CN101336949B - Method for extracting polysaccharide and flavone from Gynura divaricata - Google Patents
Method for extracting polysaccharide and flavone from Gynura divaricata Download PDFInfo
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- 229930003944 flavones Natural products 0.000 title claims abstract description 123
- 235000011949 flavones Nutrition 0.000 title claims abstract description 123
- 241001558017 Gynura Species 0.000 title claims abstract description 66
- 150000004676 glycans Polymers 0.000 title claims abstract description 40
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 40
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 40
- 150000004804 polysaccharides Polymers 0.000 title claims abstract description 40
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N flavone Chemical compound O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims description 116
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 121
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000000284 extract Substances 0.000 claims abstract description 25
- 239000006228 supernatant Substances 0.000 claims abstract description 23
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000012153 distilled water Substances 0.000 claims abstract description 12
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 239000012535 impurity Substances 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 239000000287 crude extract Substances 0.000 claims description 39
- 238000001556 precipitation Methods 0.000 claims description 33
- 239000003480 eluent Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- 238000010828 elution Methods 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 13
- 238000000746 purification Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 238000004064 recycling Methods 0.000 claims description 10
- 238000000605 extraction Methods 0.000 claims description 8
- 238000004108 freeze drying Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 6
- 238000001694 spray drying Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 abstract description 59
- 150000002213 flavones Chemical class 0.000 abstract description 7
- 238000010298 pulverizing process Methods 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- 239000002244 precipitate Substances 0.000 abstract 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N D-Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- IKGXIBQEEMLURG-BKUODXTLSA-N Rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 6
- 229940081967 Rutin Drugs 0.000 description 6
- 239000003463 adsorbent Substances 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 238000007670 refining Methods 0.000 description 6
- 229930002876 rutin Natural products 0.000 description 6
- 235000005493 rutin Nutrition 0.000 description 6
- 229960004555 rutoside Drugs 0.000 description 6
- 239000012530 fluid Substances 0.000 description 5
- 239000011344 liquid material Substances 0.000 description 5
- 230000000274 adsorptive Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 210000004369 Blood Anatomy 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010003246 Arthritis Diseases 0.000 description 1
- 241000208838 Asteraceae Species 0.000 description 1
- 210000001124 Body Fluids Anatomy 0.000 description 1
- 206010006895 Cachexia Diseases 0.000 description 1
- 241000887125 Chaptalia nutans Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 208000004396 Mastitis Diseases 0.000 description 1
- 240000002686 Solanum melongena Species 0.000 description 1
- 206010044302 Tracheitis Diseases 0.000 description 1
- 230000003213 activating Effects 0.000 description 1
- 230000000975 bioactive Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 239000010839 body fluid Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002996 emotional Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000021285 flavonoid Nutrition 0.000 description 1
- 229930003935 flavonoids Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000005445 natural product Substances 0.000 description 1
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- 238000005192 partition Methods 0.000 description 1
- 230000001717 pathogenic Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting Effects 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
Abstract
The invention discloses a method for extracting polysaccharides and flavones from Gynura divaricata, which comprises the following steps of: (1) collecting leaf or stem of Gynura divaricata as raw material, removing impurities, pulverizing, extracting with water at a constant temperature, and filtering to obtain an extractive solution; (2) concentrating the extractive solution to obtain a concentrated solution; (3) adding a precipitant to the concentrated solution to separate out the polysaccharides precipitate, and separating the precipitate and the supernatant; (4) drying the precipitate to obtain Gynura divaricata polysaccharides extract; (5) recovering the solvent from the supernatant, adding water to the substrate to obtain flavones crude extractive solution; (6) purifying the flavones crude extractive solution with a resin column, eluting with distilled water, eluting with ethanol aqueous solution until no flavones are detected in the eluate, and mixing the ethanol eluates; and (7) recovering ethanol under reduced pressure, and drying the substrate to obtain flavones extract. The inventive method has the advantages of rapidness, convenience, low cost, high yield, etc.
Description
Technical field
The invention belongs to field of natural product extraction, relate to a kind of method of from Gynura divaricata, extracting polysaccharide and flavone simultaneously.
Background technology
Gynura divaricata (Gynura divaricata (L.) DC.), have another name called white back of the body Herba Senecionis Chrysanthemoidis, fork flower Herba Senecionis Chrysanthemoidis, herbaceos perennial, the Compositae Radix Gynurae belongs to. high 30～50cm, rhizome bulk, stem aubergine, by undercoat, be distributed in the south China and the west and south, the various places, Fujian all have, and happiness is born on the moist shaded place.The herb heat reliving and toxin-eliminating, activating blood circulation to dissipate blood stasis goes emaciation due to emotional upset swollen, and root is used as medicine, and the effect of pathogenic fire purging, removing heat from blood are arranged, promoting the production of body fluid is the common Chinese herbal medicine of various inflammation such as treatment mastitis among the people, arthritis, tracheitis.
Modern science studies show that and contain abundant polysaccharide and flavonoid bioactive substance in the Gynura divaricata, and at present, to measure research more for active component content in the relevant Gynura divaricata, and do not appear in the newspapers for the extraction process of flavone, polysaccharide in the Gynura divaricata.
Summary of the invention
The purpose of this invention is to provide a kind of method of from Gynura divaricata, extracting polysaccharide and flavone.
Technical scheme of the present invention is summarized as follows:
A kind of method of extracting polysaccharide and flavone from Gynura divaricata comprises the steps:
(1) be that impurity removing is pulverized with the leaf of Gynura divaricata or stem, add the water termostat lixiviate 1～3 time, during each lixiviate, the mass ratio of water and raw material is 5～30: 1, and extraction time is 2～10 hours, and temperature is 60～90 ℃, must extracting solution after the filtration;
(2) extracting solution is concentrated, the concentrated solution volume is 1/3～1/5 of an extracting liquid volume;
(3) in concentrated solution, add precipitant, leave standstill 2～24h, polysaccharide precipitation is separated out, precipitation separation and supernatant;
(4) the precipitation drying that separation is obtained obtains the Gynura divaricata polyoses extract;
(5) solvent in the recovery supernatant is dissolved in water substrate, and described amount of water is 1-3 a times of described raw materials quality, gets the flavone crude extract;
(6) with flavone crude extract resin column purification, the control flow velocity is 1～3ml/min behind the described flavone crude extract upper prop, first distilled water eluting with 5～10 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is 60～80% ethanol water eluting to the effluent no flavone detects (TLC detects no flavone), merges ethanol elution;
(7) decompression recycling ethanol, the ethanol in the Ex-all eluent, the dry flavone extract that gets of substrate.
Described Gynura divaricata is bright Gynura divaricata, dries Gynura divaricata or parch Gynura divaricata naturally.
Described precipitant is that concentration expressed in percentage by volume is that ethanol water or the concentration expressed in percentage by volume of 90%-100% is the aqueous acetone solution of 90%-100%, and the consumption of described precipitant is 1～5 times of concentrated solution volume.
The model of described resin column is: AB-8, D-101, D-140, DM-130, LSA-10, LSA-20 or HPD-600.
Described step is separated into centrifugalize or isolated by filtration described in (3).
Described simmer down to vacuum concentration of described step (2) or membrance concentration.
Dry described in described step (4) or the step (7) is lyophilization, vacuum drying or spray drying.
Advantage of the present invention: the invention discloses a kind of method of from Gynura divaricata, extracting polysaccharide and flavone, obtain polysaccharide, two kinds of active substances of flavone simultaneously by once extracting; The macroporous resin adsorption partition method is applied in the flavone process for refining, has good separating effect, flavones content height, do not destroy advantages such as flavone original structure and activity; Polyoses content in the polyose that obtains 〉=25% (with the glucose note), yield 〉=10%, flavones content in the flavone product 〉=44% (with the rutin note), yield 〉=1%.The present invention has filled up the blank of Gynura divaricata polysaccharide, flavone extracting method, have quick, easy, cost is low, the yield advantages of higher.
The specific embodiment
The present invention is further illustrated below by specific embodiment.
Embodiment 1
A kind of method of from Gynura divaricata, extracting polysaccharide and flavone, step is:
(1) get parch Gynura divaricata leaf 50g, remove impurity is pulverized, and adds water after the pulverizing and stirs, and than 80 ℃ of 25:1, temperature, extracting at constant temperature is 1 time under the time 4h condition at the liquid material, then through 300 order filter clothes filter extracting solution;
(2) extracting solution rotary evaporator vacuum concentration, getting the concentrated solution volume is 1/4 of extracting liquid volume;
(3) adding 4 times of concentration expressed in percentage by volumes to the concentrated solution volume in concentrated solution is 95% edible ethanol aqueous solution, leaves standstill 10h then, and polysaccharide precipitation is separated out, and with alcohol deposit fluid centrifugal 10min under the condition of 3600r/min, obtains precipitation and supernatant respectively;
(4) precipitation that separation is obtained is dissolved in water to the 500ml postlyophilization, gets the Gynura divaricata polyoses extract, and yield is 10.24%, and with the glucose note, polyoses content is 23.05%;
(5) the supernatant decompression recycling ethanol that centrifugalize is obtained is dissolved in water then to 100ml, gets the flavone crude extract;
(6) carry out purification with AB-8 type macroporous adsorbent resin, with flavone crude extract upper prop, the control flow velocity is 2ml/min, after treating that flavone is fully adsorbed by resin, first distilled water eluting with 7 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is that 80% ethanol water eluting does not detect (TLC detects no flavone) to there being flavone, merges ethanol elution;
(7) with the ethanol reclaim under reduced pressure in the eluent, the ethanol in the Ex-all eluent is dissolved in water then to 125ml, must make with extra care flavone extractive, refining flavone extractive gets the Gynura divaricata flavone extract through lyophilization, and yield is 1.04%, with the rutin note, general flavone content is 53.3%.
Embodiment 2
A kind of method of from Gynura divaricata, extracting polysaccharide and flavone, step is:
(1) take from and so dry Gynura divaricata leaf 50g, add water after the pulverizing and stir, than 80 ℃ of 20:1, temperature, extracting at constant temperature is 1 time under the time 6h condition at the liquid material, then through 300 order filter clothes filter extracting solution;
(2) extracting solution is used the rotary evaporator vacuum concentration, getting the concentrated solution volume is 1/4 of extracting liquid volume;
(3) adding 4 times of concentration expressed in percentage by volumes to the concentrated solution volume in concentrated solution is 95% edible ethanol aqueous solution, leaves standstill 10h then, and polysaccharide precipitation is separated out, and alcohol deposit fluid is filtered, and obtains precipitation and filtrate respectively;
(4) precipitation that separation is obtained is dissolved in water to the 500ml postlyophilization, gets the Gynura divaricata polyoses extract, and yield is 10%, and with the glucose note, polyoses content is 24.87%;
(5) ethanol in the recovery supernatant is dissolved in water then to 100ml, gets the flavone crude extract;
(6) carry out purification with AB-8 type macroporous adsorbent resin, with flavone crude extract upper prop, the control flow velocity is 2ml/min, after treating that flavone is fully adsorbed by resin, first distilled water eluting with 5 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is that 60% ethanol water eluting does not detect (TLC detects no flavone) to there being flavone, merges ethanol elution;
(7) with the ethanol reclaim under reduced pressure in the eluent, be dissolved in water then to 125ml, must make with extra care flavone extractive; Refining flavone extractive gets the Gynura divaricata flavone extract through lyophilization, and yield is 1.31%, and with the rutin note, general flavone content is 44.2%.
Embodiment 3
A kind of method of from Gynura divaricata, extracting polysaccharide and flavone, step is:
(1) get parch Gynura divaricata leaf 200g, add water after the pulverizing and stir, the liquid material than 20:1,80 ℃ of temperature, time 4h condition under extracting at constant temperature 2 times, through 300 order filter clothes filter extracting solution, merge extractive liquid;
(2) extracting solution is used the rotary evaporator vacuum concentration, getting the concentrated solution volume is 1/3 of extracting liquid volume;
(3) adding 4 times of concentration expressed in percentage by volumes to the concentrated solution volume in concentrated solution is 95% ethanol water, leaves standstill 8h then, and polysaccharide precipitation is separated out, and then with alcohol deposit fluid centrifugal 10min under the condition of 3600r/min, obtains precipitation and supernatant respectively;
The precipitation vacuum drying that (4) will separate mutually gets the Gynura divaricata polyoses extract, and yield is 13.5%, and with the glucose note, polyoses content is 21.05%;
(5) the supernatant decompression recycling ethanol that centrifugalize is obtained is dissolved in water then to 300ml, gets the flavone crude extract;
(6) carry out purification with AB-8 type macroporous adsorbent resin, with flavone crude extract upper prop, the control flow velocity is 3ml/min, after treating that flavone is fully adsorbed by resin, first distilled water eluting with 5 times of flavone crude extract volumes, reuse 70% ethanol elution does not detect (TLC detects no flavone) to there being flavone, merges ethanol elution;
(7) with the ethanol reclaim under reduced pressure in the eluent, the ethanol in the Ex-all eluent is dissolved in water then to 500ml, must make with extra care flavone extractive; Refining flavone extractive gets the Gynura divaricata flavone extract through lyophilization, and yield is 1.41%, and with the rutin note, general flavone content is 55.3%.
Embodiment 4
A kind of method of from Gynura divaricata, extracting polysaccharide and flavone, step is:
(1) get parch Gynura divaricata leaf 200g, than 25:1,80 ℃ of extracting at constant temperature 4h of temperature, extracting at constant temperature is 2 times under the time 3h condition at the liquid material, through 300 order filter clothes filter extracting solution, merge extractive liquid;
(2) extracting solution is used the rotary evaporator vacuum concentration, getting the concentrated solution volume is 1/3 of extracting liquid volume;
(3) adding 3 times of concentration expressed in percentage by volumes to the concentrated solution volume in concentrated solution is 90% edible ethanol aqueous solution, leaves standstill 24h then, and polysaccharide precipitation is separated out, and then with alcohol deposit fluid centrifugal 10min under the condition of 3600r/min, obtains precipitation and supernatant respectively;
(4) with above-mentioned precipitation vacuum drying, get the Gynura divaricata polyoses extract, yield is 13.3%, with the glucose note, polyoses content is 21.08%;
(5) the supernatant decompression recycling ethanol that centrifugalize is obtained is dissolved in water substrate to 300ml, gets the flavone crude extract;
(6) carry out purification with DM-130 type macroporous adsorbent resin, with flavone crude extract upper prop, the control flow velocity is 3ml/min, after treating that flavone is fully adsorbed by resin, first distilled water eluting with 5 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is that 70% ethanol water eluting does not detect (TLC detects no flavone) to there being flavone, merges ethanol elution;
(7) with the ethanol reclaim under reduced pressure in the eluent, be dissolved in water then to 500ml, must make with extra care flavone extractive; Refining flavone extractive gets the Gynura divaricata flavone extract through lyophilization, and yield is 1.01%, and with the rutin note, general flavone content is 54.9%.
Embodiment 5
A kind of method of from Gynura divaricata, extracting polysaccharide and flavone, step is:
(1) get bright Gynura divaricata stem 500g, add water after the pulverizing and stir, the liquid material than 8:1,80 ℃ of temperature, time 4h condition under extracting at constant temperature 1 time, through 300 order filter clothes filter extracting solution, merge extractive liquid;
(2) extracting solution is used the rotary evaporator vacuum concentration, getting the concentrated solution volume is 1/5 of extracting liquid volume;
(3) adding 4 times of concentration expressed in percentage by volumes to the concentrated solution volume in concentrated solution is 95% ethanol water, leaves standstill 12h then, and polysaccharide precipitation is separated out, and then with alcohol deposit fluid centrifugal 10min under the condition of 3600r/min, obtains precipitation and supernatant respectively;
(4) the precipitation vacuum drying that separation is obtained gets the Gynura divaricata polyoses extract, and yield is 20%, and with the glucose note, polyoses content is 20.05%;
(5) the supernatant decompression recycling ethanol that centrifugalize is obtained is dissolved in water then to 500ml, gets the flavone crude extract;
(6) carry out purification with AB-8 type macroporous adsorbent resin, with flavone crude extract upper prop, the control flow velocity is 3ml/min, after treating that flavone is fully adsorbed by resin, first distilled water eluting with 5 times of flavone crude extract volumes, reuse 70% ethanol elution does not detect (TLC detects no flavone) to there being flavone, merges ethanol elution;
(7) with the ethanol reclaim under reduced pressure in the eluent, the ethanol in the Ex-all eluent is dissolved in water then to 500ml, must make with extra care flavone extractive; Refining flavone extractive gets the Gynura divaricata flavone extract through lyophilization, and yield is 1.01%, and with the rutin note, general flavone content is 44.3%.
Embodiment 6
A kind of method of extracting polysaccharide and flavone from Gynura divaricata comprises the steps:
(1) be that impurity removing is cut into pulverizing with bright Gynura divaricata leaf, add the water termostat lixiviate 1 time, during each lixiviate, the mass ratio of water and raw material is 5: 1, and extraction time is 2 hours, and temperature is 60 ℃, must extracting solution after the filtration;
(2) with the extracting solution membrance concentration, the concentrated solution volume is 1/3 of an extracting liquid volume;
(3) adding concentration expressed in percentage by volume in concentrated solution is that 100% ethanol is precipitant, and the consumption of precipitant is 4 times of concentrated solution volume, leaves standstill 2h, and polysaccharide precipitation is separated out, centrifugalize precipitation and supernatant;
(4) the precipitation spray drying that separation is obtained obtains the Gynura divaricata polyoses extract;
(5) solvent in the recovery supernatant is dissolved in water substrate, and described amount of water is 1 times of described raw materials quality, gets the flavone crude extract;
(6) the flavone crude extract is used D-101 type macroporous adsorptive resins purification, the control flow velocity is 13ml/min behind the described flavone crude extract upper prop, first distilled water eluting with 5 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is 70% ethanol water eluting to the effluent no flavone detects (TLC detects no flavone), merges ethanol elution;
(7) decompression recycling ethanol, the ethanol in the Ex-all eluent, the substrate spray drying gets flavone extract.
Embodiment 7
A kind of method of extracting polysaccharide and flavone from Gynura divaricata comprises the steps:
(1) be that impurity removing is pulverized with drying the Gynura divaricata stem naturally, add the water termostat lixiviate 3 times, during each lixiviate, the mass ratio of water and raw material is 20: 1, and extraction time is 8 hours, and temperature is 90 ℃, must extracting solution after the filtration;
(2) with the extracting solution vacuum concentration, the concentrated solution volume is 1/4 of an extracting liquid volume;
(3) adding concentration expressed in percentage by volume in concentrated solution is that 100% acetone is precipitant, and the consumption of precipitant is 1 times of concentrated solution volume, leaves standstill 24h, and polysaccharide precipitation is separated out, isolated by filtration precipitation and supernatant;
(4) the precipitation vacuum drying that separation is obtained obtains the Gynura divaricata polyoses extract;
(5) solvent in the recovery supernatant is dissolved in water substrate, and described amount of water is 3 times of described raw materials quality, gets the flavone crude extract;
(6) the flavone crude extract is used D-140 type macroporous adsorptive resins purification, the control flow velocity is 1ml/min behind the described flavone crude extract upper prop, first distilled water eluting with 10 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is 80% ethanol water eluting to the effluent no flavone detects, and merges ethanol elution;
(7) decompression recycling ethanol, the ethanol in the Ex-all eluent, the substrate vacuum drying gets flavone extract.
Embodiment 8
A kind of method of extracting polysaccharide and flavone from Gynura divaricata comprises the steps:
(1) be that impurity removing is pulverized with parch Gynura divaricata stem, add the water termostat lixiviate 1 time, during each lixiviate, the mass ratio of water and raw material is 30: 1, and extraction time is 10 hours, and temperature is 85 ℃, must extracting solution after the filtration;
(2) extracting solution is concentrated, the concentrated solution volume is 1/5 of an extracting liquid volume;
(3) adding concentration expressed in percentage by volume in concentrated solution is that 90% aqueous acetone solution is a precipitant, and the consumption of precipitant is 5 times of concentrated solution volume, leaves standstill 10h, and polysaccharide precipitation is separated out, precipitation separation and supernatant;
(4) the precipitation drying that separation is obtained obtains the Gynura divaricata polyoses extract;
(5) solvent in the recovery supernatant is dissolved in water substrate, and described amount of water is 2 times of described raw materials quality, gets the flavone crude extract;
(6) the flavone crude extract is used LSA-10 type macroporous adsorptive resins purification, the control flow velocity is 2ml/min behind the described flavone crude extract upper prop, first distilled water eluting with 8 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is 80% ethanol water eluting to the effluent no flavone detects, and merges ethanol elution;
(7) decompression recycling ethanol, the ethanol in the Ex-all eluent, the dry flavone extract that gets of substrate.
Embodiment 9
A kind of method of extracting polysaccharide and flavone from Gynura divaricata comprises the steps:
(1) be that impurity removing is pulverized with parch Gynura divaricata leaf, add the water termostat lixiviate 1 time, during each lixiviate, the mass ratio of water and raw material is 30: 1, and extraction time is 10 hours, and temperature is 85 ℃, must extracting solution after the filtration;
(2) extracting solution is concentrated, the concentrated solution volume is 1/5 of an extracting liquid volume;
(3) adding concentration expressed in percentage by volume in concentrated solution is that 95% aqueous acetone solution is a precipitant, and the consumption of precipitant is 3 times of concentrated solution volume, leaves standstill 12h, and polysaccharide precipitation is separated out, precipitation separation and supernatant;
(4) the precipitation drying that separation is obtained obtains the Gynura divaricata polyoses extract;
(5) reclaim solvent in the supernatant, substrate is dissolved in water, and amount of water is 1 times of described raw materials quality, gets the flavone crude extract;
(6) the flavone crude extract is used LSA-20 type macroporous adsorptive resins purification, the control flow velocity is 3ml/min behind the described flavone crude extract upper prop, first distilled water eluting with 7 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is 75% ethanol water eluting to the effluent no flavone detects, and merges ethanol elution;
(7) decompression recycling ethanol, the ethanol in the Ex-all eluent, the dry flavone extract that gets of substrate.
Macroporous adsorbent resin in the present embodiment also can be selected the HPD-600 type for use, to form new embodiment.
Claims (7)
1. a method of extracting polysaccharide and flavone from Gynura divaricata is characterized in that comprising the steps:
(1) be that impurity removing is pulverized with the leaf of Gynura divaricata or stem, add the water termostat lixiviate 1～3 time, during each lixiviate, the mass ratio of water and raw material is 5～30: 1, and extraction time is 2～10 hours, and temperature is 60～90 ℃, must extracting solution after the filtration;
(2) extracting solution is concentrated, the concentrated solution volume is 1/3～1/5 of an extracting liquid volume;
(3) in concentrated solution, add precipitant, leave standstill 2～24h, polysaccharide precipitation is separated out, precipitation separation and supernatant;
(4) the precipitation drying that separation is obtained obtains the Gynura divaricata polyoses extract;
(5) solvent in the recovery supernatant is dissolved in water substrate, and described amount of water is 1-3 a times of described raw materials quality, gets the flavone crude extract;
(6) with flavone crude extract resin column purification, the control flow velocity is 1～3ml/min behind the described flavone crude extract upper prop, first distilled water eluting with 5～10 times of flavone crude extract volumes, the reuse concentration expressed in percentage by volume is 60～80% ethanol water eluting to the effluent no flavone detects, and merges ethanol elution;
(7) decompression recycling ethanol, the ethanol in the Ex-all eluent, the dry flavone extract that gets of substrate.
2. the method for extracting polysaccharide and flavone from Gynura divaricata according to claim 1 is characterized in that described Gynura divaricata is bright Gynura divaricata, dries Gynura divaricata or parch Gynura divaricata naturally.
3. the method for from Gynura divaricata, extracting polysaccharide and flavone according to claim 1, it is characterized in that described precipitant is that concentration expressed in percentage by volume is that ethanol water or the concentration expressed in percentage by volume of 90%-100% is the aqueous acetone solution of 90%-100%, the consumption of described precipitant is 1～5 times of concentrated solution volume.
4. the method for extracting polysaccharide and flavone from Gynura divaricata according to claim 1 is characterized in that the model of described resin column is: AB-8, D-101, D-140, DM-130, LSA-10, LSA-20 or HPD-600.
5. the method for extracting polysaccharide and flavone from Gynura divaricata according to claim 1 is characterized in that being separated into centrifugalize or isolated by filtration described in the described step (3).
6. the method for extracting polysaccharide and flavone from Gynura divaricata according to claim 1 is characterized in that described simmer down to vacuum concentration of described step (2) or membrance concentration.
7. the method for extracting polysaccharide and flavone from Gynura divaricata according to claim 1 is characterized in that dry described in described step (4) or the step (7) is lyophilization, vacuum drying or spray drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810118639 CN101336949B (en) | 2008-08-21 | 2008-08-21 | Method for extracting polysaccharide and flavone from Gynura divaricata |
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| CN102224803B (en) * | 2011-05-05 | 2012-07-11 | 山西菩净生物科技有限公司 | Artificial cultivation method of gynura divaricata (Linn.) DC. |
| CN104825517A (en) * | 2015-05-07 | 2015-08-12 | 李伟权 | Application of gynura divaricata in preparation of drugs for treating gouty arthritis |
| CN105017438B (en) * | 2015-07-13 | 2018-10-30 | 青岛海洋生物医药研究院股份有限公司 | A kind of Radix et Rhizoma Gynurae divaricatae polysaccharide and its application in preparing for immunological regulation and anti-tumor drug and functional food |
| CN104945532B (en) * | 2015-07-20 | 2017-09-05 | 山西省中医药研究院 | The preparation method of Gynura divaricata polysaccharide |
| CN106727824A (en) * | 2016-12-30 | 2017-05-31 | 天津市中升挑战生物科技有限公司 | The preparation method and application of chrysanthemum leaf Notogineng Extract and its compound preparation |
| CN107582589A (en) * | 2017-09-18 | 2018-01-16 | 漳州片仔癀药业股份有限公司 | A kind of purposes of the white phoenix dish extractive of general flavone and preparation method thereof with treating hyperuricemia |
| CN107582587A (en) * | 2017-09-18 | 2018-01-16 | 漳州片仔癀药业股份有限公司 | A kind of purposes of the white phoenix dish extractive of general flavone and preparation method thereof with treating NASH |
| CN109045075A (en) * | 2018-10-26 | 2018-12-21 | 陕西师范大学 | The preparation method of Matteuccia strthiopteris flavones and polysaccharide |
| CN110279873A (en) * | 2019-07-30 | 2019-09-27 | 广西中医药大学 | Research method of the Gynura divaricata to type II diabetes mouse inflammatory factor influencing mechanism |
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