively concentrated, obtains concentrated solution 1;
Described adsorbing separation is that concentrated solution 1 is injected to AB-8 adsorption resin column, discards post effluent; After having adsorbed, be eluted to post effluent as colourless taking 20% alcoholic solution of 2 times of bed volumes;
Described eluting 1 is the 75% alcoholic solution eluting with 3.5 times of bed volumes, collects eluent 1;
It is that the ethanol reduction vaporization in eluent 1 is reclaimed and obtains extractum that described ethanol reclaims 1;
Described resin decolorization is to add water by reclaiming the later extractum of ethanol, through D-280 ion-exchange resin decolorization;
By post effluent drying under reduced pressure, obtain light yellow product, i.e. Momordica-Glycosides crude product;
Described macroporous resin adsorption is to adopt adsorbing separation again, and resin is selected D201, or HPD100;
Described eluting 2 is the alcoholic solution eluting with 70%, and elution speed is 100 minutes, collects eluent 2; Ethanol in eluent 2, after reduction vaporization reclaims, is obtained to concentrated solution 2,
Described drying under reduced pressure is that concentrated solution 2 is carried out to drying under reduced pressure, obtains white or light yellow product, obtains the Fructus Momordicae extract that mogroside IV content is 15%-55%.
2. method according to claim 1, is characterized in that: described microfiltration, the aperture of micro-filtration membrane is controlled at 022-0.45 μ m.
3. method according to claim 1, it is characterized in that: described eluting 2, after referring to that absorption finishes, with 70% alcoholic solution eluting, first control is 80 minutes by 70% alcoholic solution elution time, and eluent is separately used as him, then uses 70% alcoholic solution eluting, the elution time of controlling eluent is 100 minutes, collects this eluent.
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Cited By (3)
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| CN104762132A (en) * | 2015-03-05 | 2015-07-08 | 云南中烟工业有限责任公司 | Preparation method and application of Siraitia grosvenorii extract |
| CN106176888A (en) * | 2016-09-27 | 2016-12-07 | 桂林益天成生物科技有限公司 | Without returning the extracting method of bitterness Momordica-Glycosides |
| WO2018196476A1 (en) * | 2017-04-25 | 2018-11-01 | 广西甙元植物制品有限公司 | Process for preparing decolored concentrated fresh momordica grosvenori juice |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104762132A (en) * | 2015-03-05 | 2015-07-08 | 云南中烟工业有限责任公司 | Preparation method and application of Siraitia grosvenorii extract |
| CN106176888A (en) * | 2016-09-27 | 2016-12-07 | 桂林益天成生物科技有限公司 | Without returning the extracting method of bitterness Momordica-Glycosides |
| WO2018196476A1 (en) * | 2017-04-25 | 2018-11-01 | 广西甙元植物制品有限公司 | Process for preparing decolored concentrated fresh momordica grosvenori juice |
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