CN103396463A - Method for extracting icariin from epimedium - Google Patents
Method for extracting icariin from epimedium Download PDFInfo
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- CN103396463A CN103396463A CN2013103671427A CN201310367142A CN103396463A CN 103396463 A CN103396463 A CN 103396463A CN 2013103671427 A CN2013103671427 A CN 2013103671427A CN 201310367142 A CN201310367142 A CN 201310367142A CN 103396463 A CN103396463 A CN 103396463A
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- TZJALUIVHRYQQB-UHFFFAOYSA-N icariine Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(O)C(O)C(C)O2)O)C(=O)C2=C(O)C=C(OC3C(C(O)C(O)C(CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 24
- 241000893536 Epimedium Species 0.000 title abstract description 7
- TZJALUIVHRYQQB-XFDQAQKOSA-N Icariin Natural products O(C)c1ccc(C2=C(O[C@H]3[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O3)C(=O)c3c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O4)c(C/C=C(\C)/C)c3O2)cc1 TZJALUIVHRYQQB-XFDQAQKOSA-N 0.000 title abstract description 6
- 235000018905 epimedium Nutrition 0.000 title abstract description 6
- TZJALUIVHRYQQB-XLRXWWTNSA-N icariin Chemical compound C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O)[C@@H](O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O3)O)C(CC=C(C)C)=C2O1 TZJALUIVHRYQQB-XLRXWWTNSA-N 0.000 title abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000004587 chromatography analysis Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 239000012535 impurity Substances 0.000 claims abstract description 7
- 238000001694 spray drying Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 150000001408 amides Chemical class 0.000 claims description 15
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- 230000001488 breeding effect Effects 0.000 claims description 6
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- 239000000284 extract Substances 0.000 claims description 5
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- 239000007787 solid Substances 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 9
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- 238000000746 purification Methods 0.000 abstract description 7
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- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- ZRGOVKQDBSFQIU-RDYCXQFPSA-N C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](COC(C)=O)O3)O)[C@@H](OC(C)=O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O)C(CC=C(C)C)=C2O1 Chemical compound C1=CC(OC)=CC=C1C1=C(O[C@H]2[C@@H]([C@H](O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](COC(C)=O)O3)O)[C@@H](OC(C)=O)[C@H](C)O2)O)C(=O)C2=C(O)C=C(O)C(CC=C(C)C)=C2O1 ZRGOVKQDBSFQIU-RDYCXQFPSA-N 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
- 238000005516 engineering process Methods 0.000 description 2
- 229930187783 epimedoside Natural products 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- -1 flavonoid compound Chemical class 0.000 description 2
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- ZRGOVKQDBSFQIU-UHFFFAOYSA-N korepimedoside A Natural products C1=CC(OC)=CC=C1C1=C(OC2C(C(OC3C(C(O)C(O)C(COC(C)=O)O3)O)C(OC(C)=O)C(C)O2)O)C(=O)C2=C(O)C=C(O)C(CC=C(C)C)=C2O1 ZRGOVKQDBSFQIU-UHFFFAOYSA-N 0.000 description 2
- 239000013558 reference substance Substances 0.000 description 2
- 241001362421 Epimedium brevicornu Species 0.000 description 1
- 241000893531 Epimedium koreanum Species 0.000 description 1
- 241001660849 Epimedium pubescens Species 0.000 description 1
- 241001362411 Epimedium sagittatum Species 0.000 description 1
- IYCPMVXIUPYNHI-UHFFFAOYSA-N Icariside I Natural products C1=CC(OC)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(OC3C(C(O)C(O)C(CO)O3)O)C(CC=C(C)C)=C2O1 IYCPMVXIUPYNHI-UHFFFAOYSA-N 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
- 201000001880 Sexual dysfunction Diseases 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
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- 230000003712 anti-aging effect Effects 0.000 description 1
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- 238000010812 external standard method Methods 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 229930182721 icariside Natural products 0.000 description 1
- 230000001900 immune 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
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 229960001285 quercetin Drugs 0.000 description 1
- 235000005875 quercetin Nutrition 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A disclosed method for extracting icariin from epimedium comprises the following steps: taking an aqueous solution of ethanol as an extraction solvent, under the condition of microwave heating, extracting from stems and leaves of epimedium to obtain an extraction liquor A; performing vacuum condensation to obtain a concentrate B; removing particle impurities via a millipore filtration film to obtain a filtrate C; performing separation purification by simulated moving bed chromatography to obtain a component D rich in icariin; and concentrating the component D, and employing a spray drying method to obtain a finished product with an icariin content of 90% or more. The method is simple in technological steps, simple in operation, substantially shortened in production time and improved in production efficiency, and has a wider application prospect in practical production.
Description
Technical field
The present invention relates to a kind of from Herba Epimedii, extracting the method for icarin.
Background technology
The dry cauline leaf of Epimedium Berberidaceae plant Epimedium brevicornum (Epimedium brevicomum Maxim), arrow leaf Herba Epimedii (Epimedium sagittatum Maxim), pubescence Herba Epimedii (Epimedium pubescens Maxim) or Herba Epimedii (Epimedium koreanum Nakai).Herba Epimedii mainly contains and mainly contains flavonoid compound, lignanoid, alkaloid, volatilization wet goods, and wherein flavonoid mainly comprises icarin (icariin), icariside (icarisoside) etc.; Herba Epimedii contains icarin, epimedoside (epimedoside) A, B, C, D, E etc.; Arrow leaf Herba Epimedii contains icarin, dehydration epimedium aglucone-3-O-α-rhamnoside, epimedium aglucone-3-O-α-rhamnoside, Quercetin etc.Icarin is mainly used in improving cardio-cerebrovascular function, enhancing body immunological competence, promotion DNA is synthetic and prevention and the treatment of sexual dysfunction etc., and icarin also has anti-ageing and antitumor action.
At present, the icarin extracting method mainly contains water extract-alcohol precipitation, alcohol extracting-water precipitating, Enzymatic Extraction, ultrasonic extraction, microwave and helps and carry etc., and purification process has flocculation agent method of purification, macroporous resin united purification method, silica gel column chromatography method of purification, polymeric amide chromatography method of purification etc.But there is following problem in the product of existing explained hereafter: product content generally on the low side, the products production cost is higher, the poisonous Determination of Residual Organic Solvents of product is higher, purification step is tediously long, the production cycle is long, the production technique environmental pollution is more serious.
The simulated moving bed chromatography technology is that simulation moving-bed design philosophy is introduced in liquid phantom preparing chromatogram, both kept the consumption of liquid phantom preparing chromatogram little, separation purity is high, and the advantage such as temperature-changeable operation, overcome again the shortcoming that common liquid phantom preparing chromatogram can not operate continuously, make it have separating power strong, equipment volume is little, and cost of investment is low, and is particularly conducive to the characteristics such as system of separating the high and difficult separation of thermo-sensitivity.
Summary of the invention
The present invention aims to provide a kind of method from separating-purifying icarin Herba Epimedii.
Technical scheme of the present invention is:
A kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that comprising the following steps:
(1) using aqueous ethanolic solution as extracting solvent, under the condition of microwave heating, extract dry Herba Epimedii cauline leaf, obtain Herba Epimedii extracting solution A;
(2) extracting solution A is carried out to vacuum concentration and obtain concentrated solution B;
(3) concentrated solution B is removed to granulometric impurity through millipore filtration, obtain liquor C;
(4) liquor C is carried out to separating-purifying through simulated moving bed chromatography, obtain being rich in the component D of icarin, by the concentrated concentrated solution E that obtains of component D;
(5) the concentrated solution E that arrives in step (4) is spray-dried, obtain containing the finished product of 90% above icarin.
In step of the present invention (1), volume fraction of ethanol is 50%～70%, and the mass ratio that extracts etoh solvent and Herba Epimedii raw material is 9～12: 1, microwave power 700～900W, 40～60 ℃ of temperature, time 8～12min.
In step of the present invention (3), in liquor C, the total solid amount is 40～50g/L, and icarin concentration is 4～5g/L.
In step of the present invention (4), the sorbent material that simulated moving bed chromatography is filled is polymeric amide; Strippant is 50% ethanolic soln, and its consumption is 2～3 times of polymeric amide volume; Water wash zone is purified water; The polymeric amide regenerated solvent is 95% ethanol or 5% aqueous sodium hydroxide solution; Adsorption zone flow velocity 1～2BV/h; Desorption zone flow velocity 2～3BV/h; Water wash zone flow velocity 2～3BV/h; Breeding blanket flow velocity 2～3BV/h; Be 600～850s switching time; Temperature is 30～60 ℃; Pressure-controlling is at 0.2MPa～0.6MPa.
In step of the present invention (5), the centrifugal spray drying parameter is: 100～140 ℃ of inlet temperature, 30～60 ℃ of air outlet temperatures, charging mass percent concentration are 30wt.%.
Further, the ethanolic soln of the extraction solvent preferred 50%～60% in described step (1);
Further, the mass ratio preferred 10～12: 1 of the extraction solvent in described step (1) and raw material;
Further, the preferred 800～900W of microwave power in described step (1);
Further, the microwave heating temperature in described step (1) is preferred 50 ℃;
Further, preferred 10min heat-up time in described step (1).
Further, in described step (3), preferred use aperture is the millipore filtration of 0.45 μ m.
Present method processing step is simple, and is easy and simple to handle, greatly shortens the production spent time, improved production efficiency, and stronger application prospect is arranged in actual production.With the icarin that technical scheme of the present invention obtains, purity is more than 90%, and total recovery reaches more than 70%.
The accompanying drawing explanation
Fig. 1 is the HPLC spectrogram of icarin standard substance
Fig. 2 is the HPLC spectrogram of extracting solution A in embodiment 1
Fig. 3 is the HPLC spectrogram of embodiment 1 finished product
Embodiment
Below in conjunction with following embodiment, the present invention is done to explanation in more detail.
The Microwave Extraction Apparatus model: Jiang Suhui grinds MC8S-1A, and microwave power 0～1000W is adjustable, and 0～300 ℃ of temperature is adjustable.Embodiment 1
Take the dry Folium Epimedii of 10kg, pulverizing is 60 order ends, and as extraction agent, material ratio [m (ethanol): m (Herba Epimedii is pulverized dry cauline leaf)] ratio is 10: 1 with 60% aqueous ethanolic solution, be placed in Microwave Extraction Apparatus, with 800W power, temperature 50 C, carry out microwave extraction 10min.To 30L, the concentrated solution B of gained crosses the millipore filtration removal of impurities of 0.45 μ m, obtains liquor C by the extracting solution A vacuum concentration that obtains.Liquor C enters the mobile bed that separates, and sorbent material is polymeric amide, and strippant is 50% ethanolic soln, and its consumption is 3 times of polymeric amide volume; Water wash zone is purified water; Regenerated solvent is 5% sodium hydroxide; Adsorption zone flow velocity 2BV/h; Desorption zone flow velocity 3BV/h; Water wash zone flow velocity 3BV/h; Breeding blanket flow velocity 3BV/h; Be 750s switching time; Temperature is controlled at 50 ℃; Pressure-controlling is at 0.5MPa, collects the component D that is rich in icarin, and it is 90.7% icarin pale yellow powder 108.2g that concentration and recovery ethanol obtains purity by spraying drying, and product recovery rate is 73.8%.Spray-dired parameter is: 140 ℃ of inlet temperature, 30 ℃ of air outlet temperatures, charging mass percent concentration 30wt.%.
Embodiment 2
Take the dry Folium Epimedii of 10kg, pulverized 60 mesh sieves, as extraction agent, material ratio [m (ethanol): m (Herba Epimedii is pulverized dry cauline leaf)] ratio is 12: 1 with 50% aqueous ethanolic solution, be placed in Microwave Extraction Apparatus, with 800W power, temperature 60 C, carry out microwave extraction 10min.To 30L, the concentrated solution B of gained crosses the millipore filtration removal of impurities of 0.45 μ m, obtains liquor C by the extracting solution A vacuum concentration that obtains.Liquor C enters the mobile bed that separates, and sorbent material is polymeric amide, and strippant is 50% ethanolic soln, and its consumption is 3 times of polymeric amide volume; Water wash zone is purified water; Regenerated solvent is 5%NaOH; Adsorption zone flow velocity 2BV/h; Desorption zone flow velocity 3BV/h; Water wash zone flow velocity 3BV/h; Breeding blanket flow velocity 3BV/h; Be 750s switching time; Temperature is controlled at 50 ℃; Pressure-controlling is at 0.5MPa, collects the component D that is rich in icarin, and it is 91.2% icarin pale yellow powder 109.0g that concentration and recovery ethanol obtains purity by spraying drying, and product recovery rate is 74.7%.Spray-dired parameter is: 140 ℃ of inlet temperature, 30 ℃ of air outlet temperatures, charging mass percent concentration 30wt.%.
Embodiment 3
Take the dry Folium Epimedii of 10kg, pulverizing is 60 order ends, and as extraction agent, material ratio [m (ethanol): m (Herba Epimedii is pulverized dry cauline leaf)] ratio is 9: 1 with 70% aqueous ethanolic solution, be placed in Microwave Extraction Apparatus, with 700W power, temperature 50 C, carry out microwave extraction 8min.To 30L, the concentrated solution B of gained crosses the millipore filtration removal of impurities of 0.45 μ m, obtains liquor C by the extracting solution A vacuum concentration that obtains.Liquor C enters the mobile bed that separates, and sorbent material is polymeric amide, and strippant is 50% ethanolic soln, and its consumption is 3 times of polymeric amide volume; Water wash zone is purified water; Regenerated solvent is 5% sodium hydroxide; Adsorption zone flow velocity 2BV/h; Desorption zone flow velocity 3BV/h; Water wash zone flow velocity 3BV/h; Breeding blanket flow velocity 3BV/h; Be 750s switching time; Temperature is controlled at 50 ℃; Pressure-controlling is at 0.5MPa, collects the component D that is rich in icarin, and it is 92.1% icarin pale yellow powder 103.8g that concentration and recovery ethanol obtains purity by spraying drying, and product recovery rate is 71.9%.Spray-dired parameter is: 140 ℃ of inlet temperature, 30 ℃ of air outlet temperatures, charging mass percent concentration 30wt.%.
Embodiment 4
Take the dry Folium Epimedii of 10kg, pulverizing is 60 order ends, and as extraction agent, material ratio [m (ethanol): m (Herba Epimedii is pulverized dry cauline leaf)] ratio is 12: 1 with 50% aqueous ethanolic solution, be placed in Microwave Extraction Apparatus, with 900W power, temperature 50 C, carry out microwave extraction 8min.To 30L, the concentrated solution B of gained crosses the millipore filtration removal of impurities of 0.45 μ m, obtains liquor C by the extracting solution A vacuum concentration that obtains.Liquor C enters the mobile bed that separates, and sorbent material is polymeric amide, and strippant is 50% ethanolic soln, and its consumption is 3 times of polymeric amide volume; Water wash zone is purified water; Regenerated solvent is 5% sodium hydroxide; Adsorption zone flow velocity 2BV/h; Desorption zone flow velocity 3BV/h; Water wash zone flow velocity 3BV/h; Breeding blanket flow velocity 3BV/h; Be 750s switching time; Temperature is controlled at 50 ℃; Pressure-controlling is at 0.5MPa, collects the component D that is rich in icarin, and it is 92.6% icarin pale yellow powder 105.0g that concentration and recovery ethanol obtains purity by spraying drying, and product recovery rate is 73.1%.Spray-dired parameter is: 140 ℃ of inlet temperature, 30 ℃ of air outlet temperatures, charging mass percent concentration 30wt.%.
Embodiment 5
Detection method
With reverse high performance liquid chromatography, detect Icariin content.
(1) chromatographic condition
Chromatographic column: C18,4.6 * 250mm, 5 μ m
Moving phase: acetonitrile: water=30: 70 (V/V)
Flow velocity: 1.0mL/min
Sample size: 10 μ L
Detect wavelength: 270nm
(2) solution preparation
The reference substance solution preparation: precision takes the icarin reference substance, uses the dissolve with methanol constant volume.
The sample solution preparation: precision takes the icarin sample, with 50% dissolve with ethanol constant volume.
(3) sample determination
Under above-mentioned chromatographic condition, sample introduction is measured, with the content of icarin in the external standard method calculation sample.
Claims (9)
1. one kind from extracting the method for icarin Herba Epimedii, it is characterized in that comprising the following steps:
(1) using aqueous ethanolic solution as extracting solvent, under the condition of microwave heating, extract dry Herba Epimedii cauline leaf, obtain Herba Epimedii extracting solution A;
(2) extracting solution A is carried out to vacuum concentration and obtain concentrated solution B;
(3) concentrated solution B is removed to granulometric impurity through millipore filtration, obtain liquor C;
(4) liquor C is carried out to separating-purifying through simulated moving bed chromatography, obtain being rich in the component D of icarin, by the concentrated concentrated solution E that obtains of component D;
(5) the concentrated solution E that arrives in step (4) is spray-dried, obtain containing the finished product of 90% above icarin.
2. as claimed in claim 1 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (1), the volume fraction of ethanol of aqueous ethanolic solution is 50%～70%, the mass ratio that extracts solvent and Herba Epimedii raw material is 9～12: 1, microwave power 700～900W, 40～60 ℃ of Heating temperatures, heat-up time 8～12min.
3. as claimed in claim 1 or 2 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (3), in liquor C, the total solid amount is 40～50g/L, and icarin concentration is 4～5g/L.
4. as described as any one in claim 1-3 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: the sorbent material that in described step (4), simulated moving bed chromatography is filled is polymeric amide; Strippant is 50% ethanolic soln, and its consumption is 2～3 times of polymeric amide volume; Water wash zone is purified water; The polymeric amide regenerated solvent is 95% ethanol or 5% aqueous sodium hydroxide solution; Adsorption zone flow velocity 1～2BV/h; Desorption zone flow velocity 2～3BV/h; Water wash zone flow velocity 2～3BV/h; Breeding blanket flow velocity 2～3BV/h; Be 600～850s switching time; Temperature is 30～60 ℃; Pressure-controlling is at 0.2MPa～0.6MPa.
5. as described as any one in claim 1-4 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (5), the centrifugal spray drying parameter is 100～140 ℃ of inlet temperature, and 30～60 ℃ of air outlet temperatures, charging mass percent concentration are 30wt.%.
6. as described as any one in claim 1-5 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (1), the volume fraction of ethanol of aqueous ethanolic solution preferred 50%～70%.
7. as described as any one in claim 2-6 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (1), extract the mass ratio preferred 10～12: 1 of solvent and raw material.
8. as described as any one in claim 2-7 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (1), the preferred 800～900W of microwave heating power, preferred 50 ℃ of Heating temperature, heat-up time preferred 10min.
9. as described as any one in claim 2-8 a kind of from Herba Epimedii, extracting the method for icarin, it is characterized in that: in described step (3), preferred use aperture is the millipore filtration of 0.45 μ m.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106635705A (en) * | 2016-12-29 | 2017-05-10 | 广西壮族自治区药用植物园 | Health care wine with cream fragrance and preparation method thereof |
| CN110478531A (en) * | 2019-08-02 | 2019-11-22 | 中南大学湘雅医院 | A kind of platelet rich plasma tissue engineering bracket and preparation method thereof |
| WO2019241947A1 (en) * | 2018-06-21 | 2019-12-26 | 邦泰生物工程(深圳)有限公司 | Method of separating and purifying icariin from epimedium extract |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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Cited By (4)
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| CN106635705A (en) * | 2016-12-29 | 2017-05-10 | 广西壮族自治区药用植物园 | Health care wine with cream fragrance and preparation method thereof |
| CN106635705B (en) * | 2016-12-29 | 2020-06-30 | 广西壮族自治区药用植物园 | Health wine with cream faint scent and preparation method thereof |
| WO2019241947A1 (en) * | 2018-06-21 | 2019-12-26 | 邦泰生物工程(深圳)有限公司 | Method of separating and purifying icariin from epimedium extract |
| CN110478531A (en) * | 2019-08-02 | 2019-11-22 | 中南大学湘雅医院 | A kind of platelet rich plasma tissue engineering bracket and preparation method thereof |
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| CN103396463B (en) | 2016-05-18 |
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