CN102250195A - Method for producing xanthoceraside - Google Patents
Method for producing xanthoceraside Download PDFInfo
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- CN102250195A CN102250195A CN 201110186943 CN201110186943A CN102250195A CN 102250195 A CN102250195 A CN 102250195A CN 201110186943 CN201110186943 CN 201110186943 CN 201110186943 A CN201110186943 A CN 201110186943A CN 102250195 A CN102250195 A CN 102250195A
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- 238000004519 manufacturing process Methods 0.000 title claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 244000248162 Xanthoceras sorbifolium Species 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 23
- 239000000919 ceramic Substances 0.000 claims abstract description 19
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 150000001298 alcohols Chemical class 0.000 claims abstract description 16
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 9
- 229920001277 pectin Polymers 0.000 claims abstract description 9
- 239000001814 pectin Substances 0.000 claims abstract description 9
- 235000010987 pectin Nutrition 0.000 claims abstract description 9
- 238000010828 elution Methods 0.000 claims abstract description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 57
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical class CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 24
- 235000009240 Xanthoceras sorbifolium Nutrition 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 22
- 230000002411 adverse Effects 0.000 claims description 18
- 239000000284 extract Substances 0.000 claims description 17
- 239000000706 filtrate Substances 0.000 claims description 13
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 12
- 238000003809 water extraction Methods 0.000 claims description 8
- 239000000470 constituent Substances 0.000 claims description 6
- 238000005516 engineering process Methods 0.000 claims description 6
- 229930182490 saponin Natural products 0.000 claims description 6
- 150000007949 saponins Chemical class 0.000 claims description 6
- 235000017709 saponins Nutrition 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 229920001661 Chitosan Polymers 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 235000015203 fruit juice Nutrition 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000049 pigment Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 11
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004040 coloring Methods 0.000 abstract 1
- 239000003480 eluent Substances 0.000 abstract 1
- 238000010262 high-speed countercurrent chromatography Methods 0.000 abstract 1
- 239000002023 wood Substances 0.000 description 9
- 241000196324 Embryophyta Species 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000012141 concentrate Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 229920006395 saturated elastomer Polymers 0.000 description 4
- -1 glycoside compound Chemical class 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 238000005374 membrane filtration Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 208000024827 Alzheimer disease Diseases 0.000 description 1
- 208000014644 Brain disease Diseases 0.000 description 1
- 208000036626 Mental retardation Diseases 0.000 description 1
- 208000027089 Parkinsonian disease Diseases 0.000 description 1
- 206010034010 Parkinsonism Diseases 0.000 description 1
- 241000612118 Samolus valerandi Species 0.000 description 1
- 206010039966 Senile dementia Diseases 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 230000003925 brain function Effects 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000003181 encephalopathic effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 208000005346 nocturnal enuresis Diseases 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
- Saccharide Compounds (AREA)
Abstract
The invention relates to the field of development and utilization of shiny-leaved yellowhorn and discloses a method for extracting xanthoceraside from shells, fruit stems and/or flowers of the shiny-leaved yellowhorn. The method provided by the invention comprises the following steps of: firstly, selecting dry and mildew-free shells, fruit stems and/or flowers of the shiny-leaved yellowhorn; crushing until the granularity is 20-40 meshes; extracting by utilizing alcohols with the volume percentage concentration of 50-95% or water to obtain an extracting solution; processing the extracting solution extracted with the alcohols by a macroporous resin or concentrating the extracting solution extracted by water and then processing the concentrated solution by the macroporous resin to remove sugar and pectin; enriching effective components and carrying out a gradient elution on the resin column through utilizing the ethanol with the volume percentage concentration of 20-95% and de-coloring the eluent; respectively selecting ceramic membranes with the molecular weights of 400-800 and 3000-10000 to filter ineffective components two times and intercepting a part containing the xanthoceraside; then separating and purifying by utilizing a high-speed countercurrent chromatography to obtain the single-component xanthoceraside. The method provided by the invention has the advantages of high product purity, high yield, short time, capabilities of saving raw materials and cost and realizing large-scale production and the like.
Description
Technical field
The present invention relates to Wood of Shinyleaf Yellowhorn development and use field, a kind of specifically from shinyleaf yellowhorn fruit shell, carpopodium and/or the active substance-shinyleaf yellowhorn shell glycoside compound of extraction spending, the method for accomplishing scale production.
Background technology
Wood of Shinyleaf Yellowhorn (Xanthoceras sorbifolia Bunge) is that the distinctive oil of China is used and medicinal economic tree among the people; only a genus is a kind of; mainly be distributed in Liaoning, the Inner Mongol and Hexi Corridor one band; Wood of Shinyleaf Yellowhorn is machaka or arbor, has excellent characteristics such as drought-enduring, cold-resistant, anti-lean book, is the desirable seeds of protection environment and greening environment; yield positive results behind the growth of seedling 2-3; the best fruiting period is long, and the tree life-span is also long, and century-old above veteran still can yield positive results.
Wood of Shinyleaf Yellowhorn kind benevolence oil-containing 55-60% can be used for food, medicine, makeup, also can make technical oils, is superior oil resource.Cauline leaf can be used as medicine.Plant benevolence and be developed as the clinical application for the treatment of bed-wetting.Country has classified Wood of Shinyleaf Yellowhorn as northern important energy matter plant, plant in a large number, to satisfy social needs.
Xanthoceraside has control brain aging and cerebro-vascular diseases, increases intelligence, treats the encephalopathics that brain function is unsound or obstacle causes such as senile dementia, parkinsonism, urine urgency-frequency and mental retardation unusual effect is all arranged.Can be prepared as the medicine and the healthcare products of disease of brain; Xanthoceraside also can be prepared as the medicine and the healthcare products of anti-curing oncoma.
Summary of the invention
At above shortcomings part in the prior art, the object of the present invention is to provide a kind of production method of Xanthoceraside.
The present invention adopts following technical scheme:
A kind of production method of Xanthoceraside, press following technology and step:
1) choose drying, do not have shinyleaf yellowhorn fruit shell, carpopodium and/or the flower go mouldy;
2) step 1) is selected shell, carpopodium and/or pollen are broken into the 20-40 order;
3) with step 2) in shell, carpopodium and/or the flower pulverized to adopt concentration of volume percent be alcohols or the water extraction of 50-95%, obtain extracting solution;
4) extracting solution that extracts through alcohols of step 3) is crossed macroporous resin or concentrated macroporous resin, remove desaccharification, pectin through the extracting solution of water extraction, active constituent-enriched, with concentration of volume percent is the ethanol gradient elution resin column of 20-95%, the elutriant decolouring;
5) solution after the decolouring, selecting molecular weight respectively is that 400～800 and 3000～10000 ceramic membrane filters invalid components twice, holds back the part that contains Xanthoceraside, separates and purifying with high speed adverse current chromatogram then, promptly gets the Xanthoceraside of single component.
The solution system of high speed adverse current chromatogram methyl alcohol by volume wherein: water: phosphoric acid is 60～80: 20～50: 0.01～0.04; Flow velocity is 2～40ml/min, and the detection wavelength is 225nm.
The alcohols that adopts in the step 3) is one or more the combination in methyl alcohol, ethanol, butanols or the propyl carbinol.
Solid-liquid ratio is 1 in the step 3): 5-15 times (W: V), temperature is 20-100 ℃, and the time is 1-3 hour, and stirs, lixiviate 2-3 time, and united extraction liquid reclaims alcohols, and water liquid is standby.
Adopt intensified by ultrasonic wave to extract and/or microwave reinforced extraction in the step 3), ultrasonic wave or microwave power are 400-800W.
The one or more kinds of mixing in magnesium oxide, gac and/or the atlapulgite are adopted in decolouring in the step 4).
Ceramic membrane liquid is before crossed in the decolouring back in the step 5), uses n-butanol extraction, reclaims propyl carbinol.
The present invention also can take following method and step:
A kind of production method of Xanthoceraside, press following technology and step:
1) choose drying, do not have shinyleaf yellowhorn fruit shell, carpopodium and/or the flower go mouldy;
2) step 1) is selected shell, carpopodium and/or pollen are broken into the 20-40 order;
3) with step 2) in shell, carpopodium and/or the flower pulverized to adopt concentration of volume percent be alcohols or the water extraction of 50-95%, obtain extract;
4) with the extract that extracts through alcohols of step 3) or through the spissated water liquid of the extracting solution of water extraction with flocculation agent chitosan, 101 fruit juice precipitation, remove desaccharification, pectin, enrichment contains the filtrate of effective composition;
5) through the saturated n-butanol extraction of filtrate water of step 4), reclaim propyl carbinol, the total saponins dissolving, the selection molecular weight is 500～10000 ceramic membrane filter invalid components, hold back the part that contains Xanthoceraside, separate with high speed adverse current chromatogram then, promptly get the Xanthoceraside of single component.
The solution system of high speed adverse current chromatogram methyl alcohol by volume wherein: water: phosphoric acid is 60～80: 20～50: 0.01～0.04; Flow velocity is 2～40ml/min, and the detection wavelength is 225nm.
The alcohols that adopts in present method step 3) is one or more the combination in methyl alcohol, ethanol, butanols or the propyl carbinol.
Solid-liquid ratio is 1 in the step 3): 5-15 times (W: V), temperature is 20-100 ℃, and the time is 1-3 hour, and stirs, lixiviate 2-3 time, and united extraction liquid reclaims alcohols, and water liquid is standby.
Adopt intensified by ultrasonic wave to extract and/or microwave reinforced extraction in the step 3), ultrasonic wave or microwave power are 400-800W.
Adopt decolouring macroporous resin adsorption pigment before crossing ceramic membrane in the step 5).
The structure of the Xanthoceraside that employing the inventive method is used to prepare is shown below 3-O-(α-L-arabinofuranosyl (1 → 3)-β-D-galactopyranosyl (1 → 2))-β-D-glucuronopyranosyl-21,22-diangeloyl-R
1-barrigenol,
The present invention has following technique effect and advantage:
1. the inventive method prepares Xanthoceraside purity and reaches more than 99%, and yield reaches 5 ‰, prepares the used time shortly to be no more than 1 hour, can be used for large-scale production;
2. adopt ultrasonic or the microwave-assisted extraction, can destroy the cell of plant, make solvent energy rapid osmotic in cell, quicken the leaching of effective constituent, greatly strengthened yield, have the time weak point, the extraction yield height does not destroy the advantages such as effective constituent of plant;
3. adopting and selecting molecular weight respectively is 400～800 and 3000～10000 ceramic membrane filter, removes unwanted composition, has saved separating step and time;
4. adopt the technology of high speed adverse current chromatogram to separate and purifying obtains final product and has the selectivity height, pollution-free, do not have extremely and adsorb the process repeatability advantages of higher;
5. utilize the inventive method can realize the extraction of high purity Xanthoceraside, the cost that economizes in raw materials is realized scale operation, make shinyleaf yellowhorn fruit shell, carpopodium and spend in active substance can fully develop, promote its economic worth.
Embodiment
Embodiment 1
Get and pulverize 50 jin of 20 order shinyleaf yellowhorn fruit shells, concentration of volume percent 70% ethanol lixiviate with 7 times of volumes, 100 ℃ of temperature, are extracted 3 times at 2 hours time, the stirring that does not stop, united extraction liquid reclaims ethanol, and water liquid is crossed macroporous resin, be respectively 20%, 50% and 95% ethanol gradient elution resin column with concentration of volume percent, reclaim ethanol; Water liquid decolours with magnesium oxide, and the employing molecular weight is twice filtration of ceramic membrane of 800 and 10000, separates with high speed adverse current chromatogram, and solution system is methyl alcohol by volume: water: phosphoric acid is 60: 20: 0.01; Flow velocity is 2ml/min, and the detection wavelength is 225nm, obtains Xanthoceraside, and purity is more than 99%, and yield is 3.5 ‰.
Embodiment 2
Get and pulverize 40 jin on 30 purpose Wood of Shinyleaf Yellowhorn carpopodiums, with concentration of volume percent 60% propyl carbinol of 8 times of volumes, 50 ℃ of temperature, assisting ultrasonic is extracted, power 500W, 1 hour time, extract 2 times, reclaim propyl carbinol, water liquid is crossed macroporous resin, be respectively 40%, 60% and 90% ethanol gradient elution resin column with concentration of volume percent, reclaim ethanol, water liquid is with adopting decolorizing with activated carbon.The selection molecular weight is 500 and 5000 ceramic membrane filter, will contain the Xanthoceraside part, separates with high speed adverse current chromatogram, and solution system is methyl alcohol by volume: water: phosphoric acid is 70: 30: 0.02; Flow velocity is 10ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 4 ‰.
Embodiment 3
Get pulverizing 20 purpose Wood of Shinyleaf Yellowhorn and spend 20 jin, with concentration of volume percent 65% methyl alcohol of 6 times of volumes, 60 ℃ of temperature, microwave-assisted extracts, power 400W, extracts 2 times at 50 minutes time, reclaim methyl alcohol, water liquid removes desaccharification, pectin with the flocculation agent chitosan, and enrichment contains the filtrate of effective composition; The n-butanol extraction that filtrate water is saturated, reclaim propyl carbinol, the total saponins dissolving, with D941 decolouring macroporous resin adsorption pigment, the selection molecular weight is 500 and 3000 ceramic membrane membrane filtration, holding back needs part, separates with high speed adverse current chromatogram, and solution system is methyl alcohol by volume: water: phosphoric acid is 80: 50: 0.04; Flow velocity is 30ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 3 ‰.
Embodiment 4
Get pulverizing 40 purpose Wood of Shinyleaf Yellowhorn and spend 20 jin, with concentration of volume percent 65% methyl alcohol of 10 times of volumes, 60 ℃ of temperature, microwave-assisted extracts, power 400W, extracts 2 times at 50 minutes time, reclaim methyl alcohol, water liquid removes desaccharification, pectin with 101 fruit juice precipitation, and enrichment contains the filtrate of effective composition; The n-butanol extraction that filtrate water is saturated, reclaim propyl carbinol, the total saponins dissolving, with ADS-7 decolouring macroporous resin adsorption pigment, the selection molecular weight is 800 and 3500 ceramic membrane membrane filtration, holding back needs part, separates with high speed adverse current chromatogram, and solution system is methyl alcohol by volume: water: phosphoric acid is 75: 25: 0.03; Flow velocity is 30ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 3 ‰.
Embodiment 5
Get and pulverize 50 jin of 25 purpose shinyleaf yellowhorn shells, water with 10 times of volumes, and adopt ultrasonic and microwave-assisted simultaneously, ultrasonic and microwave all is power 500W, 50 ℃ of temperature, 1.5 hours time, extract 2 times, united extraction liquid also concentrates, and crosses macroporous resin, be 50% with concentration of volume percent respectively, 70%, with 95% ethanol gradient elution resin column, activated carbon adds activated decoloration, and its filtrate selection molecular weight is 700 and 4000 ceramic membrane filter, and holding back needs part, separate with high speed adverse current chromatogram, solution system is methyl alcohol by volume: water: phosphoric acid is 60: 200: 0.01; Flow velocity is 40ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 5 ‰.
Embodiment 6
Get and pulverize 60 jin of 40 purpose shinyleaf yellowhorn shells, water with 15 times of volumes, and adopt microwave-assisted simultaneously, microwave power 600W, 70 ℃ of temperature, 3 hours time, extract 2 times, united extraction liquid also concentrates, and crosses macroporous resin, it with concentration of volume percent respectively 20%, 60% and 85% ethanol gradient elution resin column, activated decoloration, its filtrate selection molecular weight is 800 and 6000 ceramic membrane filter, holding back needs part, separate with high speed adverse current chromatogram, solution system is methyl alcohol by volume: water: phosphoric acid is 80: 50: 0.01; Flow velocity is 35ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 5 ‰.
Embodiment 7
Get and pulverize 70 jin of 30 purpose shinyleaf yellowhorn shells, water with 15 times of volumes, and adopt ultrasonic auxiliary simultaneously, power 600W, 70 ℃ of temperature, 1 hour time, extract 2 times, united extraction liquid also concentrates, and crosses macroporous resin, it with concentration of volume percent respectively 20%, 50% and 90% ethanol gradient elution resin column, the magnesium oxide decolouring, its filtrate selection molecular weight is 400 and 7000 ceramic membrane filter, holding back needs part, separate with high speed adverse current chromatogram, solution system is methyl alcohol by volume: water: phosphoric acid is 70: 20～50: 0.04; Flow velocity is 40ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 4 ‰.
Embodiment 8
Get and pulverize 40 jin on 30 purpose Wood of Shinyleaf Yellowhorn carpopodiums, with concentration of volume percent 60% propyl carbinol of 8 times of volumes, 50 ℃ of temperature, assisting ultrasonic is extracted, power 500W, extracts 2 times at 1 hour time, reclaim propyl carbinol, water liquid adopts the flocculation agent chitosan to remove desaccharification, pectin, and is active constituent-enriched, the n-butanol extraction that filtrate water is saturated, reclaim propyl carbinol, the total saponins dissolving.The selection molecular weight is 700 and 3000 ceramic membrane filter, will contain the Xanthoceraside part, separates with high speed adverse current chromatogram, and solution system is methyl alcohol by volume: water: phosphoric acid is 70: 30: 0.01; Flow velocity is 30ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 4 ‰.
Embodiment 9
Get and pulverize 60 jin of 40 purpose shinyleaf yellowhorn shells,, and adopt microwave-assisted simultaneously with the water of 15 times of volumes, microwave power 600W, 70 ℃ of temperature, are extracted 2 times at 3 hours time, united extraction liquid also concentrates, water liquid adopts 101 fruit juice precipitation to remove desaccharification, pectin, and is active constituent-enriched, the n-butanol extraction that filtrate water is saturated, reclaim propyl carbinol, the total saponins dissolving.The selection molecular weight is 800 and 3000 ceramic membrane filter, will contain the Xanthoceraside part, separates with high speed adverse current chromatogram, and the solution system of high speed adverse current chromatogram is methyl alcohol by volume: water: phosphoric acid is 80: 30: 0.02; Flow velocity is 25ml/min, and the detection wavelength is 225nm, prepares Xanthoceraside, and purity is more than 99%, and yield is 3.5 ‰.
Claims (10)
1. the production method of an Xanthoceraside is characterized in that, presses following technology and step:
1) choose drying, do not have shinyleaf yellowhorn fruit shell, carpopodium and/or the flower go mouldy;
2) step 1) is selected shell, carpopodium and/or pollen are broken into the 20-40 order;
3) with step 2) in shell, carpopodium and/or the flower pulverized to adopt concentration of volume percent be alcohols or the water extraction of 50-95%, obtain extracting solution;
4) extracting solution that extracts through alcohols of step 3) is crossed macroporous resin or concentrated macroporous resin, remove desaccharification, pectin through the extracting solution of water extraction, active constituent-enriched, with concentration of volume percent is the ethanol gradient elution resin column of 20-95%, the elutriant decolouring;
5) solution after the decolouring, selecting molecular weight respectively is that 400～800 and 3000～10000 ceramic membrane filters invalid components twice, holds back the part that contains Xanthoceraside, separates and purifying with high speed adverse current chromatogram then, promptly gets the Xanthoceraside of single component.
2. the production method of an Xanthoceraside is characterized in that, presses following technology and step:
1) choose drying, do not have shinyleaf yellowhorn fruit shell, carpopodium and/or the flower go mouldy;
2) step 1) is selected shell, carpopodium and/or pollen are broken into the 20-40 order;
3) with step 2) in shell, carpopodium and/or the flower pulverized to adopt concentration of volume percent be alcohols or the water extraction of 50-95%, obtain extract;
4) with the extract that extracts through alcohols of step 3) or through the spissated water liquid of the extracting solution of water extraction with flocculation agent chitosan, 101 fruit juice precipitation, remove desaccharification, pectin, enrichment contains the filtrate of effective composition;
5) through the saturated n-butanol extraction of filtrate water of step 4), reclaim propyl carbinol, the total saponins dissolving, the selection molecular weight is 500～10000 ceramic membrane filter invalid components, hold back the part that contains Xanthoceraside, separate with high speed adverse current chromatogram then, promptly get the Xanthoceraside of single component.
3. the production method of Xanthoceraside according to claim 1 and 2, it is characterized in that: the solution system of high speed adverse current chromatogram is methyl alcohol by volume: water: phosphoric acid is 60～80: 20～50: 0.01～0.04; Flow velocity is 2～40ml/min, and the detection wavelength is 225nm.
4. the production method of Xanthoceraside according to claim 1 and 2 is characterized in that: the alcohols that adopts in the step 3) is one or more the combination in methyl alcohol, ethanol, butanols or the propyl carbinol.
5. the production method of Xanthoceraside according to claim 1 and 2, it is characterized in that: solid-liquid ratio is 1 in the step 3): doubly (W: V), temperature is 20-100 ℃ to 5-15, time is 1-3 hour, and stirs lixiviate 2-3 time, united extraction liquid reclaims alcohols, and water liquid is standby.
6. the production method of Xanthoceraside according to claim 5 is characterized in that: adopt intensified by ultrasonic wave to extract and/or microwave reinforced extraction in the step 3), ultrasonic wave or microwave power are 400-800W.
7. the production method of Xanthoceraside according to claim 1 is characterized in that: the one or more kinds of mixing in the step 4) in decolouring employing magnesium oxide, gac and/or the atlapulgite.
8. the production method of Xanthoceraside according to claim 1 is characterized in that: cross ceramic membrane liquid before in the step 5) after the decolouring, use n-butanol extraction, reclaim propyl carbinol.
9. the production method of Xanthoceraside according to claim 2 is characterized in that: adopt decolouring macroporous resin adsorption pigment before crossing ceramic membrane in the step 5).
10. the production method of Xanthoceraside according to claim 1, it is characterized in that: the structure of described Xanthoceraside is shown below, 3-O-(α-L-arabinofuranosyl (1 → 3)-β-D-galactopyranosyl (1 → 2))-β-D-glucuronopyra nosyl-21,22-diangeloyl-R
1-barrigenol,
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102783656A (en) * | 2012-09-04 | 2012-11-21 | 山东理工大学 | Application of shiny-leaved yellowhorn flavone in lipid-lowering weight-losing field and preparation method of shiny-leaved yellowhorn flavone |
| CN102784090A (en) * | 2012-09-04 | 2012-11-21 | 山东理工大学 | Application of bunkanka saponin in whitening field and preparation method thereof |
| CN102784087A (en) * | 2012-09-04 | 2012-11-21 | 山东理工大学 | Application of shinyleaf yellowhorn flavone extracts in whitening field and extraction method thereof |
| CN102783654A (en) * | 2012-09-04 | 2012-11-21 | 山东理工大学 | Application of bunkanka saponin extract in weight losing and fat lowering fields |
| CN102793647A (en) * | 2012-09-04 | 2012-11-28 | 山东理工大学 | Method for extracting shinyleaf yellowhorn flavone substance and application of shinyleaf yellowhorn flavone substance in anti-aging industry |
| CN102796162A (en) * | 2012-09-04 | 2012-11-28 | 山东理工大学 | Method for extracting xanthoceras sorbifolia bunge husk saponins |
| CN102813214A (en) * | 2012-09-04 | 2012-12-12 | 山东理工大学 | Application of xanthoceras sorbifolia saponin in field of reducing lipid and losing weight and preparation method of xanthoceras sorbifolia saponin |
| CN102823873A (en) * | 2012-09-04 | 2012-12-19 | 山东理工大学 | Application of xanthoceras sorbifolia flavone to field of skin whitening and preparation method of xanthoceras sorbifolia flavone |
| CN103242412A (en) * | 2012-11-15 | 2013-08-14 | 沈阳药科大学 | Preparation method of shiny-leaved yellowhorn carpopodium and medical applications |
| CN106421077A (en) * | 2016-10-14 | 2017-02-22 | 哈尔滨理工大学 | New preparing method of high purity shiny-leaved yellowhorn total saponins extractive and application thereof |
| CN108101955A (en) * | 2018-01-26 | 2018-06-01 | 沈阳药科大学 | Compound in shinyleaf yellowhorn fruit shell and its preparation method and application |
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| CN115300559A (en) * | 2022-02-12 | 2022-11-08 | 兰州理工大学 | Application of xanthoceras sorbifolia husk saponin in resisting trichophyton rubrum and extraction and purification method thereof |
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| CN102796162A (en) * | 2012-09-04 | 2012-11-28 | 山东理工大学 | Method for extracting xanthoceras sorbifolia bunge husk saponins |
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| CN103242412A (en) * | 2012-11-15 | 2013-08-14 | 沈阳药科大学 | Preparation method of shiny-leaved yellowhorn carpopodium and medical applications |
| CN103242412B (en) * | 2012-11-15 | 2016-03-30 | 沈阳药科大学 | A kind of preparation method of Wood of Shinyleaf Yellowhorn carpopodium glycosides and medicinal use |
| CN106421077A (en) * | 2016-10-14 | 2017-02-22 | 哈尔滨理工大学 | New preparing method of high purity shiny-leaved yellowhorn total saponins extractive and application thereof |
| CN108101955A (en) * | 2018-01-26 | 2018-06-01 | 沈阳药科大学 | Compound in shinyleaf yellowhorn fruit shell and its preparation method and application |
| CN109010201A (en) * | 2018-10-30 | 2018-12-18 | 嘉文丽（福建）化妆品有限公司 | A kind of preparation method and application of almond ringdove chrysanthemum saponin(e |
| CN115300559A (en) * | 2022-02-12 | 2022-11-08 | 兰州理工大学 | Application of xanthoceras sorbifolia husk saponin in resisting trichophyton rubrum and extraction and purification method thereof |
| CN115300559B (en) * | 2022-02-12 | 2023-10-27 | 兰州理工大学 | Application of shinyleaf yellowhorn shell saponin in resisting trichophyton rubrum and extraction and purification method thereof |
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