CN101690573A - Production method of fructus monordicae extract with over 60% of mogroside V content - Google Patents
Production method of fructus monordicae extract with over 60% of mogroside V content Download PDFInfo
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- CN101690573A CN101690573A CN200910044558A CN200910044558A CN101690573A CN 101690573 A CN101690573 A CN 101690573A CN 200910044558 A CN200910044558 A CN 200910044558A CN 200910044558 A CN200910044558 A CN 200910044558A CN 101690573 A CN101690573 A CN 101690573A
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- fructus momordicae
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- Saccharide Compounds (AREA)
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Abstract
The invention provides a production method of fructus monordicae extract with over 60% of mogroside V content. In the method, the fresh momordica grosvenori is subjected to the following technique processes: smashing, saccharification, extraction by water, concentration, sedimentation and centrifugation, ion exchange resin refining, macroporous resin refining, concentration, aluminum oxide refining, concentration, spray drying and finishing product. The method can produce high-quality fructus monordicae extract products, reduce material loss, shorten period of production, increase product yield, lower production cost, and is suitable for industrial production. The mogroside V content in the fructus monordicae extract produced by the method is more than or equal to 60%; the fructus monordicae extract has high product purity, single composition, pure white color, good color and taste, fresh and cool sweet taste like that of sugar, simultaneously overcomes the technical problem for industrial production of the high-content and high-quality fructus monordicae extract, and successfully realizes large-scale production.
Description
Technical field
The invention belongs to effective ingredients in plant separation and extraction technology field, be specifically related to a kind of momordica grosvenori glycoside V content greater than 60% Fructus Monordicae extract production method.
Background technology
The tradition traditional Chinese medicine proves, Momordica grosvenori has antibechic, eliminates the phlegm, relievings asthma, rushes down, protects the liver, transaminase lowering, adjusting gastrointestinal motor, strengthen the effect such as dental caries that causes of immune, hypotensive, reducing blood lipid, inhibition mutans streptococcus, take throughout the year, can promote longevity, so have purposes widely aspect clinical and the health care.Studies show that, Momordica grosvenori contains plurality of active ingredients, as the sugariness of mogroside 300 times of sucrose, heat but has only 1/50 of sucrose, be desirable sweetener raw material, add its significant pharmacologically active, make it have very high using value at beverage and candy, cosmetic industry, so now be widely used in food, health products, medicine, cosmetic industry, the crowd who is specially adapted to diabetes, hypertension, obese people and unsuitable sugar uses.
Contain multiple saponins active component in the Momordica grosvenori, leading indicator composition wherein is momordica grosvenori glycoside V (Mogroside V).Momordia grosvenori aglycone belongs to the triterpenoid saponin constituents in the plant chemical ingredient, the typical cucurbitane type of its aglycon tool tetracyclic triterpene structure, and momordica grosvenori glycoside V (Mogroside V) is the representative in this compounds, its structural formula is as follows:
The Momordica grosvenori saponins compound is insoluble in organic solvents such as acetone, ethyl acetate owing to be combined with glycosyl and soluble in water, ethanol isopolarity solvent, is white amorphous powder.
The general production process route of Fructus Monordicae extract is: water is carried, is concentrated, filtration, macroporous absorbent resin are refining, concentrate system cream, spray-drying.By to the careful design of specific production technology with to Parameter Optimization, can obtain the Fructus Monordicae extract of different quality grade.
Also be rich in polysaccharide composition and protide chemical compositions such as protein, amino acid such as pectin, lymphatic temperament in the Momordica grosvenori, the existence of these compositions has a strong impact on the extraction and the separation and purification of Momordica grosvenori saponin active ingredient.In addition, the saponins compound in the Momordica grosvenori has foaming characteristic, easily forms colloidal solution, strengthens the difficulty of separation and purification; Add the synergistic function of compositions such as polysaccharide such as pectin in the fruit and protein, make extract in concentration process, produce a large amount of foams and be difficult to concentrate paramount solid content, the material phenomenon often takes place to run, obviously reduce product yield foam.The specification of present commercially available Fructus Monordicae extract is mainly momordica grosvenori glycoside V 25%, 30%, 40%, the supply of the momordica grosvenori glycoside V of high-load is not enough far away, and quality is relatively poor, mostly be milky to ivory buff, off-white color product, Shang Weijian has pure white and momordica grosvenori glycoside V content greater than 60% Fructus Monordicae extract.As main functional component in the Momordica grosvenori saponin(e and quality index composition, Fructus Monordicae extract is made with extra care, further improve the content of momordica grosvenori glycoside V, optimize the properties of product of Fructus Monordicae extract, beautify process optimization such as its color and luster and be very important.
A lot of about Fructus Monordicae extract Study on Production Technology report both at home and abroad, but industrialized producing technology of the momordica grosvenori glycoside V of high-load and products thereof is not met generation.This explanation, existing technical research still is in laboratory level, can't really reach industrialized production and marketing level.And the high-quality Momordia grosvenori aglycone extract of suitability for industrialized production high-load need overcome following technological difficulties: (1) reduces the interference of foamers such as pectin, protein, reduces the production difficulty, reduces loss of material; (2) separation and purification Momordica grosvenori saponin monomer class material, it is more single to obtain composition, the high and high-load momordica grosvenori glycoside V product that has good mouthfeel and present pure white color and luster of momordica grosvenori glycoside V content.
Summary of the invention
The object of the present invention is to provide a kind of momordica grosvenori glycoside V content greater than 60% Fructus Monordicae extract production method.Use this method can produce high-quality Fructus Monordicae extract, reduce loss of material, shorten the production cycle, improve product yield, reduce production costs, and be suitable for suitability for industrialized production.Utilize momordica grosvenori glycoside V 〉=60% in the Fructus Monordicae extract that this method produces, the product purity height, composition is more single, and color is pure white, and color and luster is good, and mouthfeel is good, and it has the salubrious sweet taste as the sucrose.
A kind of momordica grosvenori glycoside V content may further comprise the steps greater than 60% Fructus Monordicae extract production method:
1) saccharification: get fresh fructus momordicae 1000Kg fragmentation, the carbohydrase that will account for fresh fructus momordicae weight 3-7wt ‰ then is dissolved in the 1000L running water, the fresh fructus momordicae of fragmentation is put into wherein to stir then, places 2-4h in 35 ℃-45 ℃ insulations;
2) water extracts and concentrates: the fresh fructus momordicae with saccharification after good extracts with running water; Extract 3 times in temperature more than 90 ℃, add the running water of 5 times of volumes of raw material for the first time, extraction time is 1.5h, filters; Filter residue enters for the second time and extracts, and adds the running water of 4 times of volumes of raw material, and extraction time is 1.0h, filters; Filter residue enters for the third time and extracts, and adds the running water of 3 times of volumes of raw material weight, and extraction time is 0.5h, filters; Merge and extract the filtrate vacuum decompression for 3 times and be concentrated into 4 times of the fresh fructus momordicae weight that feeds intake below 75 ℃;
3) sedimentation is centrifugal: the extract 2000～4000r/min sedimentation centrifugation 2h after concentrating;
4) ion exchange resin is refining: the D-201 strong-base anion-exchange resin that will the account for fresh fructus momordicae quality 1/10 in advance resin column of packing into, then with centrifugate by resin column, collect and flow out liquid, be washed till no sweet taste with purified water again till, merge all outflow liquid;
5) macroreticular resin is refining: the ADS-17 macroporous absorbent resin that will account for 0.4 times of fresh fructus momordicae quality is in advance packed in the resin column, will pass through resin column through the eluent behind the ion exchange resin again; Be washed till with purified water again and flow out the liquid water white transparency, use 55% edible ethanol desorb at last, collect stripping liquid till do not have a sweet taste;
7) concentrate to reclaim ethanol: the stripping liquid vacuum decompression is concentrated into 0.5 times of the fresh fructus momordicae weight that feeds intake below 75 ℃;
7) aluminium oxide is refining: the aluminium oxide that will account for fresh fructus momordicae quality 1/25 is in advance packed in the resin column, simultaneously concentrate is diluted to 1000L with purified water; Then dilution is passed through alumina column, collect and all flow out liquid, wash post to only having sweet taste with purifying again, collect all and flow out liquid;
8) concentrated and spray-drying: will flow out the liquid vacuum decompression and be concentrated to the 11-15 Baume below 75 ℃, spray-drying is made finished product again.
The invention advantage
1. the present invention carries out saccharification with raw material earlier before extraction, and be to extract earlier to carry out enzymolysis again in the conventional art, saccharifying is incorporated in the Momordica grosvenori extraction process first, with the enzymolysis in the conventional art diverse action principle is arranged, utilize carbohydrase (to shorten to maturation and the saccharogenesis conversion that Momordica grosvenori is quickened in saccharification 2～4h) in 10 days at short notice from place in the past, make its epidermis by the dark green yellow green that transfers to, and a type glucose in the carbohydrase energy enzymolysis glycoside material molecule, increased sugariness, help improving the content of momordica grosvenori glycoside V, this process does not play any destruction to momordica grosvenori glycoside V again, thereby can more effectively improve product yield; The synchronous glycosylation enzyme polysaccharose substances such as part pectin in the fresh fructus momordicae, starch of can also degrading help the leaching and the separation of active component; Simultaneously can help controlling the phenomenon of bubbling and running material in the production process.This method is a new trial of producing Fructus Monordicae extract technology, facts have proved improving production process, the effect highly significant.
2. the present invention adopts macroporous strong basic anion exchange resin that feed liquid is decoloured, and can remove the pigment and the small-molecule substance of feed liquid the inside preferably, thereby optimizes product color, accomplishes the milk white products, improves product purity; And the macroporous strong basic resin anion (R.A.) is handled easily than weak anion resin regeneration, and the soda acid processing time shortens more than the 4h, and longer service life generally can be regenerated more than 500 times, and this also just greatly reduces production cost; In addition, adopt macroporous resin adsorption that feed liquid is made with extra care, removed polysaccharide compositions such as pectin, lymphatic temperament and protein, amino acid whose protide composition fully, made the purity of Fructus Monordicae extract further improve, and realized remarkable advantage low in calories.In addition, macroporous absorbent resin is refining further to shoal product colour, plays the effect of separation and purification.The inventor makes a large amount of experiments, has determined chromatography condition, has realized suitability for industrialized production.In the technology in the past, be refining with macroreticular resin earlier, spent ion exchange resin decolouring again, the present invention is then opposite, and the macroreticular resin secondary refining operation in the operation has in the past been removed on the one hand in such technological process, thereby shortened refining operation and the operating time, save production cost, and product color is more shallow, has realized that solution colour is for extremely shallow faint yellow; On the other hand, earlier pass through macroreticular resin again, can obviously shorten more than the charging of the macroreticular resin washing time 5h after intact through ion exchange resin.Because after the advanced ion exchange resin of concentrate, a large amount of pigments are removed, Momordica grosvenori active ingredient flows out the ion exchange resin post, and then advance macroporous resin column, Momordica grosvenori active ingredient is by macroporous resin adsorption, and material is not adsorbed substantially in the solution of all the other very slight color, directly flows out macroporous resin column, be very easy to flow out liquid when also just making the washing macroreticular resin and be washed till water white transparency, this process shortens 5h approximately; The third aspect, this technology has been saved the consumption of macroreticular resin, has improved the utilization rate of resin.Because most Momordica grosvenori pigment and Momordica grosvenori active ingredient can be by macroporous resin adsorption, there is competitive Adsorption in both, and earlier by after the ion exchange resin, most of pigment is removed, make with purer can being adsorbed effectively, improved adsorption efficiency and resin utilization rate by the Momordica grosvenori active ingredient of macroporous resin adsorption.Operation Just because of this makes that just the refining effect of product is better.
3. first that aluminium oxide is the refining process of the present invention is introduced in the Momordica grosvenori extraction process, discovery utilizes aluminium oxide further to remove remaining grosvenor momordica flavonoid and other pigment, and the effect that obtains is fine, when improving product content, key is obviously to have improved color and luster, accomplishes pure white.This is first the resin decolorization method to be combined with adsorption decoloring method.
4. to carry out sedimentation before concentrating centrifugal in the present invention, can effectively shorten the production time, reduces the operating pressure that concentrates and increase work efficiency, and whole production technology can efficiently be carried out fast.
5. the present invention improves the brand-new production technology that obtains on existing technology path, each link has all been carried out the parameter designing and the optimization of detail, the solid-liquid ratio that extracts, extraction time and number of times are all through repeatedly determining after experiment and the production practices optimization, guaranteed to extract more completely, make product quality effectively be promoted, and can't to production equipment or operation any special unapproachable requirement be arranged because of new technology, each step operation is all easy to implement, the operating cost of especially several committed steps is not high, more helps the carrying out of plant produced and the reduction of production cost.
6. the Fructus Monordicae extract that utilizes the present invention to produce, break through the bottleneck of Fructus Monordicae extract suitability for industrialized production, obtain momordica grosvenori glycoside V 〉=60%, color is lily high-load Fructus Monordicae extract, improve the mouthfeel of high-load Fructus Monordicae extract, make it have salubrious sweet taste as the sucrose; Solve the technological difficulties that suitability for industrialized production is researched and developed in experiment, becoming in the market, added value of product has satisfied the needs of problems of market to high-quality Fructus Monordicae extract product than higher Fructus Monordicae extract product.For society creates good economic benefit and social benefit.
The specific embodiment
Following examples are intended to further specify the present invention, rather than limitation of the present invention.
Embodiment 1:
1) saccharification: get fresh fructus momordicae 1000kg, drop in the extractor (being advisable not smash seed) broken back; It is moistening to add 1000L running water (with the dissolving of 4.0kg carbohydrase wherein, stirring in advance) immersion, stirs, and places 2h in 40 ℃ of insulations.
The kind that adds enzyme is a carbohydrase; The consumption of carbohydrase is fresh fructus momordicae 4.0kg per ton, and weight ratio is 4 ‰;
2) water extracts: the fresh fructus momordicae with saccharification after good carries out 3 extractions with running water in temperature more than 90 ℃.Add for the first time the running water of 5 times of volumes of raw material weight, extraction time is 1.5h, filters; Filter residue enters for the second time and extracts, and adds the running water of 4 times of volumes of raw material weight, and extraction time is 1.0h, filters; Filter residue enters for the third time and extracts, and adds the running water of 3 times of volumes of raw material weight, and extraction time is 0.5h, filters.Merge 3 extraction filter filtrates and enter next process.
3) concentrate: will extract the filtrate vacuum decompression and be concentrated into 4 times of the fresh fructus momordicae weight that feeds intake below 75 ℃.Be that the 1000kg fresh fructus momordicae is concentrated into 4000L.
4) sedimentation is centrifugal: extract sedimentation centrifuge sedimentation separation 2h, rotating speed 2000～4000r/min.
5) ion exchange resin is refining: the resin column of in advance the D201 strong-base anion-exchange resin of 100kg being packed into, then centrifugate is passed through resin column, and collect and flow out liquid, be washed till no sweet taste with purified water again and end, merge all and flow out liquid.Ion exchange resin and fresh fructus momordicae weight ratio are 1: 10, i.e. 1000kg fresh fructus momordicae 100kg ion exchange resin;
6) macroreticular resin is refining: in advance the ADS-17 macroporous absorbent resin of 400kg is packed in the resin column, will pass through resin column through the eluent behind the ion exchange resin again; After feed liquid is all passed through, be washed till outflow liquid water white transparency, use 55% alcohol desorption again, collect stripping liquid and end to there being sweet taste with purified water.
Macroreticular resin and fresh fructus momordicae weight ratio are 1: 2.5, i.e. 1000kg fresh fructus momordicae 400kg macroreticular resin;
7) concentrate: stripping liquid liquid vacuum decompression is concentrated into 0.5 times of the fresh fructus momordicae weight that feeds intake below 75 ℃.Be that the 1000kg fresh fructus momordicae is concentrated into 500L.
8) aluminium oxide is refining: in advance the 40kg aluminium oxide is packed in the resin column, simultaneously concentrate is diluted to 1000L with purified water; Then dilution is passed through alumina column, collect and all flow out liquid, wash post to only having sweet taste with purifying again, collect all and flow out liquid.
Diluted concentration: promptly be diluted to 1 times of heavy amount volume of the fresh fructus momordicae that feeds intake; Supplementary product consumption: 25: 1, i.e. 1000kg fresh fructus momordicae 40kg aluminium oxide.
9) concentrate: will flow out the liquid vacuum decompression and concentrate the 11-15 Baume below 75 ℃.
10) spray-drying: the concentrate spray-drying is made finished product.
Embodiment 2:
Embodiment is identical with embodiment 1, only changes: during saccharification, add the 5Kg carbohydrase in 1000L water, the saccharification condition is 35 ℃, insulation 4h.
Embodiment 3:
Embodiment is identical with embodiment 1, only changes: during saccharification, add the 7Kg carbohydrase in 1000L water, the saccharification condition is 45 ℃, insulation 3h.
Obtaining product specification according to the embodiment of the invention is the lily amorphism powder of momordica grosvenori glycoside V 〉=60%, color; Output 4.0-6.5kg, yield 0.40%-0.65%.
Claims (1)
1. a momordica grosvenori glycoside V content is characterized in that greater than 60% Fructus Monordicae extract production method, may further comprise the steps:
1) saccharification: get fresh fructus momordicae 1000Kg fragmentation, the carbohydrase that will account for fresh fructus momordicae weight 3-7wt ‰ then is dissolved in the 1000L running water, the fresh fructus momordicae of fragmentation is put into wherein to stir then, places 2-4h in 35 ℃-45 ℃ insulations;
2) water extracts and concentrates: the fresh fructus momordicae with saccharification after good extracts with running water; Extract 3 times in temperature more than 90 ℃, add the running water of 5 times of volumes of raw material for the first time, extraction time is 1.5h, filters; Filter residue enters for the second time and extracts, and adds the running water of 4 times of volumes of raw material, and extraction time is 1.0h, filters; Filter residue enters for the third time and extracts, and adds the running water of 3 times of volumes of raw material weight, and extraction time is 0.5h, filters; Merge and extract the filtrate vacuum decompression for 3 times and be concentrated into 4 times of the fresh fructus momordicae weight that feeds intake below 75 ℃;
3) sedimentation is centrifugal: the extract 2000～4000r/min sedimentation centrifugation 2h after concentrating;
4) ion exchange resin is refining: the D-201 strong-base anion-exchange resin that will the account for fresh fructus momordicae quality 1/10 in advance resin column of packing into, then with centrifugate by resin column, collect and flow out liquid, be washed till no sweet taste with purified water again till, merge all outflow liquid;
5) macroreticular resin is refining: the ADS-17 macroporous absorbent resin that will account for 0.4 times of fresh fructus momordicae quality is in advance packed in the resin column, will pass through resin column through the eluent behind the ion exchange resin again; Be washed till with purified water again and flow out the liquid water white transparency, use 55% edible ethanol desorb at last, collect stripping liquid till do not have a sweet taste;
6) concentrate to reclaim ethanol: the stripping liquid vacuum decompression is concentrated into 0.5 times of the fresh fructus momordicae weight that feeds intake below 75 ℃;
7) aluminium oxide is refining: the aluminium oxide that will account for fresh fructus momordicae quality 1/25 is in advance packed in the resin column, simultaneously concentrate is diluted to 1000L with purified water; Then dilution is passed through alumina column, collect and all flow out liquid, wash post to only having sweet taste with purifying again, collect all and flow out liquid;
8) concentrated and spray-drying: will flow out the liquid vacuum decompression and be concentrated to the 11-15 Baume below 75 ℃, spray-drying is made finished product again.
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