CN103623034B - The preparation method of Daxing'an Mountainrange wild euphorbia helioscopia general flavone - Google Patents
The preparation method of Daxing'an Mountainrange wild euphorbia helioscopia general flavone Download PDFInfo
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- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 48
- 229930003944 flavone Natural products 0.000 title claims abstract description 48
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 48
- 235000011949 flavones Nutrition 0.000 title claims abstract description 48
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 235000012043 Euphorbia helioscopia Nutrition 0.000 title abstract description 4
- 238000002360 preparation method Methods 0.000 title abstract description 3
- 241001553772 Euphorbia radians Species 0.000 title 1
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 26
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 238000001179 sorption measurement Methods 0.000 claims abstract description 21
- 239000004952 Polyamide Substances 0.000 claims abstract description 20
- 229920002647 polyamide Polymers 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000002608 ionic liquid Substances 0.000 claims abstract description 12
- 239000000284 extract Substances 0.000 claims abstract description 11
- 238000010262 high-speed countercurrent chromatography Methods 0.000 claims abstract description 11
- 230000002411 adverse Effects 0.000 claims abstract description 8
- 238000000746 purification Methods 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- 239000000243 solution Substances 0.000 claims description 23
- 238000010828 elution Methods 0.000 claims description 20
- 239000012488 sample solution Substances 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 13
- 238000011068 loading method Methods 0.000 claims description 11
- -1 poly tetrafluoroethylene Polymers 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 241001233914 Chelidonium majus Species 0.000 claims description 10
- 239000003480 eluent Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000004128 high performance liquid chromatography Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 230000005526 G1 to G0 transition Effects 0.000 claims description 5
- 230000009514 concussion Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000003795 desorption Methods 0.000 claims description 5
- 238000001514 detection method Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229940058401 polytetrafluoroethylene Drugs 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- AOZUYISQWWJMJC-UHFFFAOYSA-N acetic acid;methanol;hydrate Chemical compound O.OC.CC(O)=O AOZUYISQWWJMJC-UHFFFAOYSA-N 0.000 claims description 2
- LSQLKWFLOZNABG-UHFFFAOYSA-N butan-1-ol chloroform methanol hydrate Chemical compound O.OC.ClC(Cl)Cl.CCCCO LSQLKWFLOZNABG-UHFFFAOYSA-N 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 claims 1
- 238000004821 distillation Methods 0.000 claims 1
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims 1
- 240000002853 Nelumbo nucifera Species 0.000 abstract description 8
- 235000006508 Nelumbo nucifera Nutrition 0.000 abstract description 8
- 244000192024 Euphorbia helioscopia Species 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 239000004480 active ingredient Substances 0.000 abstract 2
- 229930013930 alkaloid Natural products 0.000 abstract 2
- 150000003797 alkaloid derivatives Chemical class 0.000 abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000000859 sublimation Methods 0.000 description 3
- 230000008022 sublimation Effects 0.000 description 3
- 206010030113 Oedema Diseases 0.000 description 2
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 2
- 229930182478 glucoside Natural products 0.000 description 2
- 150000008131 glucosides Chemical class 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- OIWSIWZBQPTDKI-UHFFFAOYSA-N 1-butyl-3-methyl-2h-imidazole;hydrobromide Chemical compound [Br-].CCCC[NH+]1CN(C)C=C1 OIWSIWZBQPTDKI-UHFFFAOYSA-N 0.000 description 1
- 206010003445 Ascites Diseases 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 206010036790 Productive cough Diseases 0.000 description 1
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 1
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 208000002474 Tinea Diseases 0.000 description 1
- 241000130764 Tinea Species 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000001939 inductive effect Effects 0.000 description 1
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 208000008128 pulmonary tuberculosis Diseases 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000003813 thin hair Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
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- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to field of natural organic chemistry, it is related to the new method that general flavone is extracted in a kind of wild euphorbia helioscopia from Daxing'an Mountainrange, it is more particularly to a kind of to be extracted by the use of super-pressure (ionic liquid is used as solvent), polyamide lotus root joins macroporous resin adsorption, and high speed adverse current chromatogram isolates and purifies the new method of general flavone.Advantage of the present invention：1st, ionic liquid is combined with super-pressure, with the advantage extracted faster, more efficient.And technique is simple and easy to do, fully, alkaloid is high for extracts active ingredients.2nd, polyamide lotus root connection macroporous resin adsorption purification technique, total alkaloid can be enriched with well, active ingredient is further purified.Resin is disposable, separating rate is fast, expense is low, can be industrially used.3rd, flexible, efficient, separating rate is fast, preparation amount is big, the low advantage of expense with operating for high-speed countercurrent chromatography, and can be industrially used.The present invention is high using general flavone content obtained by above-mentioned technology, high purity 98.3%.
Description
Technical field
The invention belongs to field of natural organic chemistry, it is related in a kind of wild euphorbia helioscopia from Daxing'an Mountainrange and extracts the new of general flavone
Method, more particularly to one kind utilize super-pressure（Ionic liquid is used as solvent）Extract, polyamide lotus root connection macroporous resin adsorption is high
Fast adverse current chromatogram isolates and purifies the new method of general flavone.
Background technology
Wartwort, alias WUDUOYUN, tendencies grass, annual or biennial herb.High 10~30cm, it is hairless or only branch is somewhat
Thin hair, base portion aubergine, top light green.Leaf alternate；Obovate or cochlear, long 1~3cm, wide 0.7~1cm, tip nick,
More than marginal center there are serration, stockless.Capsule is spherical, diameter about 3mm, and 3 split, smooth.Seed brown, it is avette, 2mm is about,
There are substantially raised reticulate pattern, the semicircle strophiole of tool white.Contain flavone compound Quercetin -3,5- digalactosyl glucoside, wartwort soap
Glucoside, helioscopiol.Wartwort is pungent, bitter, be slightly cold, poisonous；There are inducing diuresis to remove edema, reducing phlegm and resolving masses, removing toxic substances desinsection.The traditional Chinese medical science and clinic are often
With its treat ascites, oedema, pulmonary tuberculosis, abundant expectoration breath with cough, tinea sore etc..
Domestic typically to extract general flavone with organic solvent extraction, conventional has ultrasonic wave extraction, and methanol, alcohol solvent are carried
Follow the example of.Also have in recent years and general flavone, the report purified with macroreticular resin are extracted using Microwave-assisted ionic liquid method.Tradition
Method, which extracts general flavone, needs a few houres to ten a few houres, and operation temperature is high and yield is low, and energy consumption is big.
Present invention be distinguished in that mainly using superhigh pressure technique（Ionic liquid is used as solvent）Extract, polyamide lotus root
Join macroporous resin adsorption, then isolated and purified with high speed adverse current chromatogram.The general flavone extracted by above technology, purified has stronger
Oxidation resistance, not only yield is high for product, and purity is high.Detected using HPLC methods, content reaches as high as 98.3 %.
The content of the invention
Advantage of the present invention：Extract quick, product purity high, substantially increase extraction rate, at the same be greatly improved effectively into
Divide content, overcome the shortcoming that traditional extraction extract purity is low, yield is low.
To achieve the above object, the technical solution adopted by the present invention is：
One kind uses ultra high pressure extraction technology（Ionic liquid is used as solvent）, polyamide lotus root connection macroporous resin adsorption, then use
High speed adverse current chromatogram is isolated and purified, and obtains the new method of high-purity general flavone, and its step is as follows：
（1）Ultra high pressure extraction：Wartwort herb cut off, using various concentrations ionic liquid solution as solvent, certain solid-liquid ratio,
A few minutes are handled under appropriate hyperpressure；
（2）Refined filtration processing：Using poly tetrafluoroethylene, 0.1 μm of filtering accuracy, under certain temperature and pressure at refined filtration
Reason；
（3）Polyamide is adsorbed and eluted：
Using the polyamide powder of certain mesh number, sample solution concentration is controlled, sample solution volume is inhaled with certain flow rate at room temperature
Attached saturation；First removal of impurities during desorption, then desorbed with certain density ethanol solution, coutroi velocity collects eluent, detects general flavone
Content；
（4）Macroreticular resin second adsorption and elution：
From the macroreticular resin of different model（XAD-16、DM130、D312）, control sample solution mass concentration, loading speed
Rate；First with 2 BV deionized water rinsing resins, then with the ethanol solution of various concentrations, eluted with certain flow rate, collect eluent,
Detect general flavone content；
（5）Vacuum freeze drying：General flavone solution is collected, is freeze-dried under proper temperature, drying pressure；
（6）Split-phase：Extractive of general flavone is weighed, HSCCC solvent systems are selected, various solvents are added into a point liquid leakage in proportion
In bucket, concussion is sufficiently mixed solution, stands overnight.Upper and lower phase is separated after split-phase balance；
（7）HSCCC is isolated and purified：Using the upper as stationary phase of solvent system, lower phase is mobile phase, rotating speed is adjusted, with one
Constant current speed is pumped into mobile phase, separates extractive of general flavone；
（8）Detect：Using high performance liquid chromatography, UV-detector is detected in certain wavelength, and wartwort general flavone is pure
Spend for more than 95%.
Embodiment：
Case study on implementation 1：
One kind uses ultra high pressure extraction technology（Ionic liquid is used as solvent）, polyamide lotus root connection macroporous resin adsorption, then use
High speed adverse current chromatogram is isolated and purified, and obtains the new method of high-purity general flavone, and its step is as follows：
（1）Ultra high pressure extraction：1kg wartwort herb is cut off, with the 1- octyl group -3- methyl imidazolium tetrafluoroborates of 50% concentration
Solution is solvent, solid-liquid ratio 1:2min is handled under 8,200-400 MPA pressure；
（2）Refined filtration processing：Extract solution is collected, using poly tetrafluoroethylene, 0.1 μm of filtering accuracy, in 60 DEG C, 0.2MPa
Refined filtration is handled under pressure；
（3）Polyamide is adsorbed and eluted：
Using the polyamide powder of 80 mesh, sample solution concentration is controlled in 0.5 mg/mL, sample solution volume 2BV, at room temperature
With 2BV/h flow velocity adsorption saturations；2BV water removal of impurities is first used during desorption, then is desorbed with 75% ethanol, elution volume is 4BV, flow velocity
2BV/h, collects eluent.After measured, general flavone purity is 72.36%；
（4）Macroreticular resin second adsorption and elution：
Then purified with DM130 macroreticular resin second adsorptions, sample solution mass concentration be 3mg/ml, loading speed 2BV/h,
The BV/h of loading volume 4；First with 2 BV deionized water rinsing resins during elution, then with the ethanol solution of 80% concentration, flowed with 1BV/h
Speed elution, elution volume is 5 BV；Eluent is collected, after measured, general flavone purity is 81.29%,；
（5）Vacuum freeze drying：General flavone solution is collected, in -15 DEG C of pre-freezing temperature, operating pressure 20Pa, sublimation temperature
55 DEG C, it is freeze-dried at 60 DEG C of resolution temperature；
（6）Split-phase：The mg of extractive of general flavone 300 is weighed, using acetate-methanol-water (4：1：3) HSCCC solvents system
System, in proportion adds various solvents in separatory funnel, and concussion is sufficiently mixed solution, stands overnight.Separated after split-phase balance
Upper and lower phase；
（7）HSCCC is isolated and purified：Using the upper as stationary phase of solvent system, lower phase is mobile phase, adjustment rotating speed 700 r/
Min, mobile phase is entered with 2.0 mL/min flow pumps, separates extractive of general flavone；
（8）Detection：Using high performance liquid chromatography, UV-detector is detected, general flavone purity is 97.7%.
Case study on implementation 2：
One kind uses ultra high pressure extraction technology（Ionic liquid is used as solvent）, polyamide lotus root connection macroporous resin adsorption, then use
High speed adverse current chromatogram is isolated and purified, and obtains the new method of high-purity general flavone, and its step is as follows：
（1）Ultra high pressure extraction：2kg wartwort herb cut off, using the 1- butyl -3- methylimidazole bromide solution of 60% concentration as
Solvent, solid-liquid ratio 1:3min is handled under 10,300 MPA pressure；
（2）Refined filtration processing：Extract solution is collected, using poly tetrafluoroethylene, 0.1 μm of filtering accuracy, in 65 DEG C, 0.3MPa
Refined filtration is handled under pressure；
（3）Polyamide is adsorbed and eluted：
Using the polyamide powder of 100 mesh, sample solution concentration is controlled in 1.5 mg/mL, sample solution volume 3BV, at room temperature
With 3BV/h flow velocity adsorption saturations；3BV water removal of impurities is first used during desorption, then is desorbed with 80% ethanol, elution volume is 5BV, flow velocity
3BV/h, collects eluent.After measured, general flavone purity is 73.65%；
（4）Macroreticular resin second adsorption and elution：
Then purified with D312 macroreticular resin second adsorptions, sample solution mass concentration be 4mg/ml, loading speed 3BV/h,
The BV/h of loading volume 5；First with 3 BV deionized water rinsing resins during elution, then with the ethanol solution of 90% concentration, flowed with 2BV/h
Speed elution, elution volume is 6BV, collects eluent, after measured, and general flavone purity is 80.17%,；
（5）Vacuum freeze drying：General flavone solution is collected, in -20 DEG C of pre-freezing temperature, operating pressure 25Pa, sublimation temperature
50 DEG C, it is freeze-dried at 65 DEG C of resolution temperature；
（6）Split-phase：The mg of extractive of general flavone 200 is weighed, using n-hexane-ethyl acetate-alcohol-water (5：:3：2：4)
HSCCC solvent systems, in proportion add various solvents in separatory funnel, and concussion is sufficiently mixed solution, stands overnight.Split-phase
Upper and lower phase is separated after balance；
（7）HSCCC is isolated and purified：Using the upper as stationary phase of solvent system, lower phase is mobile phase, adjustment rotating speed 800 r/
Min, mobile phase is entered with 3.0 mL/min flow pumps, separates extractive of general flavone；
（8）Detection：Using high performance liquid chromatography, UV-detector is detected, general flavone purity is 97.1%.
Case study on implementation 3：
One kind uses ultra high pressure extraction technology（Ionic liquid is used as solvent）, polyamide lotus root connection macroporous resin adsorption, then use
High speed adverse current chromatogram is isolated and purified, and obtains the new method of high-purity general flavone, and its step is as follows：
（1）Ultra high pressure extraction：5kg wartwort herb is cut off, molten with the 1- ethoxy -3- methyl hexafluorophosphates of 70% concentration
Liquid is solvent, solid-liquid ratio 1:2min is handled under 12,400 MPA pressure；
（2）Refined filtration processing：Extract solution is collected, using poly tetrafluoroethylene, 0.1 μm of filtering accuracy, in 60 DEG C, 0.4MPa
Refined filtration is handled under pressure；
（3）Polyamide is adsorbed and eluted：
Using the polyamide powder of 200 mesh, sample solution concentration is controlled in 1.0 mg/mL, sample solution volume 2BV, at room temperature
With 4BV/h flow velocity adsorption saturations；4BV water removal of impurities is first used during desorption, then is desorbed with 85% ethanol, elution volume is 6BV, flow velocity
3BV/h, collects eluent.After measured, general flavone purity is 74.4%；
（4）Macroreticular resin second adsorption and elution：
Then purified with D101 macroreticular resin second adsorptions, sample solution mass concentration is 4.5mg/ml, loading speed 4BV/
h；The BV/h of loading volume 6；First with 2 BV deionized water rinsing resins during elution, then with the ethanol solution of 85% concentration, with 1BV/h
Flow velocity is eluted, the BV of elution volume 7, collects eluent, after measured, and general flavone purity is 82.93%,；
（5）Vacuum freeze drying：General flavone solution is collected, in -25 DEG C of pre-freezing temperature, operating pressure 30Pa, sublimation temperature
50 DEG C, it is freeze-dried at 60 DEG C of resolution temperature；
（6）Split-phase：The mg of extractive of general flavone 200 is weighed, using chloroform-methanol-butanol-water (4：3：2：1) HSCCC is molten
Agent system, in proportion adds various solvents in separatory funnel, and concussion is sufficiently mixed solution, stands overnight.After split-phase balance
Separate upper and lower phase；
（7）HSCCC is isolated and purified：Using the upper as stationary phase of solvent system, lower phase is mobile phase, adjustment rotating speed 850 r/
Min, mobile phase is entered with 2.0 mL/min flow pumps, separates extractive of general flavone；
（8）Detection：Using high performance liquid chromatography, UV-detector is detected, general flavone purity is 98.3%.
Claims (1)
1. one kind uses ultra high pressure extraction technology, polyamide combination macroporous resin adsorption, then is isolated and purified with high speed adverse current chromatogram,
The method for obtaining high-purity general flavone, its step is as follows：
（1）Ultra high pressure extraction：Wartwort herb is cut off, using various concentrations ionic liquid solution as solvent, in certain solid-liquid ratio, suitably
A few minutes are handled under hyperpressure；
（2）Refined filtration processing：Using poly tetrafluoroethylene, 0.1 μm of filtering accuracy, refined filtration is handled under certain temperature and pressure；
（3）Polyamide is adsorbed and eluted：
Using the polyamide powder of certain mesh number, sample solution concentration is controlled, sample solution volume is full with certain flow rate absorption at room temperature
With；First removal of impurities during desorption, then desorbed with certain density ethanol solution, coutroi velocity, eluent is collected, detection general flavone contains
Amount；
（4）Macroreticular resin second adsorption and elution：
From the macroreticular resin of different model, sample solution mass concentration, loading speed are controlled；First with 2 BV deionized water rinsing trees
Fat, then with the ethanol solution of various concentrations, eluted with certain flow rate, eluent is collected, general flavone content is detected；
（5）Vacuum freeze drying：General flavone solution is collected, is freeze-dried under proper temperature, drying pressure；
（6）Split-phase：Extractive of general flavone is weighed, HSCCC solvent systems are selected, various solvents are added into separatory funnel in proportion
In, concussion is sufficiently mixed solution, stands overnight, and upper and lower phase is separated after split-phase balance；
（7）HSCCC is purified：Using the upper as stationary phase of solvent system, lower phase is mobile phase, rotating speed is adjusted, with certain flow rate pump
Enter mobile phase, purification of flavone extract；
（8）Detection：Using high performance liquid chromatography, UV-detector is detected in certain wavelength, and wartwort general flavone purity is
More than 95%；
Wherein, in described step（1）In, ionic liquid is 1- octyl group -3- methyl imidazolium tetrafluoroborates, 1- butyl -3- first
Any one in base imidazoles bromide, 1- ethoxy -3- methyl hexafluorophosphates, volumetric concentration is 50-70%；
In described step（3）In, polyamide is 80-200 mesh, and sample solution concentration is controlled in 0.5-1.5 mg/mL, loading
Liquid accumulates 2-3BV, at room temperature with 2-4BV/h flow velocity adsorption saturations；Removal of impurities water 2-4BV during parsing, ethanol parsing concentration is 75-
85%, elution volume 4-6 BV, flow velocity 2-4BV/h；
In described step（4）In, macroreticular resin is any one in D312, DM130, D101；Sample solution mass concentration is
3-4.5mg/ml, loading speed 2-4BV/h, loading volume 4-6 BV/h；Ethanol solution concentration is 80-90%, elution stream during elution
Speed is 1-3BV/h, and elution volume is 5-7 BV；
In described step（5）In, general flavone solution pre-freezing temperature is -15 DEG C to -25 DEG C, operating pressure 20-30Pa, distillation temperature
50-55 DEG C of degree, 60-65 DEG C of resolution temperature；
In described step（6）In, solvent is that ratio is 4：1：3 acetate-methanol-water, ratio are 5：:3：2：4 just
Hexane-ethyl acetate-alcohol-water, ratio are 4：3：2：Any one in 1 chloroform-methanol-butanol-water；
In described step（7）In, rotating speed 700-850 r/min, flow velocity is 2.0-3.0 mL/min.
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| CN104825586A (en) * | 2014-07-17 | 2015-08-12 | 兰州大学 | Method of extracting flavones from waste liquid after extraction of rose essential oil |
| CN104587014B (en) * | 2014-12-29 | 2017-04-19 | 杭州师范大学 | Method for extracting flavonoid active ingredient from traditional Chinese medicine fructus aurantii |
| CN106568850A (en) * | 2015-10-10 | 2017-04-19 | 勐海茶业有限责任公司 | Method for determining flavone components in tea leaf by using HPLC |
| CN105639653A (en) * | 2015-12-23 | 2016-06-08 | 华南农业大学 | oil-tea camellia flower granule with antioxidant activity and preparation method and application thereof |
| CN110283050A (en) * | 2019-07-01 | 2019-09-27 | 大兴安岭林格贝寒带生物科技股份有限公司 | Utilize the method for superhigh pressure technique enriching and purifying cannabidiol |
| CN111729003A (en) * | 2020-07-31 | 2020-10-02 | 黄大帅 | Traditional Chinese medicine preparation for treating postpartum wind |
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| CN103040902A (en) * | 2012-12-13 | 2013-04-17 | 大兴安岭林格贝有机食品有限责任公司 | Novel method for purifying wild codonopsis pilosula saponin |
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