CN108864238A - The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii - Google Patents
The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii Download PDFInfo
- Publication number
- CN108864238A CN108864238A CN201810747506.7A CN201810747506A CN108864238A CN 108864238 A CN108864238 A CN 108864238A CN 201810747506 A CN201810747506 A CN 201810747506A CN 108864238 A CN108864238 A CN 108864238A
- Authority
- CN
- China
- Prior art keywords
- fruit seed
- slag
- extracting
- siraitia grosvenorii
- arhat fruit
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J9/00—Normal steroids containing carbon, hydrogen, halogen or oxygen substituted in position 17 beta by a chain of more than two carbon atoms, e.g. cholane, cholestane, coprostane
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/008—Refining fats or fatty oils by filtration, e.g. including ultra filtration, dialysis
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Microbiology (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
- Cosmetics (AREA)
Abstract
The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii, the method for extracting arhat fruit seed oil includes the following steps：（1）Refluxing extraction：It is extracted to Siraitia grosvenorii and water and fat-soluble organic solvent is added in slag, be stirred at reflux extraction, stratification obtains organic extract；（2）Packed column absorption：Upper packed column absorption, collects efflux, obtains arhat fruit seed crude oil solution；（3）Purification：Decolorising agent is added, heating stirring is cooling, then uses ultrafiltration membrance filter, is concentrated, obtains arhat fruit seed olein product.The invention also discloses the methods for extracting cupreol simultaneously.In arhat fruit seed oil obtained by the method for the present invention, the content of oleic acid, linoleic acid and palmitinic acid is high, and arhat fruit seed oil yield is up to 97.3%；The content of gained cupreol is up to 99.9%, and yield is up to 94.1%；The method of the present invention technical process strong operability, at low cost, the comprehensive utilization of Siraitia grosvenorii resource high-efficiency is suitable for industrialized production.
Description
Technical field
The present invention relates to the methods for extracting arhat fruit seed oil and cupreol, and in particular to a kind of to extract in slag from Siraitia grosvenorii
The method for extracting arhat fruit seed oil and cupreol.
Background technique
Siraitia grosvenorii（Siraitia grosvenorii (Swingle) C. Jeffrey）It is Dicotyledoneae
（Dicotyledoneae）Curcurbitaceae（Cucurbitaceac）The fruit of Genus Siraitia Merr, vegetable formal name " Semen Momordicae ",
Alias draws river fruit, balloonvine heartseed herb, is the distinctive economy in China, medicinal plant, main product is in the warm of the provinces such as Guangxi, Guangdong, Hunan, Jiangxi
Band, Subtropical mountains have more than 200 years cultivation histories.Siraitia grosvenorii is sweet in flavor cool in nature, and return lung, large intestine channel have moistening lung to arrest cough, raw
The effect of saliva quenches the thirst it is suitable for lung heat or xeropulmonary cough, pertussis and hot summer weather fluid deficiency and thirst etc., in addition, there are also relax bowel and defecation
Effect.Modern medical studies have confirmed that Siraitia grosvenorii contains a kind of natural sweetener --- sweet Momordica grosvenori of about 400 times than sucrose sweet tea
Glycosides, but it does not generate heat, therefore, it is the ideal replacement beverage of the unsuitable sugar eater such as diabetes, obesity.Except mogroside with
Outside, there are also a large amount of oligofructose, pectin, cellulose, more than ten kinds of essential amino acids, fat for the nutritional ingredient in Siraitia grosvenorii
Acid, cupreol, flavone compound, vitamin C, microelement etc..
It is reported that the content of fatty acid is up to 40% in the arhat fruit seed of drying, main component therein is oleic acid, sub- oil
Acid and palmitinic acid, these types of fatty acid have treatment coronary heart disease and prevent the physiological activity of vascular sclerosis, are rouge needed by human
Fat acid, Development volue with higher.
Cupreol belongs to three note class compound of Fourth Ring, each vegetable oil, the nut etc. being widely present in nature
In vegetable seeds, exist in certain plants medicine.Cupreol has effects that be substantially reduced serum cholesterol, can replace
Cholesterol is as liposome membrane material.Cupreol is a kind of medical material and intermediate with preciousness value, has drop gallbladder solid
Alcohol, prevention cardiovascular disease, improves hypertrophy of the prostate, prevention prostate cancer, prevents to draw because cholesterol is excessively high in diet reducing blood lipid
The cholecystolithiasis and other effects risen.
Currently, the main method for extracting arhat fruit seed oil from arhat fruit seed has alcohol extracting, squeezing etc..
Model cloud field etc. discloses a kind of process optimization of arhat fruit seed oil extract, by arhat fruit seed through drying, crushing, ethyl alcohol
Extraction, centrifuge separation, concentration, drying and other steps obtain arhat fruit seed oil.But this method needs to dry arhat fruit seed, at
This is high, is not suitable for industrialized production.
CN107057829A discloses a kind of technique that separating-purifying arhat fruit seed oil in slag is extracted from Siraitia grosvenorii, is with sieve
It is raw material that Chinese fruit, which extracts slag, passes through the separation of seed shell liquid, low temperature drying, crushing, wet process extruding, cold press, centrifugal filtration, counter-current extraction
Degumming deacidification, vacuum dehydration, composite decoloration, plate-frame filtering, ceramic membrane clarification, obtain arhat fruit seed oil.But the party
Method is also needed the drying of arhat fruit seed, and the tedious complexity of step, and equipment investment is big, and yield is relatively low, is not suitable for industrialized production.
Currently, there is no the report for extracting cupreol from Siraitia grosvenorii.
Summary of the invention
The technical problem to be solved by the present invention is to overcome drawbacks described above of the existing technology, provide a kind of gained sieve
Chinese fruit seed oil, cupreol content and high income, technical process strong operability is at low cost, the comprehensive benefit of Siraitia grosvenorii resource high-efficiency
With the slave Siraitia grosvenorii for being suitable for industrialized production extracts the method for extracting arhat fruit seed oil and cupreol in slag.
The technical solution adopted by the present invention to solve the technical problems is as follows：One kind is extracted in slag from Siraitia grosvenorii and extracts arhat
The method of fruit seed oil, includes the following steps：
（1）Refluxing extraction：It is extracted to Siraitia grosvenorii and water and fat-soluble organic solvent is added in slag, extraction is stirred at reflux, by extracting solution
Stratification obtains organic extract except the water layer of sub-cloud；
（2）Packed column absorption：By step（1）Packed column adsorbs on gained organic extract, collects efflux, it is thick to obtain arhat fruit seed
Oil solution；
（3）Purification：To step（2）It is added decolorising agent in gained arhat fruit seed crude oil solution, heating stirring, after being cooled to room temperature,
Ultrafiltration membrance filter is used again, and ultrafiltrate is concentrated into solvent-free, obtains arhat fruit seed olein product.
Preferably, step（1）In, the water content that the Siraitia grosvenorii extracts slag is 50~60%.
Preferably, step（1）In, it is that the waste residue after sweet tea glycosides is extracted with water in Siraitia grosvenorii fresh fruit that the Siraitia grosvenorii, which extracts slag,
It mainly include arhat fruit seed slag and Siraitia grosvenorii shell slag, wherein mass content of the contained arhat fruit seed oil in wet basis is 5
~8%, mass content of the cupreol in wet basis is 1~4%.
Preferably, step（1）In, the volume and Siraitia grosvenorii of water and fat-soluble organic solvent extract the body of slag wet basis quality
Product mass ratio（L/L/kg）It is 0.5~1.0:15~20:1.The purpose for adding water is the Huang for dissolving and separating in Siraitia grosvenorii extraction slag
The water-soluble impurity such as ketone, protein, polysaccharide.If the dosage of water is excessive, the leaching of arhat fruit seed oil and cupreol will affect
Out, and the discharge amount of waste water will be increased；If the dosage of water is very few, water-solubility impurity leaching is not thorough, and will reduce arhat fruit seed
The appearance color and content of oil and cupreol.If fat-soluble consumption of organic solvent is excessive, the processing of subsequent step will increase
The consumption of amount and solvent, causes to waste；If fat-soluble consumption of organic solvent is very few, arhat fruit seed oil and cupreol will be difficult
Sufficiently to leach.
Preferably, step（1）In, the fat-soluble organic solvent is petroleum ether, 6# solvent for extraction, 120# extraction solvent
One or more of oil or ethyl acetate etc..
Preferably, step（1）In, the revolving speed for being stirred at reflux extraction is 20~60 r/min, and temperature is 75~85 DEG C,
Time is 2~4h.The purpose of stirring is to come into full contact with organic solvent, water and extraction slag, improves the efficiency of extraction.If stirring
Revolving speed is too fast, then easily leads to organic solvent and water emulsification, so that subsequent step is difficult to be layered；If the revolving speed of stirring is excessively slow, have
Solvent, water and extraction slag are difficult to come into full contact with, and cause to extract incomplete.
Preferably, step（1）In, the time of the stratification is 1~2h.Stratification is the difference using density,
Fat-soluble organic solvent layer containing arhat fruit seed oil and cupreol and the water layer containing water-solubility impurity are layered, by water layer
After discharge, water-solubility impurity is removed then.
Preferably, step（2）In, the flow velocity of upper prop is 0.1~1.0BV/h.
Preferably, step（2）In, the ratio of height to diameter of the packed column is 2~10:1（More preferable 4~8:1）.
Preferably, step（2）In, filler and Siraitia grosvenorii in the packed column extract the volume mass ratio of slag wet basis
（L/kg）It is 0.1~0.5:1.
The purpose of upper prop absorption：First is that cupreol is adsorbed on filler, make its in organic solvent extracting solution
The separation of arhat fruit seed oil；Second is that removing the fat-soluble pigment in organic solvent extracting solution；Third is that removing organic solvent extracting solution
In a small amount of water.If upper column flow rate is too fast, the ratio of height to diameter of packed column is too small or the dosage of filler is very few, will all be difficult to sufficiently
Reach above-mentioned purpose；If upper column flow rate is excessively slow, the ratio of height to diameter of packed column is excessive or the dosage of filler is excessive, will all cause
The waste of the energy and material.
Preferably, step（2）In, the filler in the packed column is one in silica gel, reverse phase silica gel or aluminium oxide etc.
Kind is several." silica gel " in the filler is different from " purification on normal-phase silica gel " of " reverse phase silica gel ", and " silica gel " is this field pair
" silica gel " and " reverse phase silica gel " and hyponymy is not present in the usual address of " purification on normal-phase silica gel ".
Preferably, step（3）In, the dosage of the decolorising agent is equivalent to 1~5% that Siraitia grosvenorii extracts slag wet basis quality（More
It is preferred that 2~4%）.If the dosage of decolorising agent is excessive, the waste of material will be caused, and increases the burden of ultrafiltration membrance filter；If de-
The dosage of toner is very few, then the effect decolourized is not thorough, and directly affects the appearance of arhat fruit seed oil.
Preferably, step（3）In, the decolorising agent is diatomite, active carbon, bentonite, activated alumina or concave convex rod
One or more of Deng.
Preferably, step（3）In, the temperature of the heating stirring is 40~60 DEG C, and the time is 1~2h.Heating, stirring
Purpose is to come into full contact with decolorising agent with arhat fruit seed crude oil solution, plays decolorising agent to the adsorption effect of pigment.If heating
Temperature it is excessively high or stirring overlong time, then will cause the loss of solvent and the energy；If heating temperature it is too low or stirring when
Between it is too short, then decolorising agent will be not thorough the absorption of pigment.
Preferably, step（3）In, the molecular cut off of the ultrafiltration membrane is 500~3000Da（More preferable 800~
2000Da）.
Preferably, step（3）In, the pressure of the filtering is 0.5~2.0MPa.
The purpose of ultrafiltration is to remove protein micro in decolorising agent, suspended matter and arhat fruit seed crude oil solution, carbohydrate
Etc. big molecular impurities, and reduce the turbidity of arhat fruit seed crude oil solution.If ultrafiltration retaining molecular weight is excessive or filter pressure mistake
Greatly, then big molecular impurity is possible to enter permeate through ultrafiltration membrane, causes the turbidity of arhat fruit seed crude oil solution higher；If super
Membrane retention molecular weight is too small or filter pressure is too small, then will cause the loss of arhat fruit seed oil, and the speed that will slow down filtering.
It is as follows that the present invention further solves technical solution used by its technical problem：It is extracted in slag described from Siraitia grosvenorii
The method for extracting cupreol while extracting arhat fruit seed oil, by step（2）Packed column after middle upper prop absorption is washed with lye
De-, eluent is extracted with fat-soluble organic solvent, stratification, and except the water layer of sub-cloud, organic layer is washed with water to neutrality, dense
Contracting, it is dry, obtain cupreol crude product；Cupreol crude product is dissolved by heating with low-carbon alcohols again, water is added, is cooled down, stirring and crystallizing,
Crystal is washed in filtering, dry, obtains cupreol fine work.
Preferably, the dosage of the lye is 2~5BV.
Preferably, the lye is the aqueous solution of sodium hydroxide and/or potassium hydroxide, and mass concentration is 1~5%.
Preferably, the flow velocity of the elution is 0.1~1.0BV/h.
With the purpose of eluted through lye：First is that the cupreol being adsorbed on resin column is desorbed；Second is that will desorb simultaneously
Ester impurities out are saponified into salt, make it dissolve in lye, and can not be extracted by organic solvent, to improve β-in extract liquor
The purity of sitosterol.If the dosage of lye is very few, concentration is too low or elution flow rate is too fast, will all be difficult to sufficiently achieve above-mentioned mesh
's；If the dosage of lye is excessive, excessive concentration or elution flow rate are excessively slow, the waste of the energy and material will be all caused.
Preferably, the fat-soluble organic solvent and Siraitia grosvenorii extract the volume mass ratio of slag wet basis（L/kg）For 0.5~
1.0:1.It is to extract the cupreol in eluted through lye liquid with the purpose that fat-soluble organic solvent extracts.If fat-soluble have
The dosage of solvent is very few, then cupreol will be difficult to sufficiently extract, and yield will reduce；If the dosage mistake of fat-soluble organic solvent
It is more, then it will cause the waste of the energy and material.
Preferably, the fat-soluble organic solvent is petroleum ether, 6# solvent for extraction, 120# solvent for extraction or acetic acid second
One or more of ester etc..
Preferably, the time of the stratification is 1~3h.Stratification is the difference using density, will contain β-paddy
The fat-soluble organic solvent layer of sterol is layered with the water layer containing water-solubility impurity, and after water layer is discharged, water-solubility impurity obtains then
With removal.
Preferably, the volume mass ratio of the low-carbon alcohols and cupreol crude product（L/kg）It is 2~5:1.If low-carbon alcohols
Dosage is very few, then cupreol crude product will be difficult to be completely dissolved；If the dosage of low-carbon alcohols is excessive, the concentration of solution is too low, will
Cause the yield of crystallization relatively low.
Preferably, the temperature of the heating is 40~70 DEG C.
Preferably, the volume ratio of the water and low-carbon alcohols is 0.5~3.0:1.The purpose for adding water is to increase low-carbon alcohol solution
Polarity, make cupreol solubility reduce and be precipitated.If the additional amount of water is excessive, the polarity of low-carbon alcohol solution is excessive,
Other impurity will also be precipitated, to influence the purity of cupreol crystallization；If the additional amount of water is very few, the analysis of cupreol
It will be not thorough out, to influence the yield of cupreol crystallization.
Preferably, the temperature of the stirring and crystallizing is 5~10 DEG C, and the speed of stirring is 20~60 r/min, stirring and crystallizing
Time be 12~24 h.
Preferably, the low-carbon alcohols are one or more of methanol, ethyl alcohol, isopropanol or n-butanol etc..
Preferably, described to be filtered into centrifugal filtration.
Preferably, crystal is washed with the low-carbon alcohols of freezing.It is with the purpose that the low-carbon alcohols of freezing wash crystal：Remove crystal
Surface can not thoroughly filter clean crystalline mother solution, to improve the purity and content of crystal.
Preferably, the volume mass ratio of the low-carbon alcohols of the freezing and cupreol crude product（L/kg）It is 0.5~1.0:1.
Preferably, the temperature of the low-carbon alcohols of the freezing is -5~5 DEG C.
If the dosage for freezing low-carbon alcohols is very few or temperature is too low, will all be difficult to thoroughly wash away the remaining crystallization mother of plane of crystal
Liquid；If the dosage for freezing low-carbon alcohols is excessive or temperature is excessively high, the loss of cupreol all will lead to.
Preferably, the low-carbon alcohols are one or more of methanol, ethyl alcohol, isopropanol or n-butanol etc..
In the method for the present invention, 1 BV=1 column volume.
The principle of the method for the present invention is：Siraitia grosvenorii extraction slag is stirred at reflux extraction, sieve with water and fat-soluble organic solvent
Chinese fruit seed oil and cupreol are easy to be extracted by fat-soluble organic solvent, and a large amount of water-solubility impurity is then dissolved in the water,
Water and dissolution water-solubility impurity therein can be removed by stratification；Filler is recycled only to adsorb cupreol without inhaling
The characteristic of attached arhat fruit seed oil, can separate the two.
The method of the present invention has the beneficial effect that：
（1）Arhat fruit seed olein product obtained by the method for the present invention be it is faint yellow, organoleptic requirements and physical and chemical index have reached GB
2716-2005 《Edible vegetable oil sanitary standard》, wherein the content of oleic acid, linoleic acid and palmitinic acid is up to 26.5% respectively,
36.6% and 23.4%, the yield of arhat fruit seed oil is up to 97.3%；In gained cupreol fine work, the content of cupreol is up to
99.9%, yield is up to 94.1%；
（2）The method of the present invention is that the completely new slave Siraitia grosvenorii of one kind extracts extraction arhat fruit seed oil in slag and extracts cupreol simultaneously
Method, technical process strong operability is at low cost, Siraitia grosvenorii resource high-efficiency comprehensive utilization, not only solve Siraitia grosvenorii production
The processing problem of middle solid waste, moreover it is possible to create considerable economic benefit, be suitable for industrialized production.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
It is that the waste residue after sweet tea glycosides, water is extracted with water in Siraitia grosvenorii fresh fruit that Siraitia grosvenorii used in the embodiment of the present invention, which extracts slag,
Content is 52%, mainly includes arhat fruit seed slag and Siraitia grosvenorii shell slag, wherein contained arhat fruit seed oil is in wet basis
Mass content is 6.28%, and mass content of the cupreol in wet basis is 2.3%；It is silica gel used in the embodiment of the present invention, anti-
Phase silica gel and aluminium oxide are purchased from Xi'an Sunresin New Materials Co., Ltd.；Ultrafiltration membrane used in the embodiment of the present invention
It is purchased from Jinan Hai De Water Management Equipment Ltd.；Raw material or chemical reagent used in the embodiment of the present invention, such as without special
Illustrate, is obtained by routine business approach.
In the embodiment of the present invention, using the content of gas chromatograph-mass spectrometer (GC-MS) detection arhat fruit seed oil, using efficient liquid
The content of phase chromatography detection cupreol.
Embodiment 1
The method that arhat fruit seed oil is extracted in slag is extracted from Siraitia grosvenorii：
（1）Refluxing extraction：It is extracted to 100kg Siraitia grosvenorii and 50L water and 1500L 6# solvent for extraction is added in slag, in revolving speed 30r/
Min at 80 DEG C, is stirred at reflux and extracts 3h, extracting solution stratification 2h is obtained organic extract except the water layer of sub-cloud；
（2）Silicagel column absorption：By step（1）Gained organic extract is with flow velocity 0.5BV/h, upper silicagel column（The Gao Jing of silicagel column
Than being 4:1, the volume of silica gel is 50L）Absorption collects efflux, obtains arhat fruit seed crude oil solution；
（3）Purification：To step（2）2kg diatomite is added in gained arhat fruit seed crude oil solution, at 50 DEG C, heating stirring 1h,
After being cooled to room temperature, then the ultrafiltration membrane for being 1000Da with molecular cut off, it is filtered at 2.0MPa, ultrafiltrate is concentrated into without molten
Agent obtains 6.05kg arhat fruit seed olein product.
The method for extracting cupreol simultaneously：
By step（2）Silicagel column 100L, the sodium hydrate aqueous solution that mass concentration is 2% after middle upper prop absorption, with flow velocity
0.5BV/h elution, eluent are extracted with 100L 6# solvent for extraction, stratification 1.5h, except the water layer of sub-cloud, organic layer
It is washed with water to neutrality, is concentrated, it is dry, obtain 2.5kg cupreol crude product；Again by 2.5kg cupreol crude product 7.5L ethyl alcohol,
It is dissolved by heating at 60 DEG C, 4.5L water is added, is cooled to 5 DEG C, at revolving speed 30r/min, stirring and crystallizing 12h, centrifugal filtration is used
1.8L, 0 DEG C of ethanol washing crystal freezed, it is dry, obtain 2.16kg cupreol fine work.
Arhat fruit seed olein product obtained by the embodiment of the present invention be it is faint yellow, organoleptic requirements and physical and chemical index have reached GB
2716-2005 《Edible vegetable oil sanitary standard》；It is detected through gas chromatograph-mass spectrometer (GC-MS), arhat fruit seed obtained by the present embodiment
In olein product, the content of oleic acid, linoleic acid and palmitinic acid is respectively 25.2%, 36.6% and 21.7%, and the yield of arhat fruit seed oil is
97.3%；Through high performance liquid chromatography detection, in cupreol fine work obtained by the present embodiment, the content of cupreol is 99.8%, β-
The yield of sitosterol is 93.7%.
Embodiment 2
The method that arhat fruit seed oil is extracted in slag is extracted from Siraitia grosvenorii：
（1）Refluxing extraction：It is extracted to 200kg Siraitia grosvenorii and 150L water and 4000L petroleum ether is added in slag, in revolving speed 60r/min, 85
At DEG C, it is stirred at reflux and extracts 2h, extracting solution stratification 2h is obtained into organic extract except the water layer of sub-cloud；
（2）The absorption of reverse phase silica gel column：By step（1）Gained organic extract is with flow velocity 1.0BV/h, upper reverse phase silica gel column（Reverse phase
The ratio of height to diameter of silicagel column is 8:1, the volume of reverse phase silica gel is 40L）Absorption collects efflux, obtains arhat fruit seed crude oil solution；
（3）Purification：To step（2）5kg diatomite is added in gained arhat fruit seed crude oil solution, at 40 DEG C, heating stirring 2h,
After being cooled to room temperature, then the ultrafiltration membrane for being 2000Da with molecular cut off, it is filtered at 1.0MPa, ultrafiltrate is concentrated into without molten
Agent obtains 11.8kg arhat fruit seed olein product.
The method for extracting cupreol simultaneously：
By step（2）Reverse phase silica gel column 100L, the potassium hydroxide aqueous solution that mass concentration is 3% after middle upper prop absorption, with stream
Fast 1.0BV/h elution, eluent 150L petroleum ether extraction, stratification 2h, except the water layer of sub-cloud, organic layer is washed with water
To neutrality, it is concentrated, it is dry, obtain 5.1kg cupreol crude product；Again by 5.1kg cupreol crude product 20.4L methanol, at 50 DEG C
Lower heating for dissolving is added 40.8L water, is cooled to 5 DEG C, and at revolving speed 40r/min, stirring and crystallizing for 24 hours, use by centrifugal filtration
5.1L, -2 DEG C of methanol freezed wash crystal, dry, obtain 4.33kg cupreol fine work.
Arhat fruit seed olein product obtained by the embodiment of the present invention be it is faint yellow, organoleptic requirements and physical and chemical index have reached GB
2716-2005 《Edible vegetable oil sanitary standard》；It is detected through gas chromatograph-mass spectrometer (GC-MS), arhat fruit seed obtained by the present embodiment
In olein product, the content of oleic acid, linoleic acid and palmitinic acid is respectively 24.7%, 34.9% and 20.5%, and the yield of arhat fruit seed oil is
95.2%；Through high performance liquid chromatography detection, in cupreol fine work obtained by the present embodiment, the content of cupreol is 99.9%, β-
The yield of sitosterol is 94.1%.
Embodiment 3
The method that arhat fruit seed oil is extracted in slag is extracted from Siraitia grosvenorii：
（1）Refluxing extraction：It is extracted to 100kg Siraitia grosvenorii and 80L water and 2000L ethyl acetate is added in slag, in revolving speed 40r/min,
At 78 DEG C, it is stirred at reflux and extracts 4h, extracting solution stratification 1.5h is obtained into organic extract except the water layer of sub-cloud；
（2）Alumina column absorption：By step（1）Gained organic extract is with flow velocity 0.5BV/h, upper alumina column（Alumina column
Ratio of height to diameter be 5:1, the volume of aluminium oxide is 40L）Absorption collects efflux, obtains arhat fruit seed crude oil solution；
（3）Purification：To step（2）3kg active carbon is added in gained arhat fruit seed crude oil solution, at 45 DEG C, heating stirring 2h,
After being cooled to room temperature, then the ultrafiltration membrane for being 800Da with molecular cut off, filtered at 2.0MPa, ultrafiltrate be concentrated into it is solvent-free,
Obtain 5.72kg arhat fruit seed olein product.
The method for extracting cupreol simultaneously：
By step（2）Alumina column 160L, the sodium hydrate aqueous solution that mass concentration is 1.5% after middle upper prop absorption, with stream
Fast 0.5BV/h elution, eluent are extracted with 100L ethyl acetate, stratification 2.5h, except the water layer of sub-cloud, organic layer water
Washing is concentrated, drying obtains 2.4kg cupreol crude product to neutrality；Again by 2.4kg cupreol crude product 12L isopropanol,
It is dissolved by heating at 65 DEG C, 36L water is added, is cooled to 10 DEG C, at revolving speed 20r/min, stirring and crystallizing 16h, centrifugal filtration is used
1.2L, 5 DEG C of isopropanols freezed wash crystal, dry, obtain 2.13 kg cupreol fine work.
Arhat fruit seed olein product obtained by the embodiment of the present invention be it is faint yellow, organoleptic requirements and physical and chemical index have reached GB
2716-2005 《Edible vegetable oil sanitary standard》；It is detected through gas chromatograph-mass spectrometer (GC-MS), arhat fruit seed obtained by the present embodiment
In olein product, the content of oleic acid, linoleic acid and palmitinic acid is respectively 26.5%, 34.1% and 23.4%, and the yield of arhat fruit seed oil is
92.3%；Through high performance liquid chromatography detection, in cupreol fine work obtained by the present embodiment, the content of cupreol is 99.8%, β-
The yield of sitosterol is 92.6%.
Claims (10)
1. a kind of extract the method for extracting arhat fruit seed oil in slag from Siraitia grosvenorii, which is characterized in that include the following steps：
（1）Refluxing extraction：It is extracted to Siraitia grosvenorii and water and fat-soluble organic solvent is added in slag, extraction is stirred at reflux, by extracting solution
Stratification obtains organic extract except the water layer of sub-cloud；
（2）Packed column absorption：By step（1）Packed column adsorbs on gained organic extract, collects efflux, it is thick to obtain arhat fruit seed
Oil solution；
（3）Purification：To step（2）It is added decolorising agent in gained arhat fruit seed crude oil solution, heating stirring, after being cooled to room temperature,
Ultrafiltration membrance filter is used again, and ultrafiltrate is concentrated into solvent-free, obtains arhat fruit seed olein product.
2. the method for extracting arhat fruit seed oil in slag is extracted from Siraitia grosvenorii according to claim 1, it is characterised in that：Step
（1）In, it is that the waste residue after sweet tea glycosides is extracted with water in Siraitia grosvenorii fresh fruit that the Siraitia grosvenorii, which extracts slag, mainly comprising arhat fruit seed slag and
Siraitia grosvenorii shell slag, wherein mass content of the contained arhat fruit seed oil in wet basis is 5~8%, and cupreol is in wet basis
In mass content be 1~4%；The volume of water and fat-soluble organic solvent and Siraitia grosvenorii extract the volume matter of slag wet basis quality
Amount is than being 0.5~1.0:15~20:1；The fat-soluble organic solvent is petroleum ether, 6# solvent for extraction, 120# extraction solvent
One or more of oil or ethyl acetate.
3. according to claim 1 or claim 2 extract the method for extracting arhat fruit seed oil in slag from Siraitia grosvenorii, it is characterised in that：Step
Suddenly（1）In, the revolving speed for being stirred at reflux extraction is 20~60 r/min, and temperature is 75~85 DEG C, and the time is 2~4h；It is described
The time of stratification is 1~2h.
4. extracting the method for extracting arhat fruit seed oil in slag described according to claim 1~one of 3 from Siraitia grosvenorii, feature exists
In：Step（2）In, the flow velocity of upper prop is 0.1~1.0BV/h；The ratio of height to diameter of the packed column is 2~10:1；The packed column
In filler and Siraitia grosvenorii extract slag wet basis volume mass ratio be 0.1~0.5:1；Filler in the packed column is silicon
One or more of glue, reverse phase silica gel or aluminium oxide.
5. extracting the method for extracting arhat fruit seed oil in slag described according to claim 1~one of 4 from Siraitia grosvenorii, feature exists
In：Step（3）In, the dosage of the decolorising agent is equivalent to 1~5% that Siraitia grosvenorii extracts slag wet basis quality；The decolorising agent is silicon
One or more of diatomaceous earth, active carbon, bentonite, activated alumina or concave convex rod；The temperature of the heating stirring be 40~
60 DEG C, the time is 1~2h；The molecular cut off of the ultrafiltration membrane is 500~3000Da；The pressure of the filtering be 0.5~
2.0MPa。
6. extracting β-paddy while a kind of extraction arhat fruit seed oil from Siraitia grosvenorii extraction slag described in one of Claims 1 to 5
The method of sterol, it is characterised in that：By step（2）Packed column eluted through lye after the absorption of middle upper prop, eluent is with fat-soluble
Organic solvent extraction, stratification, except the water layer of sub-cloud, organic layer is washed with water to neutrality, is concentrated, dry, obtains β-paddy steroid
Alcohol crude product；Cupreol crude product is dissolved by heating with low-carbon alcohols again, water is added, cooling, stirring and crystallizing, crystal is washed in filtering, dry
It is dry, obtain cupreol fine work.
7. the side of cupreol is extracted while extracting from Siraitia grosvenorii and extracting arhat fruit seed oil in slag according to claim 6
Method, it is characterised in that：The dosage of the lye is 2~5BV；The lye is the aqueous solution of sodium hydroxide and/or potassium hydroxide,
Mass concentration is 1~5%；The flow velocity of the elution is 0.1~1.0BV/h.
8. extracting cupreol while extracting from Siraitia grosvenorii and extracting arhat fruit seed oil in slag described according to claim 6 or 7
Method, it is characterised in that：The volume mass ratio that the fat-soluble organic solvent and Siraitia grosvenorii extract slag wet basis is 0.5~1.0:
1；The fat-soluble organic solvent be one of petroleum ether, 6# solvent for extraction, 120# solvent for extraction or ethyl acetate or
It is several；The time of the stratification is 1~3h.
9. extracting β-paddy while extracting from Siraitia grosvenorii and extracting arhat fruit seed oil in slag according to one of claim 6~8
The method of sterol, it is characterised in that：The volume mass ratio of the low-carbon alcohols and cupreol crude product is 2~5:1；The heating
Temperature is 40~70 DEG C；The volume ratio of the water and low-carbon alcohols is 0.5~3.0:1；The temperature of the stirring and crystallizing is 5~10
DEG C, the speed of stirring is 20~60 r/min, and the time of stirring and crystallizing is 12~24 h；The low-carbon alcohols are methanol, ethyl alcohol, different
One or more of propyl alcohol or n-butanol.
10. extracting β-paddy while extracting from Siraitia grosvenorii and extracting arhat fruit seed oil in slag according to one of claim 6~9
The method of sterol, it is characterised in that：It is described to be filtered into centrifugal filtration；Crystal is washed with the low-carbon alcohols of freezing；The freezing it is low
The volume mass ratio of carbon alcohol and cupreol crude product is 0.5~1.0:1；The temperature of the low-carbon alcohols of the freezing is -5~5 DEG C；Institute
Stating low-carbon alcohols is one or more of methanol, ethyl alcohol, isopropanol or n-butanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810747506.7A CN108864238A (en) | 2018-07-09 | 2018-07-09 | The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810747506.7A CN108864238A (en) | 2018-07-09 | 2018-07-09 | The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108864238A true CN108864238A (en) | 2018-11-23 |
Family
ID=64300454
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810747506.7A Pending CN108864238A (en) | 2018-07-09 | 2018-07-09 | The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108864238A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111112304A (en) * | 2020-02-05 | 2020-05-08 | 湖南华诚生物资源股份有限公司 | Method for extracting mixed alcohol from waste residue generated in production of natural ferulic acid |
| CN111171099A (en) * | 2020-01-17 | 2020-05-19 | 杭州益品新五丰药业有限公司 | Method for extracting sitosterol by double-solvent crystallization and sitosterol extracted by using method |
| CN111393400A (en) * | 2020-04-23 | 2020-07-10 | 湖南华诚生物资源股份有限公司 | Method for preparing squalene, vitamin E and sterol from fructus momordicae seed kernels |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001321121A (en) * | 2000-05-11 | 2001-11-20 | Ichimaru Pharcos Co Ltd | Hair growing and restoring food and drink |
| CN101177648A (en) * | 2007-12-12 | 2008-05-14 | 国家粮食储备局无锡科学研究设计院 | Method for extracting grape seed oil and procyanidine from grape seeds by one-step process |
-
2018
- 2018-07-09 CN CN201810747506.7A patent/CN108864238A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001321121A (en) * | 2000-05-11 | 2001-11-20 | Ichimaru Pharcos Co Ltd | Hair growing and restoring food and drink |
| CN101177648A (en) * | 2007-12-12 | 2008-05-14 | 国家粮食储备局无锡科学研究设计院 | Method for extracting grape seed oil and procyanidine from grape seeds by one-step process |
Non-Patent Citations (2)
| Title |
|---|
| 李俊 等: "罗汉果化学成分的研究", 《中国中药杂志》 * |
| 陈全斌 等: "不同方法提取罗汉果种籽油脂的研究", 《广东化工》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111171099A (en) * | 2020-01-17 | 2020-05-19 | 杭州益品新五丰药业有限公司 | Method for extracting sitosterol by double-solvent crystallization and sitosterol extracted by using method |
| CN111112304A (en) * | 2020-02-05 | 2020-05-08 | 湖南华诚生物资源股份有限公司 | Method for extracting mixed alcohol from waste residue generated in production of natural ferulic acid |
| CN111393400A (en) * | 2020-04-23 | 2020-07-10 | 湖南华诚生物资源股份有限公司 | Method for preparing squalene, vitamin E and sterol from fructus momordicae seed kernels |
| CN111393400B (en) * | 2020-04-23 | 2022-02-08 | 湖南华诚生物资源股份有限公司 | Method for preparing squalene, vitamin E and sterol from fructus momordicae seed kernels |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101690573B (en) | Production method of fructus monordicae extract with over 60% of mogroside V content | |
| CN101386636B (en) | Mogroside extraction method from grosvenor momordica | |
| CN102106928B (en) | Method for preparing high-purity oil tea saponins | |
| CN108752231B (en) | Method for extracting theanine from sweet tea and simultaneously extracting rubusoside and tea polyphenol | |
| CN108864238A (en) | The method that arhat fruit seed oil and cupreol are extracted in slag is extracted from Siraitia grosvenorii | |
| CN109674843A (en) | A kind of method for extraction and purification of dried fructus momordicae comprehensive utilization | |
| CN111960930A (en) | Method for separating and purifying cannabidiol from industrial cannabis sativa leaves | |
| CN101407535B (en) | Preparation of high-purity Momordica grosvenori mogroside V | |
| CN106967133B (en) | A method of extracting high-purity rebaudioside D from steviol glycoside refinement mother liquor | |
| CN110105458A (en) | The method that polysaccharide and PEARLITOL 25C are extracted in waste liquid is extracted from mogroside | |
| CN105132172A (en) | Method for preparing orris root flavonoid matter for tobaccos from orris roots | |
| CN109320400A (en) | A method of natural mannitol is extracted from mogroside production waste liquid | |
| CN102432651A (en) | Preparation method of geniposide | |
| CN107721967A (en) | A kind of green-tea extract production technology of high EGCG content | |
| CN104926719B (en) | A kind of method that trigonelline is extracted from fructus cannabis | |
| WO2022247097A1 (en) | Method for separating active ingredients from siraitia grosvenorii flowers | |
| CN102070411A (en) | Method for refining honokiol | |
| CN109369733A (en) | A method of extracting a variety of flavone compounds simultaneously from leaf of Radix Et Rhizoma Fagopyri Tatarici | |
| CN108516996A (en) | The extracting method of Siraitia grosvenorii prebiotics and the method for extracting momordica glycoside V simultaneously | |
| CN109021046A (en) | A method of extracting quercitin and mountain naphthalene glycosides simultaneously from Siraitia grosvenorii cauline leaf | |
| CN102942611A (en) | Method for preparing high-purity siamenoside I | |
| CN100424092C (en) | Triterpene glucoside natural sweet taste inhibitor, its extraction method and application | |
| CN105566944B (en) | The method that decolouring chilli extract and capsochrome are separated in chilli extract crude product | |
| CN103833809A (en) | Novel extraction and separation process of naringin | |
| CN103408539A (en) | Production method of high-purity silibinin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181123 |
|
| RJ01 | Rejection of invention patent application after publication |