CN1436786A - Extraction process of mangosteen glycoside from mangosteen - Google Patents
Extraction process of mangosteen glycoside from mangosteen Download PDFInfo
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- CN1436786A CN1436786A CN 03117430 CN03117430A CN1436786A CN 1436786 A CN1436786 A CN 1436786A CN 03117430 CN03117430 CN 03117430 CN 03117430 A CN03117430 A CN 03117430A CN 1436786 A CN1436786 A CN 1436786A
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Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The extraction process of mangosteen glycoside from fresh mangosteen fruit has water as extracting solvent and includes mainly microfiltering, ultrafiltering and nano filtering. The microfiltering is with porous filtering membrane of 0.05-0.3 micron pores; the ultrafiltering is to use hollow fiber ultrafiltering membrane for intercepting matter of molecular weight 20000-80000; and the nano filtering is to use nano filtering membrane for intercepting matter of molecular weight 100-400 or is to concentrate with RO reverse osmosis apparatus. The process is performed under low temperature condition, and this results in good product color, dissolvability, clarity and taste, less loss of active components, lowered power consumption and cost, high product yield and quality.
Description
(1) technical field:
The present invention relates to a kind of biological extraction process, particularly a kind of method of extraction separation Momordica-Glycosides.
(2) background technology:
Momordica-Glycosides is as the natural product of higher-grade of a kind of unique security and nutrient health-care function, compare with medicine, healthcare products, cosmetic material and the artificial sweetening agent of synthetic, though its price height has the high cost performance advantage, will have the very strong market competitiveness.
The trend of back to nature has caused the consumption boom of natural product, and the excessive use of synthetic product can produce toxic side effect, often is strictly controlled.Momordica-Glycosides is compared with natural sweetenerss such as stevioside, oligose, sugar alcohol on the market, except going even farther aspect the sweet low-heat of height, also have quality better, Heat stability is good, taste novelty, pure taste uniqueness, use advantage and unique nourishing function such as simple, edible safety.Illness patients such as obesity, diabetes, carious tooth are not needed to limit intake.Get a good chance of in sugar-free low hot drink, sugar-free candy and sugar-free chewing gum market, taking a share.Momordica-Glycosides is the strong sweetener of sugar-free low-heat, and mouthfeel is good, is usually used in the seasonings of food, beverage, should be used as the sweeting agent in sugar-free low hot drink, sugar-free candy and the sugar-free chewing gum; Be used as diabetics's assisting therapy product again in a large number as the sugar-free sweeting agent.Simultaneously the stevioside that Momordica-Glycosides and present China export volume are bigger is compared, and is original and to have thousands of years use historical and accept for the people easily to the health-care treatment of human body, so have stronger competitive power in the high-end market expectation.Momordica-Glycosides has advantage and unique nourishing functions such as high sweet low-heat, edible safety.
Momordica-Glycosides has treatment Whooping cough, phlegm-fire cough, the dry constipation of blood, and acute and chronic bronchitis and tonsillitis promote multiple efficacies such as functions of intestines and stomach.Modern medicine proves, also contain multiple scavenger (scavenging agent) material in the Grosvenor Momordica, can remove the intravital active oxygen of people effectively, so can prevent and treat and cancer that assisting therapy is caused by free radical, hypertension, physiological pain, climacterium obstacle, cataract, gastritis, ulcer, constipation, eczema, pellagra or the like.In addition, Fructus Monordicae extract contains treatment coronary heart disease and angiosclerotic oleic acid of prevention and linolic acid etc.Grosvenor Momordica has also contained the composition of scavenging agent effect, by taking or put on the skin elimination lipofuscin (freckle, foxiness etc.) orally outward.Also can be used for bathing with the lipid peroxide in purifying the blood, improve whole skin metabolism.There is report to say that Grosvenor Momordica also can be used for the treatment of acne, obesity and fash alopecia.
But existing Grosvenor Momordica processing enterprise adopts traditional extraction process, traditional production technique is to be raw material with the dry fruit mostly, through organic solvent or water extraction, heats concentrating under reduced pressure with steam jacket, through the high speed centrifugation impurity elimination, use absorption with macroporous adsorbent resin, the organic solvent wash-out carries out concentrating under reduced pressure system cream again, spraying drying, or to adopt fresh Fructus Momordicae be raw material, adopts the Enzymatic Extraction technology, extracts Momordica-Glycosides from fresh Fructus Momordicae.In the traditional course of processing of Momordica-Glycosides, except that Momordica-Glycosides, remain in the extracting solution in a large amount of tannins, protein, starch, macromolecular substance and many particulates such as bacterium thermal source, submicron and floss etc., they are not effect not only, and have a strong impact on quality product, traditional high speed centrifugation, sedimentation, impurity-removing methods such as filtration, be difficult to it is removed fully, and product is heated through processing for a long time, and it is big to exist loss of effective components to destroy, appearance color is dark and difference is big, content's index is uneven, the sweet taste deficiency, mouthfeel is poor, water-soluble and clarity is poor, yield is low, problems such as cost height.
And traditional post adsorption separating method, it is long to operate loaded down with trivial details, extraction yield poor stability, production cycle, and loss of effective components is big, and the elution process of chromatography will consume ethanol, resin regeneration will consume soda acid, has not only increased cost, has also brought problem of environmental pollution.
In recent years, the research that new technologies such as membrane sepn are applied to extract effective ingredients in plant becomes increasingly active, and membrane separation technique is an emerging new and high technology, be referred to as in the world " 20 end of the centurys; mid-term 21 century is the most rising, even can cause one of great technology of the Industrial Revolution ".Because its process undergoing phase transition not, energy consumption is low, and the effective film area is big, the separation efficiency height, and the operational condition gentleness needn't be added chemical reagent, and is particularly suitable to the product that separates thermo-sensitivity and chemical substance is responded.But this technology mostly is in conceptual phase now, is not applied to scale production as yet, and utilizes the research and development of membrane separation technique extraction separation Momordica-Glycosides not appear in the newspapers.
(3) summary of the invention:
The present invention will disclose a kind of method of utilizing membrane separation technique extraction separation Momordica-Glycosides.
Membrane separation technique is to be separating medium with the selective permeation film, survey with film two to have certain impellent (as pressure difference, concentration difference), with mixing solutions be divided into keep liquid with by liquid two portions, thereby make different components separated.Momordica-Glycosides is a triterpene compound, is soluble in polar solvent, selects suitable separatory membrane according to the size of required molecular weight cut-off, just can reach the purpose of separation and purification Momordica-Glycosides.
Membrane sepn extracts the main technique flow process of Momordica-Glycosides technology: narrate a step below pre-treatment → extraction → concentrate → micro-filtration → ultrafiltration → nanofiltration → spraying drying → sterilising packaging respectively
Extract:
Because Momordica-Glycosides is triterpene compound, be soluble in polar solvent, as methyl alcohol, ethanol, water etc., but use methyl alcohol, ethanol equal solvent cost higher, and, do not meet food security standard, so should not adopt because the solvent itself that has is poisonous.Combine and consider to draw after the factors such as cost, edible safety and preferably adopt water as extraction solvent.
Extraction time is a key that influences yield and content, and general extraction time is 3～4 times, according to test, takes all factors into consideration the utilization ratio of extraction equipment usage space and the working substance content of finished product, and extraction time is preferably twice; The solvent consumption is 2～4 times, is preferably 3 times; Temperature is 40～100 ℃, and preferred 60～80 ℃, the best is 80 ℃, in case the effective constituent in the too high destruction extract of temperature.
Micro-filtration:
In order fully to effectively utilize the volume of equipment, can earlier extracting solution be concentrated the back and carry out micro-filtration, concentrate and preferably adopt vacuum concentration, vacuum concentration temperature preferably to be controlled at below 60 degree, to prevent that high temperature from concentrating product appearance and mouthfeel are exerted an influence.
The general millipore filtration that adopts 0.05 μ m～0.3 μ m aperture of microfiltration membrane, the millipore filtration in preferred 0.08 μ m～0.12 μ m aperture, preferably adopt the stainless steel millipore filtration in 0.1 μ m aperture, remove impurity such as water soluble protein, pectin and suspended substance most in the solution, reach the specification of quality of high-quality product.
Ultrafiltration:
The ultra-filtration membrane material that present membrane separation technique is mainly used has cellulose acetate (CA), polyacrylonitrile (PAN), polysulfones (PS), SPSF (SPS), polysulfones acyl ammonia (PSA) etc.By its affinity classification, be broadly divided into two classes: hydrophobic film material and hydrophilic film material to water.Hydrophilic film such as CA, PNA material is few to solute absorption, and molecular weight cut-off is less, but poor heat stability, physical strength, chemical proof, antibacterium erosional competency are not high usually; Hydrophobic film mechanical strength height such as PS, high temperature resistant, anti-solvent, anti-biological degradation, but because of containing a large amount of hydrophobicity genes or chain link in the molecular chain, and have a more static charge, thereby the permeable speed of film is low, and contamination resistance is lower, so the present invention selects hollow fiber ultrafiltration membrane.
In the ultra-filtration process if with the little ultra-filtration membrane of relative molecular weight that dams, interception capacity height, but cause yield on the low side, and,, cause content inclined to one side then by too much with the big ultra-filtration membrane of the relative molecular weight that dams; Therefore, select to dam the moderate ultra-filtration membrane of relative molecular weight, the content yield all reaches requirement, can play good separating effect.Ultra-filtration membrane is general, and to adopt the relative molecular weight that dams be 20000～80000 ultra-filtration membrane, and it is 40000 hollow fiber ultrafiltration membrane that the present invention adopts the relative molecular weight that dams, and carries out separating between Momordica-Glycosides and other component.
Working pressure in the ultra-filtration process, temperature, material flow and feed concentration etc. pollute influential to the film in the ultra-filtration process, and the most obvious with the influence of flow velocity.
Nanofiltration:
It is that 100～400 nanofiltration equipment or RO reverse osmosis equipment concentrate that the relative molecular weight that dams is adopted in nanofiltration, take all factors into consideration yield, purity and speed, preferably adopting the relative molecular weight that dams is 200 film, to reach the impurity of moisture and part ion or small-molecule substance, salt.
The parameter of whole technological process sees Table one:
The preferred parameter of whole technological process sees Table two:
The optimum parameter of whole technological process is seen three tables:
Membrane sepn extracts the gordian technique content of Momordica-Glycosides technology: with the Grosvenor Momordica fresh fruit is raw material, is extraction solvent with water, and integrated application membrane sepn micro-filtration, ultrafiltration, nanofiltration solve removal of impurities, separation, thickening problem in the Momordica-Glycosides extraction.
The micro-filtration of the integrated membrane sepn of the present invention, ultrafiltration, nanofiltration, with the fresh fruit is raw material, with water is extraction solvent, form advanced separation purifying technique flow process, the separation of finishing Momordica-Glycosides reaches and concentrates, simplified production technique, shortened the production cycle, owing under cryogenic condition, operate, thereby product color degree, solvability, clarity and taste are better, in addition, membrane separation technique is high-precision molecular screening, avoid the loss of activeconstituents, reduced energy consumption and cost, improved product yield and quality.
The present invention is according to the membrane sepn micro-filtration, ultrafiltration, the ultimate principle of nanofiltration, after Momordica-Glycosides structure and physico-chemical property carried out further investigation, the careful close application micro-filtration removal of impurities of having proved, ultra-filtration and separation, nanofiltration concentrates in the technical feasibility that Momordica-Glycosides extracts, reasonableness and science, through a large amount of tests repeatedly, having captured the film material selects and compliance test result, the discovery of processing parameter with technical barrier such as determine, operational path of the present invention and critical technical parameter are feasible, technique reproducible, good stability, show and pass through Application of membrane, product yield and production efficiency have been improved, the product purity height, cost is low, has reached good effect.The product of producing with the present invention is compared with the product of traditional method for extracting has following characteristics:
1. be raw material with the fresh fruit, effective constituent and pure taste are avoided baking and destroyed, and have improved product quality greatly, and be very crucial for the raising of product market competitiveness.And through the dry fruit raw material of overbaking, not only its functional component has certain loss, and its extract product lost the natural delicate fragrance local flavor of Grosvenor Momordica, and slightly burnt bitter taste.
2. the present invention is extraction solvent with water, than using organic solvent, more can guarantee to extract pure degree and original local flavor of product, has also improved processing safety, greatly reduces production cost simultaneously.
3. adopt the micro-filtration technology of membrane sepn, replaced traditional high speed centrifugation, sedimentation, filter and wait the clarification impurity removal process, can remove in the filtrate＞impurity of 0.1um, as: suspended solids, bacterium, colloid, solid protein, solved for a long time, in the traditional course of processing of Momordica-Glycosides, except that Momordica-Glycosides, remain in the extracting solution in a large amount of tannins, protein, starch, macromolecular substance and many particulates such as bacterium thermal source, the problem of submicron and floss, above-mentioned impurity is not effect not only, and have a strong impact on quality product, traditional high speed centrifugation, sedimentation, impurity-removing methods such as filtration are difficult to it is removed fully.Micro-filtration removal of impurities process plays good clarification, impurity elimination effect, has improved product purity and quality.
4. adopt the ultra-filtration technique of membrane sepn, replaced traditional macroporous adsorbent resin separation method.Ultrafiltration is the effective constituent sepn process, can isolate molecular weight ranges by hundreds of to millions of compounds, when having avoided environment is polluted with the soda acid wash-out, and whole ultra-filtration and separation technological process is carried out continuously, reduced operation, shortened the production cycle, avoided the influence of human factor quality product; The separation efficiency height helps scale operation; Sepn process and separating effect are easy to control, are beneficial to the stable prod yield; Do not consume organic solvent, reduce cost greatly, reduce environmental pollution, improved the quality of product.
5. adopt the nanofiltration of membrane sepn, replaced traditional steam jacket heating and concentrated mode.Nanofiltration is a concentration process, can molecular weight cut-off greater than the material of 150-200, inorganic salt and water then can pass through, and by nanofiltration with solvent and solute in the Grosvenor Momordica extracting solution separately, reach spissated purpose.Nanofiltration is relatively concentrating under the low temperature (40 ℃), owing to do not have phase transformation when concentrating, helps keeping the physiologically active and the physical and chemical stability of Momordica-Glycosides, and its content of effective is high by 10%～100% than traditional method, and need not heat dissipation.And traditional steam jacket heats spissated method, and higher because of the concentration process temperature, heated time is long, and loss of effective components is big, and product colour, mouthfeel change, and also will consume heat energy.
6. membrane technique separation efficiency height, equipment volume is little, and the membrane sepn processing power is easy to amplify, and easily is coupled with other abstraction processes, can directly insert existing technical process.
(4) embodiment: following is non-limiting examples of the present invention
1) pre-treatment: press the Grosvenor Momordica fresh fruit broken.
2) refluxing extraction: the processing parameter definite according to test, with raw material and deionized water by 1: 3 mixed extractor of packing into, be heated to the boiling back and kept temperature 2 hours, collect and extract feed liquid for the first time, extract the deionized water that adds 3 times of amounts more for the second time, ebuillition of heated insulation 2 hours is collected and is extracted feed liquid for the second time.Can be achieved as follows technical indicator in this stage:
| Yield (%) | Content (%) | Extraction yield (%) |
| ＞10.0 | ＞15.0 | ?＞90.0 |
3) concentrating under reduced pressure: extracting solution imported carry out concentrating under reduced pressure in the thickener, temperature is controlled at below 60 degrees centigrade, and vacuum degree control is more than 0.08.
The micro-filtration removal of impurities: in decompressed concentrate suction tubular type stainless steel microfiltration membrane equipment, pressure is 0.2Mpa in the operating process, collects the filtrate through microfiltration membrane.
4) ultra-filtration and separation: micro-filtration filtrate is imported in the hollow-fibre membrane ultrafiltration apparatus storage tank, and pressure is 1Mpa in the operating process, is 40000 ultra-filtration membrane by the relative molecular weight that dams, and collects the filtrate through ultra-filtration membrane.This stage is realized technical indicator:
| Yield (%) | Content (%) | Extraction yield (%) |
| ＞2.0 | ＞80.0 | ?＞90.0 |
5) nanofiltration concentrates: ultrafiltrate is imported in the container for storing liquid of nanofiltration equipment, regulate pressure to 3Mpa, when solution to be concentrated reaches 8 Baumes, collect concentrated solution.
6) spraying drying: nanofiltration concentrated solution spraying drying.
7) sterilising packaging: the dry powder after will sieving is put sterilising chamber's medium ultraviolet sterilising packaging.
Claims (9)
1, a kind of method of extracting Momordica-Glycosides from Grosvenor Momordica is characterized in that with the fresh Fructus Momordicae being raw material, is extraction solvent with water, and adopting micro-filtration, ultrafiltration, nanofiltration is main extraction process, and wherein microfiltration membrane adopts the millipore filtration in 0.05 μ m～0.3 μ m aperture; It is 20000～80000 ultra-filtration membrane that ultra-filtration membrane adopts the relative molecular weight that dams; It is that 100～400 nanofiltration membrane or RO reverse osmosis equipment concentrate that the relative molecular weight that dams is adopted in nanofiltration.
2, the method for from Grosvenor Momordica, extracting Momordica-Glycosides according to claim 1, it is characterized in that: described microfiltration membrane is the millipore filtration in 0.08 μ m～0.12 μ m aperture; Ultra-filtration membrane is 30000～50000 hollow fiber ultrafiltration membrane; Nanofiltration membrane is that the relative molecular weight that dams is 150～250 ceramic membrane.
3, the method for from Grosvenor Momordica, extracting Momordica-Glycosides according to claim 2, it is characterized in that: described microfiltration membrane is the stainless steel millipore filtration in 0.1 μ m aperture; Ultra-filtration membrane is 40000 hollow fiber ultrafiltration membrane; Nanofiltration membrane is that the relative molecular weight that dams is 100 ceramic membrane.
4, according to the described method of extracting Momordica-Glycosides from Grosvenor Momordica of claim 1～3, it is characterized in that: extraction time is 3～4 times, and the solvent consumption is 2～4 times, and temperature is 40～100 ℃.
5, the method for from Grosvenor Momordica, extracting Momordica-Glycosides according to claim 4, it is characterized in that: extraction time is 2 times, and the solvent consumption is 3 times, and temperature is 70～80 ℃.
6, the method for extracting Momordica-Glycosides from Grosvenor Momordica according to claim 4, it is characterized in that: extracting temperature is 80 ℃.
7, the method for from Grosvenor Momordica, extracting Momordica-Glycosides according to claim 4, it is characterized in that: temperature is 20～60 ℃ in the microfiltration process, and working pressure is 0.4～1.0Mpa, and the feed liquid flow velocity is 40～80 L/H/0.72M
2The temperature of ultra-filtration process is 20～60 ℃, and working pressure is 0.6～1.2Mpa, and the feed liquid flow velocity is 30～70 L/H/0.72M
2The temperature of nanofiltration process is 20～60 ℃, and working pressure is 0.6～1.2Mpa, and the feed liquid flow velocity is 30～70 L/H/0.72M
2
8, the method for from Grosvenor Momordica, extracting Momordica-Glycosides according to claim 7, it is characterized in that: the temperature of microfiltration process is 30～50 ℃, and working pressure is 0.8Mpa, and the feed liquid flow velocity is 50～70 L/H/0.72M
2The temperature of ultra-filtration process is 30～50 ℃, and working pressure is 1.0Mpa, and the feed liquid flow velocity is 40～60 L/H/0.72M
2The temperature of nanofiltration process is 30～50 ℃, and working pressure is 1.0Mpa, and the feed liquid flow velocity is 40～60 L/H/0.72 M
2
9, the method for from Grosvenor Momordica, extracting Momordica-Glycosides according to claim 8, it is characterized in that: the temperature of microfiltration process is 40 ℃, and working pressure is 0.8Mpa, and the feed liquid flow velocity is 60L/H/0.72M
2The temperature of ultra-filtration process is 30～50 ℃, and working pressure is 1.0Mpa, and the feed liquid flow velocity is 50 L/H/0.72M
2The temperature of nanofiltration process is 35 ℃, and working pressure is 1.0Mpa, and the feed liquid flow velocity is 50 L/H/0.72 M
2
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| CN100364460C (en) * | 2004-01-01 | 2008-01-30 | 刘清楚 | Method of normal temperature extracting fresh fruit effective extract and method of normal temperature preserving fresh fruit |
| CN101407535B (en) * | 2007-10-10 | 2011-05-25 | 桂林市振达生物科技有限责任公司 | Preparation of high-purity Momordica grosvenori mogroside V |
| CN101669622B (en) * | 2009-09-27 | 2012-02-22 | 何伟平 | Grosvenor momordica preparation, grosvenor momordica drink containing preparation and preparation method thereof |
| CN102084982B (en) * | 2009-12-02 | 2012-10-03 | 桂林莱茵生物科技股份有限公司 | Sweetening agent composition |
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