CN104490956B - A kind of total seabuckthorn flavone purifying technique - Google Patents
A kind of total seabuckthorn flavone purifying technique Download PDFInfo
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- CN104490956B CN104490956B CN201410844325.8A CN201410844325A CN104490956B CN 104490956 B CN104490956 B CN 104490956B CN 201410844325 A CN201410844325 A CN 201410844325A CN 104490956 B CN104490956 B CN 104490956B
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- seabuckthorn flavone
- total seabuckthorn
- purifying technique
- vegetable oil
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- 235000003145 Hippophae rhamnoides Nutrition 0.000 title claims abstract description 24
- 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 24
- 229930003944 flavone Natural products 0.000 title claims abstract description 24
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 24
- 235000011949 flavones Nutrition 0.000 title claims abstract description 24
- 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 24
- 238000000034 method Methods 0.000 title claims abstract description 18
- 240000000950 Hippophae rhamnoides Species 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 64
- 241000229143 Hippophae Species 0.000 claims abstract description 35
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 15
- 239000008158 vegetable oil Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000003935 Hippophae Nutrition 0.000 claims abstract description 12
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 238000000746 purification Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 22
- 239000012071 phase Substances 0.000 description 8
- 239000003814 drug Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000004927 clay Substances 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 2
- 208000024172 Cardiovascular disease 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
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 208000026106 cerebrovascular disease Diseases 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000002526 effect on cardiovascular system Effects 0.000 description 2
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 2
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 2
- 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 2
- 235000005493 rutin Nutrition 0.000 description 2
- 229960004555 rutoside Drugs 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 208000001953 Hypotension Diseases 0.000 description 1
- GQODBWLKUWYOFX-UHFFFAOYSA-N Isorhamnetin Natural products C1=C(O)C(C)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 GQODBWLKUWYOFX-UHFFFAOYSA-N 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- 244000241838 Lycium barbarum Species 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
- 238000004458 analytical method Methods 0.000 description 1
- 230000000879 anti-atherosclerotic effect Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 208000021822 hypotensive Diseases 0.000 description 1
- 230000001077 hypotensive effect Effects 0.000 description 1
- 235000008800 isorhamnetin Nutrition 0.000 description 1
- IZQSVPBOUDKVDZ-UHFFFAOYSA-N isorhamnetin Chemical compound C1=C(O)C(OC)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 IZQSVPBOUDKVDZ-UHFFFAOYSA-N 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000013094 purity test Methods 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/55—Liquid-liquid separation; Phase separation
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- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
- Biotechnology (AREA)
- Botany (AREA)
- Medical Informatics (AREA)
- Medicinal Chemistry (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of total seabuckthorn flavone purifying technique, including step:Fructus hippophae is cleaned, drained and is clayed into power;Add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;By extract solution liquid separation, water alcohol phase is obtained;Water alcohol phase is dried into powder, the total seabuckthorn flavone as purified.The present invention purifying technique obtain total seabuckthorn flavone purity it is high, simple to operate, cost is cheap, be adapted to large-scale production.
Description
Technical field
The invention belongs to food and medicine manufacture field, is related to a kind of purifying technique of total seabuckthorn flavone.
Background technology
Hippophate flavone contains Quercetin, Isorhamnetin and Kaempferol isoreactivity composition.With hypotensive, reducing blood lipid, reduce
Blood viscosity, the enhancing function such as blood vessel elasticity, antiatherosclerosis is cardiovascular and cerebrovascular disease " jinx ".It is the elderly
The preferred health products of cardiovascular and cerebrovascular disease are prevented and treated, existing market demand is huge.The extraction process of present main flow is supercritical CO 2
Extraction method, cost high-purity are low.And now, traditional purifying technique is generally decocting method used by domestic pharmaceutical factory, and products therefrom is pure
Degree generally below 14%.
The content of the invention
In view of the drawbacks described above of prior art, the technical problems to be solved by the invention are by relatively simple purification
Technique and less expensive cost solve the problems, such as that the cost high-purity of current generally existing is low.
To achieve the above object, the invention provides a kind of total seabuckthorn flavone purifying technique, comprise the following steps:
1) fructus hippophae is cleaned, drained and clayed into power;
2) add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;
3) by extract solution liquid separation, water alcohol phase is obtained;
4) water alcohol phase is dried into powder, the total seabuckthorn flavone as purified.
Wherein, fructus hippophae described in step 1) is commercially available fructus hippophae.
The concentration that ethanol solution is added in step 2) is preferably 40%-70% ethanol, and the amount of addition is preferably every gram of sand
The ethanol solution of spine fruit addition 3-8 milliliters, most preferably 5 milliliters;The amount for adding vegetable oil is preferably that every gram of fructus hippophae adds 1-
1.5 milliliters of vegetable oil, most preferably 1.25 milliliters;The time of ultrasonic extraction is preferably 40-60 minutes.
The temperature of drying is preferably 40-60 DEG C in step 4).
The present invention detects the absorbance of sample using ELIASA using rutin as standard items, draws standard curve and calculates
Go out the purity of total seabuckthorn flavone in sample.Testing result shows the total seabuckthorn flavone for adding the combination of vegetable oil to extract with 60% ethanol
Purity reached 50% or so.The effect of wherein vegetable oil has two aspects:One side vegetable oil can be used in extraction sea-buckthorn
The flavonoid substance being dissolved in organic phase, reduce loss;Another aspect vegetable oil forms fluid-tight on the surface of water alcohol phase, super
The volatilization of water alcohol is prevented during sound, reduces loss.
Total seabuckthorn flavone purity that the purifying technique of the present invention obtains is high, simple to operate, cost is cheap, is adapted to extensive raw
Production;And the method for purification of the present invention is applicable not only to the purification of total seabuckthorn flavone, other water and ethanol but not of being dissolved in are applied also for
It is dissolved in the purification of the medicine of lipid solvent.
Therefore, the purifying technique of the further present invention is used to being dissolved in water and ethanol but the medicine insoluble in lipid solvent
Purification step is:
1) medicine is cleaned, drained and clayed into power;
2) add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;
3) by extract solution liquid separation, water alcohol phase is obtained;
4) water alcohol phase is dried into powder, the medicine as purified.
Embodiment
Embodiments of the invention are elaborated below:The present embodiment is carried out lower premised on technical solution of the present invention
Implement, give detailed embodiment and specific operating process, but protection scope of the present invention is not limited to following implementation
Example.
Embodiment 1
2g fructus hippophaes are weighed, cleans, drain and clay into power, add the ethanol solutions of 10ml 40% and 2.5ml vegetable oil,
Ultrasonic extraction 40min, extract solution is obtained after filtering.Liquid separation, water alcohol phase are evaporated, and it is the sea-buckthorn purified to obtain brown powder solid
General flavone.
Embodiment 2
2g fructus hippophaes are weighed, cleans, drain and clay into power, add the ethanol solutions of 10ml 60% and 2.5ml vegetable oil,
Ultrasonic extraction 40min, extract solution is obtained after filtering.Liquid separation, water alcohol phase are evaporated, and it is the sea-buckthorn purified to obtain brown powder solid
General flavone.
Embodiment 3
2g fructus hippophaes are weighed, cleans, drain and clay into power, add the ethanol solutions of 10ml 70% and 2.5ml vegetable oil,
Ultrasonic extraction 40min, extract solution is obtained after filtering.Liquid separation, water alcohol phase are evaporated, and it is the sea-buckthorn purified to obtain brown powder solid
General flavone.
Comparative example
With decocting method conventional in the market as a comparison, specific method is;2g fructus hippophaes are weighed, cleans, drain simultaneously
Clay into power, 1h is decocted in the ethanol solutions of 10ml 40%, filter, be evaporated to obtain powder.
Product purity determines
Using ELIASA, with glucose as a standard product measure absorbance, draw standard curve.From embodiment 1-3 and contrast
It is each in the total seabuckthorn flavone that example obtains to weigh 20mg samples, absorbance is measured, calculates the purity of total seabuckthorn flavone in sample.Its
Step is:Sampling, is 10mL with absolute ethyl alcohol constant volume;1mL constant volume solution is taken, adds 1mL 1% alchlor ethanol solution,
Again 10mL is settled to absolute ethyl alcohol;Stand 10 minutes;With the absorbance at ELIASA detection 430nm.
In order to judge the validity of detection means and sensitivity, we employ standard items rutin and tested first.Mark
Quasi- product be purity close to 100% sterling.We are equipped with the standard items under different diluted concentrations, and use our test hand
Duan Jinhang is identified.Analyze test result to show, our detection method, can effectively identify the various concentrations of standard items.
The standard items curve of acquisition is Y=0.4419X+0.0379, R2=0.9984 (X is sample purity, and Y is spectrophotometric value).From
On standard items curve, it is more that we may determine that the detection method that we use can efficiently and accurately detect target substance matrimony vine
The content of sugar.
Product purity testing result is as shown in the table:
Sample | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
Spectrophotometric value | 0.173 | 0.257 | 0.208 | 0.095 |
Purity | 30.6% | 49.6% | 38.5% | 12.9% |
Preferred embodiment of the invention described in detail above.It should be appreciated that one of ordinary skill in the art without
Creative work can is needed to make many modifications and variations according to the design of the present invention.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical scheme, all should be in the protection domain being defined in the patent claims.
Claims (4)
1. a kind of total seabuckthorn flavone purifying technique, it is characterised in that comprise the following steps:
1) fructus hippophae is cleaned, drained and clayed into power;
2) add ethanol solution and vegetable oil, ultrasonic extraction for a period of time, obtain extract solution after filtering;
3) by extract solution liquid separation, water alcohol phase is obtained;
4) water alcohol phase is dried into powder, the total seabuckthorn flavone as purified, wherein,
It is 40%-70% that ethanol solution concentration is added in step 2), and the amount of the ethanol solution of addition adds 3-8 for every gram of fructus hippophae
The ethanol solution of milliliter,
The amount that vegetable oil is added in step 2) adds 1-1.5 milliliter vegetable oil for each gram of fructus hippophae.
2. total seabuckthorn flavone purifying technique according to claim 1, it is characterised in that the time of ultrasonic extraction in step 2)
For 40-60 minutes.
3. total seabuckthorn flavone purifying technique according to claim 1, it is characterised in that the temperature of drying is in step 4)
40-60℃。
4. the total seabuckthorn flavone of the total seabuckthorn flavone purifying technique purification according to claim any one of 1-3.
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Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1451658A (en) * | 2003-05-20 | 2003-10-29 | 傅建熙 | Method for extracting seabuckthorn fruit total flavonoids by three-solvent system |
CN102308987A (en) * | 2011-06-27 | 2012-01-11 | 新疆科宇科技有限公司 | Production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaf |
-
2014
- 2014-12-25 CN CN201410844325.8A patent/CN104490956B/en not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1451658A (en) * | 2003-05-20 | 2003-10-29 | 傅建熙 | Method for extracting seabuckthorn fruit total flavonoids by three-solvent system |
CN102308987A (en) * | 2011-06-27 | 2012-01-11 | 新疆科宇科技有限公司 | Production method for extracting glucoside type seabuckthorn flavones from sea-buckthorn leaf |
Non-Patent Citations (1)
Title |
---|
微波辅助提取沙棘总黄酮的工艺研究;冯纪南等;《安徽农业科学》;20111231(第26期);15952-15954 * |
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