CN1683387A - Method for extracting momordica glycoside from momordica grosvenori - Google Patents
Method for extracting momordica glycoside from momordica grosvenori Download PDFInfo
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- CN1683387A CN1683387A CN 200510055229 CN200510055229A CN1683387A CN 1683387 A CN1683387 A CN 1683387A CN 200510055229 CN200510055229 CN 200510055229 CN 200510055229 A CN200510055229 A CN 200510055229A CN 1683387 A CN1683387 A CN 1683387A
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Abstract
The process of extracting momordica glycoside from momordica grosvenori includes the following steps: extracting momordica grosvenori material with water or low carbon alcohol as solvent and in a heating, ultrasonic or microwave process; concentration; and separation and purification with chromatographic column or membrane. The extract has momordica glycoside content of 40-80 wt% or momordica glycoside V content of 20-40 wt%. The present invention has high momordica glycoside content in the product, less loss of active component, simple production process and short production period.
Description
Technical field
The present invention relates to a kind of preparation method of Fructus Monordicae extract, specifically, relate to a kind of method of from Grosvenor Momordica, extracting Momordica-Glycosides.
Background technology
Grosvenor Momordica (Momordicae grosvenori swingle) is traditional health fruit, existing tricentennial dietotherapy history.Sweet, the slightly cool in nature of its flavor has the curative effect of removing heat from the lung to relieve cough, promotion functions of intestines and stomach, treats acute and chronic bronchitis, acute and chronic tonsillitis, acute gastritis, constipation etc.
The Grosvenor Momordica composition studies show that:
1, Grosvenor Momordica contains the strong sweet substance that 1% triterpene is glucoside S-5, its sugariness is equivalent to 300 times of sucrose, much sweeter than stevioside and Liquiritigenin, and there is not a bitter peculiar smell of stevioside, this strong sweet substance flavor is sweet and pure, free from extraneous odour, aftertaste sense are strong, thermally-stabilised good, and be stable in 100 ℃ of aqueous solution, 120 ℃ continuously heating still be not destroyed more than 12 hours.Belong to non-fermented material, be beneficial to processing and store.Japan bamboo professor Ben Changsong studies supposition, and this material has the effect of treatment cancer.
2, the Vitamin C content of Grosvenor Momordica is very abundant, it is 319-510mg that every according to surveying and determination 100g fresh Fructus Momordicae contains vitamins C, all exceed tens times to tens times than citrus, banana, Plantula Brassicae chinensis etc., more taller than the Kiwifruit (every 100g contains VITAMIN 100-420mg) that present domestic generally acknowledged vitamin contents is higher.
3, Grosvenor Momordica contains treatment coronary heart disease and prevention comparatively ideal oleic acid of arteriosclerosis and linolic acid composition.
4, Grosvenor Momordica contains 17 seed amino acids.Contain 16 kinds of inorganic microelements such as selenium again.Modern medicine proof selenium coronary heart disease is controlled, anti-ageing, anticancer aspect is all effective in cure.
Prove as Japanese scholar bamboo professor Ben Changsong research and Chinese pharmacy: the main effective constituent of Grosvenor Momordica is Momordica-Glycosides, and it is the strong sweet substance of triterpene system.Momordica-Glycosides is to be extracted by natural arhat fresh fruit, is the elite of Grosvenor Momordica, has good health-care effect, to promote stomach function and clearing and antitussive, quench the thirst reduce phlegm, the clearing heat and moistening lung effect is more remarkable.Compare with artificial synthesis edulcorant and other sweeting agent, the most outstanding advantage of Momordica-Glycosides is an edible safety, sugariness height (pure product sugariness is 300 times of sucrose) is best sweeting agent of patients such as obesity, hypertension, diabetes, heart trouble and best healthcare products.Soluble in water and the spirituous solution of this product, Heat stability is good, stable in 100 ℃ of aqueous solution, under 120 ℃ of high temperature, still be not destroyed for a long time, and belong to non-fermented material, be beneficial to food storage and processing.Can be widely used in industry such as medicine, food, daily use chemicals, beverage, health care for the aged product.
Now, extract Momordica-Glycosides from Grosvenor Momordica, the method for use generally is exactly to use flooding, and concentrate drying moisture promptly gets Momordica-Glycosides then.As the patent No. is the extracting method that the Chinese patent of ZL 87101850 discloses a kind of mangosteen sweetener.It grinds, pulls an oar with mangosteen fruit, and warm water 50-60 ℃ extraction is filtered.Separate by DA-201 acrylic type sorbent material, 50% (V/V) dissolve with ethanol, through the decolouring of D-211 acrylic type negative resin, desalination, decon, distillation method reclaims ethanol, and through the vacuum pump concentrating under reduced pressure, lyophilize obtains Momordica-Glycosides.Its complex process, and the active constituent content in the Momordica-Glycosides is not high.Its processing method is anxious to be waited to improve.
Summary of the invention
The technical issues that need to address of the present invention just are to overcome the existing defective of extracting the Momordica-Glycosides method from Grosvenor Momordica, a kind of method of extracting Momordica-Glycosides from Grosvenor Momordica is provided, active constituent content height by this method products obtained therefrom, by ultraviolet--the Momordica-Glycosides weight content is 40～80% in visible spectrophotometric UV (ultraviolet-visible spectrophotometry) the method mensuration Fructus Monordicae extract, perhaps press high-efficient liquid phase chromatogram HPLC (HighPerformance Liquid Chromatography) method and measure, the Momordica grosvenori mogroside V weight content is 20～40% in the Fructus Monordicae extract.The Momordica-Glycosides content height that the inventive method is produced, avoided activeconstituents loss, simplified production technique, shortened the production cycle.
For addressing the above problem, the present invention adopts following technical scheme:
A kind of method of from Grosvenor Momordica, extracting Momordica-Glycosides of the present invention, it be a kind of be raw material with the Grosvenor Momordica, through the method that extraction solvent extracts, concentrates, Momordica-Glycosides is extracted in separation and purification, by ultraviolet--visible spectrophotometric UV method is measured, the Momordica-Glycosides weight content is 40～80% or measures by the high-efficient liquid phase chromatogram HPLC method in the Fructus Monordicae extract, and the Momordica grosvenori mogroside V weight content is 20～40% in the Fructus Monordicae extract.
Grosvenor Momordica described in the inventive method can be fresh Fructus Momordicae or dried fructus momordicae.
Extraction solvent described in the inventive method is water or low-carbon alcohol.Described low-carbon alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols or amylalcohol, and the weight concentration of described low-carbon alcohol is 1%～95%.
The described extracting method of the inventive method is heating extraction or ultrasonic extraction or microwave extraction, and the ultrasonic extraction condition is operating frequency 15～60kHz, time 5～30min; The microwave extraction condition is operating frequency 900～2500MHz, time 5～30min.
Processing needs to decolour after dried fructus momordicae of the present invention extracts.Decoloring method is for passing through decolorizing resin or zwitterion post or Al
2O
3The post decolouring is handled.
The described simmer down to vacuum concentration of the inventive method, temperature is below 60 ℃, is concentrated into the 1/4-1/2 of original extracting liquid volume.
Separation and purification of the present invention can be column chromatographic isolation and purification or membrane separation purification.
Column chromatographic isolation and purification of the present invention is:
1) extracting solution is through concentrating (vacuum concentration, temperature are controlled at below 60 degrees centigrade, more than the vacuum tightness 0.08MPa, are concentrated into the 1/4-1/2 of original extracting liquid volume), centrifugal (horizontal centrifuge: 4800r/min), directly enter macroporous resin column;
2) it is limpid to effluent liquid to wash post with deionized water;
3) wash post to effluent liquid with low-carbon alcohol and do not have sweet taste;
4) collect the effluent liquid and the elutriant of concentration alcohol solution wash-out from low to high from macroporous resin column respectively;
5) pure water elution liquid is through vacuum concentration, and vacuum tightness 0.06-0.1MPa is concentrated into about 8 mother-in-law U.S. degree spraying drying: 190 ℃ of intake air temperatures, 80 ℃ of air outlet temperature get Momordica-Glycosides.
Wherein said low-carbon alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols or amylalcohol, the concentration of lower concentration alcohol solution is minimum to be volumetric concentration 30%, the concentration of high density alcohol solution is up to volumetric concentration 95%, and being adjusted to alcohol total content therein with the pure mixed solution that will collect liquid from macroporous resin is volume content 70%～90%; Wherein said macroporous resin is for being the material of skeleton with the polystyrene, and as the DIAION brand, model is: D101, D130, AB-8 or HP-20.
Membrane separation purification of the present invention comprises:
1) micro-filtration removal of impurities: carry out micro-filtration after extracting solution concentrated, microfiltration membrane is the millipore filtration in 0.05 μ m～0.3 μ m aperture, removes impurity such as water soluble protein, pectin and suspended substance most in the solution;
2) ultra-filtration and separation: adopting the relative molecular weight that dams is 40000 hollow fiber ultrafiltration membrane, carries out separating between Momordica-Glycosides and other component;
3) nanofiltration concentrates: adopting the relative molecular weight that dams is that 100～400 nanofiltration membrane or RO reverse osmosis equipment concentrate.
Preferably, described microfiltration membrane is the millipore filtration in 0.08 μ m～0.12 μ m aperture; Described nanofiltration is 150～250 ceramic membrane for adopting the relative molecular weight that dams,
Further preferably, the described microfiltration membrane stainless steel millipore filtration that is 0.1 μ m aperture; Described nanofiltration is 200 nanofiltration membrane for adopting the relative molecular weight that dams.
The inventive method can be carried out fragmentation with Grosvenor Momordica earlier before extraction, Grosvenor Momordica helps the abundant stripping of various compositions after fragmentation.Fresh fruit presses broken getting final product with it.
The present invention also provides a kind of Fructus Monordicae extract by method for preparing, by ultraviolet--visible spectrophotometric UV method is measured, the Momordica-Glycosides weight content is 40～80% or measures by the high-efficient liquid phase chromatogram HPLC method in the Fructus Monordicae extract, and the Momordica grosvenori mogroside V weight content is 20～40% in the Fructus Monordicae extract.
The inventive method is a raw material with the Grosvenor Momordica, 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.By ultraviolet--visible spectrophotometric UV method is measured, and the Momordica-Glycosides weight content is 40～80% or measures by the high-efficient liquid phase chromatogram HPLC method in the Fructus Monordicae extract, and the Momordica grosvenori mogroside V weight content is 20～40% in the Fructus Monordicae extract.The Momordica-Glycosides content height that the inventive method is produced, avoided activeconstituents loss, simplified production technique, shortened the production cycle.
Embodiment
Embodiment 1
1) pre-treatment: press the Grosvenor Momordica fresh fruit broken.
2) refluxing extraction: 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.
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.
4) centrifugal: the extracting solution after will concentrating is centrifugal by whizzer.
5) concentrate, the extracting solution after centrifugal directly advances macroporous resin column;
6) it is limpid to effluent liquid to wash post with water;
7) wash post to effluent liquid with ethanol and do not have sweet taste;
8) collect the effluent liquid and the elutriant of concentration alcohol solution wash-out from low to high from macroporous resin column;
9) elutriant carries out concentrating under reduced pressure, is concentrated into 8 mother-in-law U.S. degree;
10) spraying drying, sterilising packaging
Embodiment 2
1) pre-treatment: with the fragmentation of Grosvenor Momordica dry fruit.
2) refluxing extraction: with raw material and weight concentration be 1% ethanol by 1: 12 mixed, carry out ultrasonic extraction, extraction conditions is operating frequency 15～60kHz, time 5～30min extracts 3 times; Extract the back by the decolorizing resin processing of decolouring.
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 contracts to the 1/4-1/2 of original extracting liquid volume more than 0.08.
4) micro-filtration removal of impurities: in decompressed concentrate suction tubular type stainless steel microfiltration membrane equipment, microfiltration membrane is the millipore filtration in 0.05 μ m～0.3 μ m aperture, remove impurity such as water soluble protein, pectin and suspended substance most in the solution, pressure is 0.2Mpa in the operating process, collects the filtrate through microfiltration membrane.
5) ultra-filtration and separation: micro-filtration filtrate is imported in the hollow-fibre membrane ultrafiltration apparatus storage tank, pressure is 1Mpa in the operating process, by the relative molecular weight that dams is 40000 ultra-filtration membrane, carries out separating between Momordica-Glycosides and other component, collects the filtrate through ultra-filtration membrane.
6) nanofiltration concentrates: ultrafiltrate is imported in the container for storing liquid of nanofiltration equipment, regulate pressure to 3Mpa, adopting the relative molecular weight that dams is that 100～400 nanofiltration membrane concentrates.Solution to be concentrated reaches 8 mother-in-law U.S.As when spending, and collects concentrated solution.
7) spraying drying, sterilising packaging.
Embodiment 3
1) pre-treatment: with the fragmentation of Grosvenor Momordica dry fruit.
2) refluxing extraction: with raw material and weight concentration be 95% propyl alcohol by 1: 2 mixed, carry out microwave extraction, extraction conditions is operating frequency 900～2500MHz, time 5～30min.Extract, extract 2 times; Extract the back by the processing of decolouring of zwitterion post.
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 contracts to the 1/4-1/2 of original extracting liquid volume more than 0.08.
4) micro-filtration removal of impurities: in decompressed concentrate suction tubular type stainless steel microfiltration membrane equipment, microfiltration membrane is the millipore filtration in 0.08 μ m～0.12 μ m aperture, remove impurity such as water soluble protein, pectin and suspended substance most in the solution, pressure is 0.2Mpa in the operating process, collects the filtrate through microfiltration membrane.
5) ultra-filtration and separation: micro-filtration filtrate is imported in the hollow-fibre membrane ultrafiltration apparatus storage tank, pressure is 1Mpa in the operating process, by the relative molecular weight that dams is 40000 ultra-filtration membrane, carries out separating between Momordica-Glycosides and other component, collects the filtrate through ultra-filtration membrane.
6) nanofiltration concentrates: ultrafiltrate is imported in the container for storing liquid of nanofiltration equipment, regulate pressure to 3Mpa, adopting the relative molecular weight that dams is that 150～250 ceramic membrane concentrates.Solution to be concentrated reaches 8 mother-in-law U.S.As when spending, and collects concentrated solution.
7) spraying drying, sterilising packaging
Embodiment 4
1) pre-treatment: with the fragmentation of Grosvenor Momordica dry fruit.
2) refluxing extraction: with raw material and weight concentration be 50% Virahol by 1: 5 mixed, carry out microwave extraction, extraction conditions is operating frequency 900～2500MHz, time 5～30min.Extract 2 times; Pass through Al after the extraction
2O
3The post processing of decolouring.
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 contracts to the 1/4-1/2 of original extracting liquid volume more than 0.08.
4) micro-filtration removal of impurities: in decompressed concentrate suction tubular type stainless steel microfiltration membrane equipment, microfiltration membrane is the millipore filtration in 0.08 μ m～0.12 μ m aperture, remove impurity such as water soluble protein, pectin and suspended substance most in the solution, pressure is 0.2Mpa in the operating process, collects the filtrate through microfiltration membrane.
5) ultra-filtration and separation: micro-filtration filtrate is imported in the hollow-fibre membrane ultrafiltration apparatus storage tank, pressure is 1Mpa in the operating process, by the relative molecular weight that dams is 40000 ultra-filtration membrane, carries out separating between Momordica-Glycosides and other component, collects the filtrate through ultra-filtration membrane.
6) nanofiltration concentrates: ultrafiltrate is imported in the container for storing liquid of nanofiltration equipment, regulate pressure to 3Mpa, adopting the relative molecular weight that dams is that 150～250 ceramic membrane concentrates.Solution to be concentrated reaches 8 mother-in-law U.S.As when spending, and collects concentrated solution.
7) spraying drying, sterilising packaging.
Claims (19)
1, a kind of method of from Grosvenor Momordica, extracting Momordica-Glycosides, it is characterized in that it be a kind of be raw material with the Grosvenor Momordica, through the method that extraction solvent extracts, concentrates, Momordica-Glycosides is extracted in separation and purification, by ultraviolet--visible spectrophotometric UV method is measured, the Momordica-Glycosides weight content is 40～80% or measures by the high-efficient liquid phase chromatogram HPLC method in the extract, and the Momordica grosvenori mogroside V weight content is 20～40% in the extract.
2, extract the method for Momordica-Glycosides according to claim 1 from Grosvenor Momordica, it is characterized in that: described Grosvenor Momordica is fresh Fructus Momordicae or dried fructus momordicae.
3, extract the method for Momordica-Glycosides according to claim 1 from Grosvenor Momordica, it is characterized in that: described extraction solvent is water or low-carbon alcohol, and extraction time is 3～4 times, and the solvent consumption is 2～12 times; Temperature is 40～100 ℃.
4, as extract the method for Momordica-Glycosides as described in the claim 3 from Grosvenor Momordica, it is characterized in that: described low-carbon alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols or amylalcohol, and the weight concentration of described low-carbon alcohol is 1%～95%.
5, extract the method for Momordica-Glycosides according to claim 1 from Grosvenor Momordica, it is characterized in that: described extracting method is heating extraction or ultrasonic extraction or microwave extraction.
6, method as claimed in claim 5 is characterized in that: the ultrasonic extraction condition is operating frequency 15～60kHz, time 5～30min; The microwave extraction condition is operating frequency 900～2500MHz, time 5～30min.
7, as from Grosvenor Momordica, extracting the method for Momordica-Glycosides as described in the claim 2, it is characterized in that: the processing of decolouring after dried fructus momordicae extracts.
8, as extract the method for Momordica-Glycosides as described in the claim 7 from Grosvenor Momordica, it is characterized in that: described decoloring method is for by decolorizing resin or zwitterion post or Al
2O
3The post decolouring is handled.
9, extract the method for Momordica-Glycosides according to claim 1 from Grosvenor Momordica, it is characterized in that: described simmer down to vacuum concentration, temperature are below 60 ℃, are concentrated into the 1/4-1/2 of original extracting liquid volume.
10, extract the method for Momordica-Glycosides according to claim 1 from Grosvenor Momordica, it is characterized in that: described separation and purification is column chromatographic isolation and purification or membrane separation purification.
11, as from Grosvenor Momordica, extracting the method for Momordica-Glycosides as described in the claim 10, it is characterized in that column chromatographic isolation and purification comprises:
1) extracting solution through concentrate, centrifugal after, directly enter macroporous resin column;
2) it is limpid to effluent liquid to wash post with deionized water;
3) wash post to effluent liquid with low-carbon alcohol and do not have sweet taste;
4) collect the effluent liquid and the elutriant of concentration alcohol solution wash-out from low to high from macroporous resin column respectively;
5) vacuum concentration, spraying drying: vacuum tightness 0.06-0.1MPa is concentrated into 8 mother-in-law U.S. degree and carries out spraying drying: 190 ℃ of intake air temperatures, 90 ℃ of air outlet temperature.
12, the method for from Grosvenor Momordica, extracting Momordica-Glycosides as claimed in claim 11, it is characterized in that: described low-carbon alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, butanols or amylalcohol, the concentration of lower concentration alcohol solution is minimum to be volumetric concentration 30%, the concentration of high density alcohol solution is up to volumetric concentration 95%, and being adjusted to alcohol total content therein with the pure mixed solution that will collect liquid from macroporous resin is volume content 70%～90%.
13, as extract the method for Momordica-Glycosides as described in claim 11 or 12 from Grosvenor Momordica, it is characterized in that: described macroporous resin is for being the material of skeleton with the polystyrene.
14, the method for extracting Momordica-Glycosides from Grosvenor Momordica as claimed in claim 13, it is characterized in that: described polystyrene model is: D101, D130, AB-8 or HP-20.
15, as from Grosvenor Momordica, extracting the method for Momordica-Glycosides as described in the claim 10, it is characterized in that described membrane separation purification is:
1) micro-filtration removal of impurities: carry out micro-filtration after extracting solution concentrated, microfiltration membrane is the millipore filtration in 0.05 μ m～0.3 μ m aperture, removes impurity such as water soluble protein, pectin and suspended substance most in the solution;
2) ultra-filtration and separation: adopting the relative molecular weight that dams is 40000 hollow fiber ultrafiltration membrane, carries out separating between Momordica-Glycosides and other component;
3) nanofiltration concentrates: adopting the relative molecular weight that dams is that 100～400 nanofiltration membrane or RO reverse osmosis equipment concentrate.
16, as from Grosvenor Momordica, extracting the method for Momordica-Glycosides as described in the claim 15, it is characterized in that described microfiltration membrane is the millipore filtration in 0.08 μ m～0.12 μ m aperture; Described nanofiltration is 150～250 ceramic membrane for adopting the relative molecular weight that dams.
17, as from Grosvenor Momordica, extracting the method for Momordica-Glycosides as described in the claim 15, it is characterized in that described microfiltration membrane is the stainless steel millipore filtration in 0.1 μ m aperture; Described nanofiltration is 200 nanofiltration membrane for adopting the relative molecular weight that dams.
18, as from Grosvenor Momordica, extracting the method for Momordica-Glycosides as described in claim 1-17 arbitrary, it is characterized in that before extraction, earlier Grosvenor Momordica being carried out fragmentation.
19, a kind of Fructus Monordicae extract as method preparation as described in claim 1-18 arbitrary, it is characterized in that: by ultraviolet--visible spectrophotometric UV method is measured, the Momordica-Glycosides weight content is 40～80% or measures by the high-efficient liquid phase chromatogram HPLC method in the Fructus Monordicae extract, and the Momordica grosvenori mogroside V weight content is 20～40% in the Fructus Monordicae extract.
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