CN115487242A - Radix scrophulariae extract and preparation method and application thereof - Google Patents
Radix scrophulariae extract and preparation method and application thereof Download PDFInfo
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- CN115487242A CN115487242A CN202211437085.0A CN202211437085A CN115487242A CN 115487242 A CN115487242 A CN 115487242A CN 202211437085 A CN202211437085 A CN 202211437085A CN 115487242 A CN115487242 A CN 115487242A
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- 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)
- A61K36/80—Scrophulariaceae (Figwort family)
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- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
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- 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
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Abstract
The invention provides a radix scrophulariae extract as well as a preparation method and application thereof, belonging to the technical field of plant activity extraction. According to the invention, the reflux alcohol extraction mode is adopted to extract the active ingredients (angoroside C, harpagoside and cinnamic acid) in the radix scrophulariae to the greatest extent, and the HPD600, D101 or SPF825 macroporous resin is adopted to improve the yield of the active ingredients, so that the total content of the active ingredients in the radix scrophulariae extract is improved, the radix scrophulariae extract provided by the invention has good tyrosinase inhibitory activity, the melanin content secreted by cells can be obviously reduced, the cytotoxicity is low, and the safety concentration is high; has obvious inhibiting effect on inflammation medium NO and inflammation factor IL-6, has whitening effect on skin care, has the effect of promoting the restoration of canker sore on oral care, and has good application prospect in skin and oral care products. Moreover, the method provided by the invention is simple and convenient to operate and short in time consumption.
Description
Technical Field
The invention relates to the technical field of plant activity extraction, and particularly relates to a radix scrophulariae extract as well as a preparation method and application thereof.
Background
The traditional Chinese medicine radix scrophulariae is dry root of Scrophularia ningpoensis Hemsl (Scrophulariaceae), has effects of clearing heat and cooling blood, nourishing yin and lowering fire, and is used for treating heat-entering nutrient blood, warm poison and macula, fever and yin impairment, crimson tongue and polydipsia, body fluid deficiency and constipation, bone-steaming cough, conjunctival congestion, pharyngalgia, diphtheria, hectic fever and pyogenic infections (2020 version of Chinese pharmacopoeia). The radix scrophulariae extract has the effects of resisting acute cerebral ischemia, treating thromboangiitis obliterans, resisting inflammation, relieving pain, resisting oxidation and inhibiting UVB-mediated photodamage.
Chinese patent CN1679810A discloses a preparation method of radix scrophulariae total glycoside extract, which comprises the steps of extracting radix scrophulariae with 5-20 times of crude drug amount of 40-90% ethanol for 1-3 times, filtering the extract, concentrating, adding ethanol until the alcohol content is 40-80%, standing for precipitation, filtering the supernatant, concentrating, performing chromatography with nonpolar or low-polarity macroporous adsorption resin column, eluting with water until the effluent has no reducing sugar reaction, eluting with 3-20 times of crude drug amount of 20-90% ethanol, collecting ethanol eluate, concentrating, and drying to obtain radix scrophulariae total glycoside extract.
Chinese patent CN102372753A discloses a method for extracting harpagoside, which comprises the steps of taking fresh figwort roots as a raw material, crushing the raw material, adding methanol, ethanol or acetone aqueous solution for reflux extraction, recovering a reagent from an extracting solution, adding a polyamide column for separation, sequentially eluting by using 5 to 10BV water → 4 to 6BV 20 to 30% ethanol (methanol) solution → 5 to 7BV 50 to 70% ethanol (methanol) solution, concentrating an eluent, adding ethyl acetate for extraction for 4 to 6 times, concentrating an extracting solution, adding petroleum ether for crystallization, recrystallizing a methanol-chloroform mixed solution, and drying at low temperature to obtain the harpagoside. However, the figwort extract prepared by the prior art has poor whitening effect.
Disclosure of Invention
In view of the above, the present invention aims to provide a radix scrophulariae extract, and a preparation method and an application thereof, and the radix scrophulariae extract prepared by the present invention has an excellent whitening effect, and can also promote the repair of dental ulcer.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a radix scrophulariae extract, which comprises the following steps:
carrying out reflux alcohol extraction on figwort roots, and then carrying out first concentration to obtain an alcohol extraction crude extract;
loading the alcohol-extracted crude extract into a macroporous resin column, eluting with water, then eluting with a low-concentration alcohol water solution or a high-concentration alcohol water solution, and performing second concentration on the obtained alcohol water eluent to obtain a radix scrophulariae extract;
the macroporous resin in the macroporous resin column comprises at least one of HPD600 resin, D101 resin and SPF825 resin;
the volume fraction of alcohol in the low-concentration alcohol water solution is 35 to 45 percent; the volume fraction of the alcohol in the high-concentration alcohol aqueous solution is 60 to 85 percent.
Preferably, the water consumption for water elution is 2 to 4BV.
Preferably, before elution of the high-concentration alcohol aqueous solution, elution of a low-concentration alcohol aqueous solution is also included, and the volume fraction of alcohol in the low-concentration alcohol aqueous solution is 35 to 45 percent.
Preferably, the dosage of the low-concentration alcohol water solution eluted by the low-concentration alcohol is 1 to 3BV.
Preferably, the dosage of the high-concentration alcohol aqueous solution eluted by the high-concentration alcohol aqueous solution is 3 to 8BV.
Preferably, the alcohol extract for reflux alcohol extraction is an alcohol-water solution, and the volume fraction of alcohol in the alcohol-water solution is 65 to 80 percent;
the volume ratio of the dry weight of the radix scrophulariae to the alcohol extract is 1g:12 to 14mL;
the time of reflux alcohol extraction is 105 to 210min.
Preferably, the second concentrating further comprises: and freeze-drying the figwort root extract obtained by the second concentration.
Preferably, the temperature of the freeze-drying is-50 to-40 ℃.
The invention provides the figwort root extract prepared by the preparation method of the technical scheme, when low-concentration alcohol aqueous solution is adopted for elution, the active component of the figwort root extract comprises angoroside C; when eluted with a high concentration of an aqueous alcohol solution, the active ingredients of the radix scrophulariae extract include angoroside C, harpagoside and cinnamic acid.
The invention provides application of the figwort root extract in the technical scheme in skin care products or preparation of oral care products.
The invention provides a preparation method of a radix scrophulariae extract, which comprises the following steps: carrying out reflux alcohol extraction on figwort roots, and then carrying out first concentration to obtain alcohol extraction crude extract; loading the alcohol-extracted crude extract into a macroporous resin column, eluting with water, then eluting with a low-concentration alcohol water solution or a high-concentration alcohol water solution, and performing second concentration on the obtained alcohol water eluent to obtain a radix scrophulariae extract; the macroporous resin in the macroporous resin column comprises at least one of HPD600 resin, D101 resin and SPF825 resin; the volume fraction of alcohol in the low-concentration alcohol aqueous solution is 35 to 45 percent; the volume fraction of the alcohol in the high-concentration alcohol aqueous solution is 60 to 85 percent. According to the invention, active ingredients (angoroside C, harpagoside and cinnamic acid, or angoroside C) in radix scrophulariae can be extracted to the greatest extent by adopting a reflux alcohol extraction mode, the yield of the active ingredients can be improved by adopting the macroporous resin, so that the total content of the active ingredients in the radix scrophulariae extract is improved, and the excellent whitening effect on the skin care aspect of the radix scrophulariae extract is found by measuring the effects of the extract on tyrosinase inhibition effect and the influence on melanin secretion of melanoma cells; meanwhile, the figwort root extract can promote ulcer healing, and the anti-inflammatory components such as the angoroside C and the like can relieve the congestion and edema inflammatory reaction caused by ulcer, and the figwort root extract also has the analgesic effect reported in documents, has excellent effect on the phenomena of congestion, burning pain and ulcer of oral ulcer in the aspect of oral care, and has good application prospect in skin care products and oral care products. In addition, the invention takes alcohol as an extraction solvent, so the toxicity is low and the cost is low; the preparation method provided by the invention simplifies the alcohol precipitation process, is simple and convenient to operate, consumes short time, and is suitable for industrial production. Moreover, compared with the prior art, the preparation method provided by the invention simplifies an alcohol precipitation process, shortens the process time, does not use volatile organic solvents such as petroleum ether, chloroform, ethyl acetate and the like which belong to forbidden components in cosmetics and oral care products, avoids the risk of solvent residue, and improves the safety of skin care products or oral care products.
As shown in the test results of the examples, the content of the angoroside C in the figwort root extract freeze-dried powder prepared by the invention is up to 19.77wt%, the content of harpagoside is up to 12.55wt%, and the content of cinnamic acid is up to 4.42wt%. The test result for promoting the healing of the oral ulcer shows that the ulcer reduction rate of a tested sample group is highest, the total healing rate of the ulcer on the 5 th day is 40%, and the figwort root extract has a remarkable inhibiting effect on inflammation medium NO and inflammation factor IL-6. The whitening test result shows that the radix scrophulariae extract has good tyrosinase inhibitory activity; the tolerance of the mouse B16 melanoma cells to the radix scrophulariae extract is better, the cytotoxicity of the radix scrophulariae extract is lower, and the safety concentration is high; the content of melanin secreted by cells treated by the figwort root extract freeze-dried powder with the action concentration of 200 mu g/mL and 20 mu g/mL is obviously reduced.
Further, the method comprises the steps of eluting with a low-concentration alcohol-water solution (the volume fraction of alcohol is 35 to 45 percent) and then eluting with a high-concentration alcohol-water solution (the volume fraction of alcohol is 60 to 85 percent), wherein the content of active ingredients of angoloside C, harpagoside and cinnamic acid is improved by adopting a mode of alcohol-water solution gradient elution, and the total amount of active substances (the total amount of the angoloside C, the harpagoside and the cinnamic acid) is increased by 1.8 to 3 times after gradient elution; in addition, the radix scrophulariae extract can be lighter in color and higher in activity by adopting the gradient elution, and is more suitable for skin care products and oral care products.
Drawings
FIG. 1 is a graph showing the results of the yields of active ingredients under static adsorption with different macroporous resins;
FIG. 2 is a color comparison chart (physical diagram and color chart) of an aqueous solution of radix scrophulariae extract prepared from the lyophilized powder of radix scrophulariae extract prepared in examples 3-4, wherein the left is example 4, and the right is example 3;
FIG. 3 is a graph showing the inhibitory effect of Scrophularia ningpoensis extract on NO as an inflammatory mediator;
FIG. 4 is a graph showing the inhibitory effect of Scrophularia ningpoensis extract on IL-6, an inflammatory mediator;
FIG. 5 is a graph showing the results of the inhibition of tyrosinase by radix scrophulariae extract;
FIG. 6 is a graph showing tyrosinase inhibition results of the lyophilized powders of radix scrophulariae extracts prepared in example 5, comparative example 1, and comparative example 2;
FIG. 7 is a graph showing the results of cell viability of mouse B16 melanoma cells under the action of different concentrations of arbutin and figwort root extract;
FIG. 8 is a graph showing the results of cell viability of mouse B16 melanoma cells under the same concentration of beta-arbutin, kojic acid and radix scrophulariae extract;
FIG. 9 is a graph showing the effect of radix scrophulariae extract on the secretion of melanin by mouse B16-F10 melanoma cells.
Detailed Description
The invention provides a preparation method of a figwort root extract, which comprises the following steps:
carrying out reflux alcohol extraction on figwort roots, and then carrying out first concentration to obtain an alcohol extraction crude extract;
loading the alcohol-extracted crude extract into a macroporous resin column, eluting with water, then eluting with a low-concentration alcohol water solution or a high-concentration alcohol water solution, and performing second concentration on the obtained alcohol water eluent to obtain a radix scrophulariae extract;
the macroporous resin in the macroporous resin column comprises at least one of HPD600 resin, D101 resin and SPF825 resin;
the volume fraction of alcohol in the low-concentration alcohol aqueous solution is 35 to 45 percent; the volume fraction of ethanol in the high-concentration alcohol aqueous solution is 60 to 85 percent.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
The invention carries out reflux alcohol extraction on figwort roots and then carries out first concentration to obtain alcohol extraction crude extract.
In the invention, the alcohol extract for refluxing alcohol extraction is preferably an alcohol-water solution, and the volume fraction of alcohol in the alcohol-water solution is preferably 65 to 80 percent, and more preferably 70 to 75 percent; the alcohol preferably comprises methanol and/or ethanol, more preferably ethanol. In the present invention, the ratio of the dry weight of radix scrophulariae to the volume of alcoholic extract is preferably 1g:12 to 14mL, more preferably 1g:7.5mL. In the present invention, it is preferable that the figwort root is pulverized before use, and the pulverization is not particularly limited in the present invention, and the figwort root coarse powder obtained by pulverizing is preferably pulverized to have a particle size of < 24 mesh (700 μm).
In the invention, the time for refluxing and alcohol extracting is preferably 105 to 210min. In a specific embodiment of the present invention, the number of times of the alcohol reflux extraction is preferably 2, specifically: carrying out first reflux alcohol extraction on coarse powder of figwort root, and carrying out first solid-liquid separation to obtain first alcohol extract and residue respectively; carrying out second solid-liquid separation on the residues after second reflux alcohol extraction to obtain a second alcohol extract; and combining the first alcohol extract and the second alcohol extract to obtain the alcohol extract. In the present invention, the ratio of the dry weight of radix scrophulariae to the volume of the first reflux alcohol extraction alcohol is preferably 1g:7 to 8mL, more preferably 1g:7.5mL; the temperature of the first reflux alcohol extraction is preferably 60 to 120min, and more preferably 80 to 100min; the ratio of the dry weight of the radix scrophulariae to the volume of the first reflux alcohol extraction alcohol is preferably 1g:5 to 6mL, more preferably 1g:5.5mL; the temperature of the second refluxing and alcohol extracting is preferably 45 to 90min, and more preferably 50 to 80min. In the present invention, the temperature of the first concentration is preferably 50 to 70 ℃, and more preferably 60 ℃; the pressure of the first concentration is preferably-0.05 to-0.07 MPa, and more preferably-0.06 MPa. The method of the first solid-liquid separation and the second solid-liquid separation is not particularly limited, and a solid-liquid separation method known to those skilled in the art may be adopted, specifically, for example, filter paper is used for reduced pressure filtration, and the pressure of the filter paper for reduced pressure filtration is preferably-0.05 to-0.07 MPa, and more preferably-0.06 MPa.
In the invention, the temperature of the first concentration is preferably 50 to 70 ℃, and more preferably 60 ℃; the concentration pressure is preferably-0.05 to-0.07 MPa, and more preferably-0.06 MPa; the concentration time is not particularly limited, and the concentration is carried out until the mass ratio of the dry weight of the radix scrophulariae to the alcohol extraction crude extract is 1:1.5 to 3, and more preferably 1:2 to 2.5.
After the alcohol-extracted crude extract is obtained, the alcohol-extracted crude extract is loaded into a macroporous resin column and then eluted by water, then low-concentration alcohol-water solution elution or high-concentration alcohol-water solution elution is carried out, and the obtained alcohol-water eluent is subjected to second concentration to obtain a radix scrophulariae extract; the macroporous resin in the macroporous resin column comprises at least one of HPD600 resin, D101 resin and SPF825 resin; the volume fraction of alcohol in the low-concentration alcohol aqueous solution is 35 to 45 percent; the volume fraction of ethanol in the high-concentration alcohol aqueous solution is 60 to 85 percent.
In the present invention, the macroporous resin in the macroporous resin column includes at least one of an HPD600 resin, a D101 resin, and an SPF825 resin, preferably an HPD600 resin, a D101 resin, or an SPF825 resin, more preferably an HPD600 resin. In the present invention, the method for constructing the macroporous resin column preferably comprises the steps of: soaking the macroporous resin in alcohol to obtain activated macroporous resin; and filling the activated macroporous resin into a column, and washing with water to obtain the macroporous resin column. In the invention, the activating agent for alcohol leaching activation is preferably an alcohol aqueous solution, the volume fraction of alcohol in the alcohol aqueous solution is preferably 90 to 95%, and more preferably 95%, the alcohol preferably comprises methanol and/or ethanol, and more preferably ethanol; the macroporous resin is preferably immersed in the activator, and the height difference between the activator and the macroporous resin is preferably 5 to 15cm, and more preferably 10cm. In the invention, the temperature of the alcohol soaking is preferably room temperature, and the time of single alcohol soaking is preferably 6 to 18h, and more preferably 10 to 15h; the frequency of alcohol soaking is not specially limited, and the condition that 3 times of water is added into the resin soaking solution obtained by the last alcohol soaking to prevent turbidity is taken as the standard. The water washing is not particularly limited, and the washing is carried out until the effluent of the water washing is clear and has no alcohol smell. The diameter and the height of the macroporous resin column are measured preferably after the washing is finished, and the volume (BV) and the diameter-height ratio of the macroporous resin column are calculated; the diameter-height ratio of the macroporous resin column is preferably greater than 3, and more preferably 3 to 15.
In the invention, the flow rate of the sample loading is preferably 1 to 1.2BV/h, and more preferably 1.1BV/h. In a specific embodiment of the present invention, during the loading process, preferably, the resin adsorption condition during loading is observed, the loading effluent is collected, HPLC is used to determine the content of active ingredients in the loading effluent, if active ingredients are detected in the loading effluent, the amount of activated macroporous resin is insufficient or the loading column volume is insufficient, and the loading column volume is determined by integrating the resin adsorption condition and the active ingredients content.
In the invention, the flow rate of the water elution is preferably 4 to 6BV/h, more preferably 4.5 to 5.5BV/h, and even more preferably 5BV/h; the amount of water used for elution with water is preferably 2 to 4BV, more preferably 2.5 to 3.5BV, and still more preferably 3BV.
In the invention, the volume fraction of the alcohol in the low-concentration alcohol-water solution is preferably 35 to 45%, more preferably 25 to 35%, and still more preferably 30%; the alcohol preferably comprises methanol and/or ethanol, more preferably methanol; the using amount of the low-concentration alcohol-water solution is preferably 1BV to 3BV, more preferably 1.5BV to 2.5BV, and further preferably 2BV; the flow rate of elution of the low-concentration alcohol water solution is preferably 1 to 1.5BV/h, and more preferably 1 to 1.2BV/h. In the invention, the active ingredient of the figwort root extract finally obtained by eluting with the low-concentration alcohol aqueous solution comprises the angoroside C.
In the invention, the volume fraction of ethanol in the high-concentration alcohol-water solution elution is 60 to 85 percent, preferably 70 to 85 percent, and more preferably 75 to 80 percent; the dosage of the high-concentration alcohol aqueous solution is preferably 3 to 8BV, and more preferably 3 to 6BV; the flow rate of the elution of the high-concentration alcohol aqueous solution is preferably 1 to 1.5BV/h, and more preferably 1 to 1.2BV/h. In the present invention, the alcohol aqueous solution elution preferably includes sequentially performing a first high-concentration alcohol aqueous solution elution and a second high-concentration alcohol aqueous solution elution; the volume fraction of alcohol in the first high-concentration alcohol aqueous solution is preferably 60 to 65 percent, and the using amount of the first high-concentration alcohol aqueous solution is preferably 3 to 4BV; the volume fraction of alcohol in the second high-concentration alcohol aqueous solution is preferably 75 to 85%, and the using amount of the second high-concentration alcohol aqueous solution is preferably 3 to 4BV; the alcohol in the first and second highly concentrated aqueous alcohol solutions is independently preferably methanol and/or ethanol, more preferably ethanol. In the present invention, the low concentration alcohol aqueous solution elutes the active ingredients of the finally obtained figwort extract including angoroside C, harpagoside and cinnamic acid.
Before the elution of the high-concentration alcohol aqueous solution, the method preferably further comprises low-concentration alcohol aqueous solution elution (namely, gradient elution of the alcohol aqueous solution, elution of the low-concentration alcohol aqueous solution and elution of the high-concentration alcohol aqueous solution sequentially after water washing, and collection of the high-concentration alcohol aqueous eluent), wherein the volume fraction of alcohol in the low-concentration alcohol aqueous solution is preferably 35 to 45%, more preferably 25 to 35%, and further preferably 30%; the alcohol preferably comprises methanol and/or ethanol, more preferably methanol; the using amount of the low-concentration alcohol-water solution is preferably 1BV to 3BV, more preferably 1.5BV to 2.5BV, and further preferably 2BV; the flow rate of elution of the low-concentration alcohol-water solution is preferably 1 to 1.5BV/h, and more preferably 1 to 1.2BV/h. In the invention, the alcohol aqueous solution gradient elution is carried out to obtain the active ingredients of the figwort root extract, wherein the active ingredients comprise angoroside C, harpagoside and cinnamic acid.
In the present invention, the temperature of the second concentration is preferably 50 to 70 ℃, and more preferably 60 ℃; the concentration pressure is preferably-0.05 to-0.07 MPa, and more preferably-0.06 MPa; the concentration time is not particularly limited, and the concentration is carried out until the solid content of the figwort extract is 20 to 40wt%, and the solid content of the figwort extract is more preferably 30 to 40wt%.
After the second concentration, the present invention preferably further comprises: and freeze-drying the figwort root extract obtained by the second concentration to obtain the figwort root extract (namely figwort root extract freeze-dried powder). In the invention, the temperature of the freeze-drying is preferably-50 to-40 ℃, and more preferably-45 ℃; the freeze-drying time is not particularly limited, and the freeze-drying is carried out until the water content is less than 5 wt%.
The invention provides the figwort root extract prepared by the preparation method of the technical scheme, when low-concentration alcohol aqueous solution is adopted for elution, the active component of the figwort root extract comprises angoroside C; when high-concentration alcohol aqueous solution elution or alcohol aqueous solution gradient elution is adopted, the active ingredients of the figwort root extract comprise angoroside C, harpagoside and cinnamic acid. In the present invention, the figwort extract is preferably in the form of figwort extract or figwort extract freeze-dried powder.
The invention provides application of the figwort root extract in the technical scheme in skin care products or preparation of oral care products. In the present invention, the oral care product preferably comprises an oral ulcer healing agent. The radix scrophulariae extract adopted by the invention has high total content of active ingredients (angoroside C, harpagoside and cinnamic acid), has good tyrosinase inhibitory activity, can obviously reduce the content of melanin secreted by cells, and has low cytotoxicity and high safety concentration; has obvious inhibiting effect on inflammation medium NO and inflammatory factor IL-6, has whitening effect on skin care, has the effect of promoting the restoration of oral ulcer on oral care, and has good application prospect in skin care products and oral care product preparation.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preparation of activated macroporous resins used in the following examples: immersing the macroporous resin by using 95% (v/v) ethanol water solution for 10cm, immersing for 16h at room temperature, removing the resin, taking the immersion liquid, and repeating the operation until 3 times (volume) of water is added into the resin, so that the activated macroporous resin is not turbid, thereby obtaining the activated macroporous resin; wherein the activated macroporous resin is LS-109D resin, HPD600 resin, D101 resin or SPF825 resin.
Example 1
(1) Pulverizing 100g radix scrophulariae into coarse powder (particle size less than 24 mesh, i.e. particle size less than 700 μm), adding 800mL70% (v/v) ethanol water solution, heating to boil, maintaining slightly boiling first alcohol extraction for 1.5h, filtering with filter paper under reduced pressure of-0.07 MPa, and collecting first alcohol extractive solution and residue respectively; adding 600mL of 70% (v/v) ethanol aqueous solution into the residues, heating to boil, keeping slightly boiling, carrying out secondary alcohol extraction for 1h, filtering by using filter paper under reduced pressure at-0.07 MPa, collecting secondary alcohol extract, discarding filter residues, combining the first alcohol extract and the second alcohol extract, and carrying out reduced pressure concentration at 60 ℃ and-0.07 MPa to obtain 250g of crude alcohol extract.
(2) Screening four kinds of macroporous resin including LS-109D, HPD600, D101 and SPF825 by static adsorption method, weighing 15g of each resin, adding 10g of crude extract, shaking by shaking table at 150r/min for adsorption for 30min, filtering the resin by 300-mesh screen, and collecting filtrate after adsorption; then sequentially using 30mL of water and 40mL of 75% (v/v) ethanol aqueous solution, shaking and rinsing for 15min by using a shaking table at 150r/min, filtering by using a 300-mesh screen, and respectively collecting water rinsing liquid and alcohol rinsing liquid;
the contents of harpagoside, angoroside C and cinnamic acid in the filtrate, water wash and alcohol wash after adsorption of each resin were determined by HPLC method to calculate the yield of active ingredients as shown in table 1 and figure 1:
TABLE 1 yield of active ingredient by static adsorption on different resins
As is clear from Table 1 and FIG. 1, the adsorption effect of HPD-600 resin on active ingredients was the best and the yield of active ingredients was the highest, all together with the yield of active ingredients.
(3) And (3) loading the activated HPD-600 resin into a column, washing the column by purified water after the column is loaded by a water wet method until the washing effluent is clear and has no alcohol smell, wherein the diameter-height ratio is 6.6, and the volume of the activated HPD-600 resin in the HPD-600 resin column is 125mL.
(4) Sampling 125g of the alcohol-extracted crude extract at a sampling flow rate of 1BV/h, collecting the sample-loading effluent, and measuring the content of active ingredients in the sample-loading effluent by HPLC, wherein the test results are shown in Table 2.
(5) Weighing 3BV of purified water, eluting with water (the flow rate is 4 BV/h), collecting water eluent, and concentrating to 72g to obtain water washing extract; the content of active ingredient in the aqueous eluate was determined by HPLC, and the test results are shown in Table 2.
(6) Performing alcohol elution (flow rate is 1 BV/h) by using 4BV of 75% (v/v) ethanol aqueous solution, respectively taking alcohol eluent samples and performing HPLC (high performance liquid chromatography) on the 3 rd BV elution end and the 4 th BV elution end, collecting 75% alcohol eluent and concentrating to 80g to obtain a figwort extract; the content of active ingredients in the 75% alcohol-washed extract is measured by HPLC, and the test result is shown in Table 2.
TABLE 2 weight percentages of loading, water elution and alcohol elution active ingredients
As can be seen from Table 2, the resin was selected as HPD-600 according to the test results, and the eluent was water and 75% (v/v) ethanol aqueous solution, and 75% alcohol eluent was collected.
Example 2
(1) Pulverizing radix scrophulariae 200g into coarse powder (particle size less than 24 mesh), adding 1600mL 70% (v/v) ethanol water solution, heating to boil, maintaining slightly boiling for 1.5 hr for first alcohol extraction, filtering with filter paper under reduced pressure of-0.07 MPa, and collecting first alcohol extractive solution and residue respectively; adding 1200mL of 70% (v/v) ethanol aqueous solution into the residues, heating to boil, keeping the boiling for extracting for 1h with a second alcohol, filtering by using filter paper under reduced pressure, collecting the second alcohol extract, discarding filter residues, combining the first alcohol extract and the second alcohol extract, and concentrating under reduced pressure at the temperature of 60 ℃ and the pressure of-0.07 MPa to obtain 500g of crude alcohol extract.
(2) The activated HPD-600 resin is used for packing the column, purified water is used for washing the resin column after the column is loaded on the column by a water wet method until the effluent of the water washing is clear and has no alcohol smell, the volume of the activated HPD-600 resin in the HPD-600 resin column is 450mL, and the diameter-height ratio is 4.6.
(3) And (3) sampling 450g of the alcohol-extracted crude extract at the sampling flow rate of 1BV/h, observing the resin adsorption condition during sampling, collecting the sampling effluent, and measuring the content of active ingredients in the sampling effluent by HPLC.
(4) Measuring 3BV of purified water for elution (the flow rate is 4 BV/h), and discarding the water washing solution;
(5) Sequentially eluting with 2BV 40% (v/v) ethanol aqueous solution, 3BV 60% (v/v) ethanol aqueous solution and 3BV 75% (v/v) ethanol aqueous solution at the flow rate of 1BV/h, observing the color of each BV eluent, taking an alcohol eluent sample after each BV elution is finished, respectively collecting the alcohol eluents, concentrating under reduced pressure at the temperature of 60 ℃ and under the pressure of-0.07 MPa until the solid content is 40wt%, and respectively obtaining figwort extract 40% alcohol washing extract, figwort extract 60% alcohol washing extract and figwort extract 75% alcohol washing extract; and (3) measuring the content of the active ingredients in each alcohol eluent sample by HPLC, and when the elution is finished without the active ingredients, measuring the content of the active ingredients in each alcohol eluent extract by HPLC, wherein the test results are shown in Table 3.
TABLE 3 Mass percentages of active ingredients and active transfer rates of radix scrophulariae extract
Note: active transfer rate: the active ingredients transferred from the figwort crude extract account for the mass ratio of the active ingredients in the figwort crude extract.
As can be seen from the test results in Table 3, 40% (v/v) ethanol water can further remove impurities, but the loss of the angoroside C exists, 60% (v/v) ethanol water can not elute the cinnamic acid, and 75% (v/v) ethanol water can completely elute the angoroside C, the harpagoside and the cinnamic acid, which indicates that the 75% ethanol extract has the highest content of active ingredients.
Example 3
(1) Pulverizing 420g radix scrophulariae into coarse powder (particle size is less than 24 meshes), adding 2950mL 70% (v/v) ethanol water solution, heating to boil, maintaining slightly boiling first ethanol extraction for 1.5h, filtering with filter paper under reduced pressure of-0.07 MPa, and collecting first ethanol extractive solution and residue respectively; adding 2100mL of 70% (v/v) ethanol aqueous solution into the filter residue, heating to boil, keeping slightly boiling for secondary alcohol extraction for 1h, filtering with filter paper under reduced pressure, collecting secondary alcohol extract, discarding filter residue, mixing the first alcohol extract and the secondary alcohol extract, and concentrating under reduced pressure at 60 deg.C and 0.07MPa to obtain 1050g of crude alcohol extract.
(2) Loading the column with activated HPD-600 resin, loading the column with purified water, washing the column with purified water, clarifying the eluate, and purifying the column with no alcohol smell, wherein the volume of the activated HPD-600 resin in the HPD-600 resin column is 1050mL, and the diameter-height ratio is 5.3.
(3) And (3) loading the alcohol extraction crude extract at the loading flow rate of 1BV/h, observing the resin adsorption condition during loading, and discarding the loading effluent.
(4) Measuring 3BV of purified water to elute the resin column, wherein the water washing flow rate is 4BV/h, and discarding water washing liquid;
(5) Eluting with 3BV 75% (v/v) ethanol water solution at flow rate of 1BV/h, collecting eluate, and concentrating under reduced pressure at 60 deg.C and 0.07MPa to obtain radix scrophulariae extract 168g;
(6) And (3) freeze-drying the figwort root extract at-45 ℃ to obtain figwort root extract freeze-dried powder.
Example 4
(1) Pulverizing radix scrophulariae 300g into coarse powder (particle size is less than 24 meshes), adding 2400mL 70% (v/v) ethanol water solution, heating to boil, maintaining slightly boiling first ethanol extraction for 1.5h, filtering under reduced pressure with filter paper under 0.07MPa, and collecting first ethanol extractive solution and filter residue; adding 1800mL of 70% (v/v) ethanol aqueous solution into filter residue, heating to boil, keeping slightly boiling for secondary alcohol extraction for 1h, filtering by filter paper under reduced pressure, collecting secondary alcohol extract, discarding filter residue, combining the first alcohol extract and the secondary alcohol extract, and concentrating under reduced pressure at 60 ℃ and-0.07 MPa to obtain 750g of crude alcohol extract.
(2) Loading the column with activated HPD-600 resin, loading the column with purified water, washing the column with purified water until the effluent is clear and has no alcohol smell, wherein the volume of the activated HPD-600 resin in the HPD-600 resin column is 750mL, and the diameter-height ratio is 4.6.
(3) And (3) sampling the alcohol extraction crude extract at a sampling flow rate of 1BV/h, and discarding a sampling effluent.
(4) Weighing 3BV of purified water for elution, washing with water at the flow rate of 4BV/h, and discarding the water washing solution.
(5) Performing alcohol elution by using 2BV 40% (v/v) ethanol water solution, discarding eluent, performing alcohol elution by using 3BV 75% (v/v) ethanol water solution at the flow rate of 1BV/h, collecting eluent of 75% (v/v) ethanol water solution, and performing reduced pressure concentration at the temperature of 60 ℃ and the pressure of 0.07MPa to obtain 80g of figwort root extract;
(6) And (3) freeze-drying the figwort root extract at the temperature of-40 ℃ to obtain figwort root extract freeze-dried powder.
HPLC (high Performance liquid chromatography) is used for measuring the content of active ingredients in the figwort root extract freeze-dried powders prepared in examples 3 to 4, and the content is shown in Table 4; the prepared figwort root extract freeze-dried powders prepared in examples 3 to 4 were all prepared into figwort root extract aqueous solutions with a concentration of 0.04wt% (a chromaticity card formed by chromaticity values obtained by a real diagram and a colorimeter test is shown in fig. 2, the left side of fig. 2 is example 4, and the right side is example 3), and the chromaticity values of the figwort root extract aqueous solutions are shown in table 4.
Table 4 mass% of active ingredient in figwort root extract freeze-dried powder in examples 3 to 4
Note: the purification multiple = radix scrophulariae extract freeze-dried powder active ingredient content/radix scrophulariae active ingredient content.
As can be seen from table 4 and fig. 2, the figwort root extract freeze-dried powder prepared by gradient elution in the alcohol elution process has higher purification efficiency and lighter color, and is more suitable for being applied to skin care products and oral care products.
Example 5
(1) Taking 000g of figwort root, crushing into coarse powder (the grain diameter is less than 24 meshes), adding 1600mL of 70% (v/v) ethanol water, heating to boil, keeping slightly boiling for 1.5h by using first alcohol extraction, filtering by using filter paper under reduced pressure, wherein the pressure is 0.07MPa, and collecting first alcohol extraction liquid and filter residue; adding 1200mL of 70% (v/v) ethanol aqueous solution into filter residue, heating to boil, keeping slightly boiling for secondary alcohol extraction for 1h, filtering by using filter paper under reduced pressure, collecting secondary alcohol extract, discarding filter residue, combining the first alcohol extract and the secondary alcohol extract, and concentrating under reduced pressure at 60 ℃ and under the condition of-0.07 MPa to obtain 500g of crude alcohol extract.
(2) Loading 2 columns (respectively marked as a resin column A and a resin column B) with the activated HPD-600 resin, washing the resin columns with purified water after wet-process column loading until the effluent of the water washing is clear and has no alcohol smell, wherein the volume of the activated HPD-600 resin in the HPD-600 resin column is 105mL, and the diameter-height ratio is 5.
(3) Respectively taking 175g of the alcohol extraction crude extract for sample loading, wherein the sample loading flow rate is 1BV/h, and discarding the sample loading effluent liquid.
(4) Respectively weighing 3BV of purified water for elution, washing with water at the flow rate of 4BV/h, and discarding the water washing solution.
(5) Gradient elution on resin column a: performing alcohol elution by using 2BV 40% (v/v) ethanol water solution (the flow rate is 3 BV), collecting 40 (v/v) ethanol water solution eluent, performing alcohol elution by using 4BV 75% (v/v) ethanol water solution (the flow rate is 1.2 BV), collecting 75% (v/v) ethanol water solution eluent, and performing reduced pressure concentration on the 40 (v/v) ethanol water solution eluent and the 75% (v/v) ethanol water solution eluent under the conditions of 60 ℃ and 0.07MPa respectively to obtain 30g of gradient-40% alcohol-washed radix scrophulariae extract and 30g of gradient-75% alcohol-washed radix scrophulariae extract respectively.
(6) Directly eluting the resin column B by using a high-concentration alcohol aqueous solution: ethanol elution is carried out by using 4BV 75% (v/v) ethanol water solution (the flow rate is 1.2 BV), eluent is collected and is decompressed and concentrated under the conditions of 60 ℃ and 0.07MPa, and 30g of figwort extract which is directly washed by 75% ethanol is obtained.
(7) Respectively lyophilizing the gradient-40% ethanol-washed radix scrophulariae extract, the gradient-75% ethanol-washed radix scrophulariae extract and the 75% ethanol-washed radix scrophulariae extract at-40 deg.C to obtain gradient-40% ethanol-washed radix scrophulariae extract lyophilized powder, gradient-75% ethanol-washed radix scrophulariae extract lyophilized powder and 75% ethanol-washed radix scrophulariae extract lyophilized powder.
Comparative example 1
Harpagoside (purity 98%) obtained according to example 1 of CN102372753A, and a sample was designated harpagoside 98% (CN 102372753A).
Comparative example 2
Radix scrophulariae Total glycosides extract obtained according to example 3 of CN1679810A, sample is radix scrophulariae Total glycosides extract (CN 1679810A)
Test example 1
Anti-inflammatory performance test of figwort root extract freeze-dried powder prepared in example 3
(1) Test for promoting healing of oral ulcer
Canker sores are characterized primarily by ulceration, congestion, edema and burning pain, which are associated with inflammatory reactions.
(1.1) adopting 20 SPF SD male rats, establishing a canker sore model by referring to GQT/ZY-DL-016, and randomly dividing the successfully molded rats into a model control group (coated with water) and a test sample group according to the size of the canker area, wherein each group comprises 10 rats. The tested sample group is continuously smeared on the oral ulcer part for 5 days by using 0.5wt% figwort root extract aqueous solution 1 time a day, the area of the oral ulcer is measured every day, the difference is judged to have statistical significance by the test result P < 0.05, and the test result is shown in Table 5.
TABLE 5 oral ulcer healing test results
Note: compared to the model control group, < 0.05.
As can be seen from Table 5, the final ulcer decreasing rate of the test sample group was increased and the total ulcer healing rate on day 5 was 40% as compared with the model control group.
(2) Inhibition of inflammatory response assay
Mouse macrophage Raw264.7 induced by LPS is used as a cell inflammation model, the inflammation inhibition effect of the radix scrophulariae extract is evaluated by measuring the inhibition effect of the radix scrophulariae extract freeze-dried powder on inflammation medium NO and inflammatory factor IL-6, a blank control group and a positive control group are arranged, wherein the positive control drug is dexamethasone (PC), the test results are shown in figures 3-4 and tables 6-7, wherein the figure 3 shows the inhibition effect of the radix scrophulariae extract on inflammation medium NO, and the figure 4 shows the inhibition effect of the radix scrophulariae extract on inflammation medium IL-6.
TABLE 6 inhibitory effect of radix scrophulariae extract lyophilized powder on inflammation mediator NO
TABLE 7 inhibitory effect of radix scrophulariae extract lyophilized powder on IL-6 as inflammatory mediator
As can be seen from fig. 3 to 4 and tables 6 to 7, the experimental results show that: the radix scrophulariae extract has significant inhibitory effect on inflammation mediator NO and inflammation factor IL-6, and the difference has statistical significance (P is less than 0.001).
Test example 2
Whitening performance test of radix scrophulariae extract freeze-dried powder
(1) Tyrosinase inhibition assay
(1.1) tyrosinase inhibition test of the lyophilized powder of radix scrophulariae extract obtained in example 3
The diphenolase activity of tyrosinase can directly catalyze a substrate dopa to generate dopaquinone, and then melanin is finally generated through a series of reactions; the amount of melanin substances produced is proportional to the activity of the enzyme, so the amount of the enzyme activity can be reflected by measuring the amount of the melanin substances produced in the system.
0.02wt% kojic acid solution: the kojic acid is precisely weighed into a 25mL volumetric flask, is added with water to be dissolved, is diluted to a constant volume to scale and is shaken up to obtain a kojic acid solution with the concentration of 0.02wt% for later use.
0.1wt% figwort extract solution: accurately weighing radix scrophulariae extract lyophilized powder into a 25mL volumetric flask, adding water, dissolving with ultrasound, diluting to constant volume to scale, shaking, and filtering with 0.45 μm filter membrane to obtain radix scrophulariae extract solution with concentration of 0.1 wt%.
Tyrosinase inhibition results are shown in figure 5 and table 8.
TABLE 8 tyrosinase inhibition results
As can be seen from fig. 5 and table 8, the graph shows that the figwort root extract freeze-dried powder has good tyrosinase inhibitory activity, and the tyrosinase inhibitory activity of the 0.1% figwort root extract solution is equivalent to that of the 0.02% kojic acid solution.
(1.2) tyrosinase inhibition test of the lyophilized powder of radix scrophulariae extract prepared in example 5 and comparative example 1
According to the tyrosinase inhibition test method in the step (1.1), the gradient-40% alcohol-washed radix scrophulariae extract freeze-dried powder, the gradient-75% alcohol-washed radix scrophulariae extract freeze-dried powder and the 75% ethanol-washed radix scrophulariae extract freeze-dried powder prepared in the example 5, the harpagoside 98% (CN 102372753A) prepared in the comparative example 1 and the radix scrophulariae total glycoside extract (CN 1679810A) prepared in the comparative example 2 are tested, and the test results are shown in FIG. 6, as can be seen from FIG. 6, 98% of harpagoside samples prepared in the CN 72753A do not show obvious tyrosinase inhibition activity, and the tyrosinase inhibition activity of the radix scrophulariae total glycoside extract prepared in the CN1679810A is obviously lower than that of the radix scrophulariae extract freeze-dried powder prepared in the invention.
(2) Safety test
Kojic acid, derivatives thereof and arbutin are effective whitening components commonly used in whitening cosmetics at home and abroad at present, the MTT method is used for determining the influence of the kojic acid, the arbutin and the radix scrophulariae extract on the cell viability of mouse B16 melanoma cells, the cell viability is generally required to be more than 90% to judge that the cells have no problem, and the cell viability% = OD value of an experimental group/OD value of a blank control group is 100%. The safety test results are shown in fig. 7-8 and tables 9-10, wherein fig. 7 is a graph showing cell viability results of mouse B16 melanoma cells under the action of arbutin and figwort root extracts with different concentrations, and fig. 8 is a graph showing cell viability results of mouse B16 melanoma cells under the action of beta-arbutin, kojic acid and figwort root extracts with the same concentrations.
TABLE 9 cell viability of mouse B16 melanoma cells under the action of different concentrations of arbutin and radix scrophulariae extract
TABLE 10 cell viability of mouse B16 melanoma cells by the same concentrations of beta-arbutin, kojic acid and radix scrophulariae extract
Note: the cell viability data for kojic acid in table 10 are derived from the literature: effect of kojic acid oligopeptides on tyrosinase activity and melanin synthesis of mouse B16 melanoma cells [ J ] china journal of skin diseases: 2013, 27 (12): 1221-1224.
As can be seen from fig. 7 to 8 and tables 9 to 10, the tolerance of the mouse B16 melanoma cells to the figwort root extract is better, the cytotoxicity of the figwort root extract is lower, and the safe concentration is high.
(3) Effect of the test on the secretion of melanin by B16-F10 melanoma cells in mice
By taking mouse melanoma cells (B16-F10) as a model, firstly, the concentration which has no obvious influence on the cell viability is screened as the maximum safe concentration by a method for measuring the cell viability by MTT, the influence of samples with different concentrations on the melanin secretion of the cells is tested in the safe concentration range, the potential whitening effect of the radix scrophulariae extract is evaluated, and the test results are shown in fig. 9 and table 11.
TABLE 11 Effect on melanin content secreted by mouse B16-F10 melanoma cells
As can be seen from fig. 9 and table 11, the melanin content of the cells treated by the positive control group (β -arbutin, kojic acid) was significantly decreased (P < 0.05) compared to the negative control group (NC), indicating that this experiment was effective; the content of melanin secreted by cells treated by the figwort root extract freeze-dried powder with the action concentration of 200 mug/mL and 20 mug/mL is obviously reduced (P is less than 0.05), and the difference has statistical significance. Therefore, the radix scrophulariae extract prepared by the method has potential whitening effect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The preparation method of the figwort root extract is characterized by comprising the following steps:
carrying out reflux alcohol extraction on figwort roots, and then carrying out first concentration to obtain alcohol extraction crude extract;
loading the alcohol-extracted crude extract into a macroporous resin column, eluting with water, then eluting with a low-concentration alcohol water solution or a high-concentration alcohol water solution, and performing second concentration on the obtained alcohol water eluent to obtain a radix scrophulariae extract;
the macroporous resin in the macroporous resin column comprises at least one of HPD600 resin, D101 resin and SPF825 resin;
the volume fraction of alcohol in the low-concentration alcohol aqueous solution is 35 to 45 percent; the volume fraction of the alcohol in the high-concentration alcohol aqueous solution is 60 to 85 percent.
2. The method for producing a water-soluble polysaccharide according to claim 1, wherein the amount of water used for elution with water is 2 to 4BV.
3. The preparation method according to claim 1, further comprising eluting with a low-concentration alcohol aqueous solution before eluting with the high-concentration alcohol aqueous solution, wherein the volume fraction of alcohol in the low-concentration alcohol aqueous solution is 35 to 45%.
4. The production method according to claim 1 or 3, wherein the amount of the low-concentration alcohol-eluting aqueous solution is 1 to 3BV.
5. The method according to claim 1, wherein the amount of the high concentration aqueous alcohol solution eluted is 3 to 8BV.
6. The preparation method of claim 1, wherein the alcohol extraction agent for reflux alcohol extraction is an alcohol-water solution, and the volume fraction of alcohol in the alcohol-water solution is 65 to 80 percent;
the volume ratio of the dry weight of the radix scrophulariae to the alcohol extract is 1g:12 to 14mL;
the time of reflux alcohol extraction is 105 to 210min.
7. The method of claim 1, further comprising, after the second concentrating: and freeze-drying the figwort root extract obtained by the second concentration.
8. The method according to claim 7, wherein the temperature of the lyophilization is-50 to-40 ℃.
9. The figwort root extract prepared by the preparation method according to any one of claims 1 to 8, wherein when the figwort root extract is eluted by a low-concentration alcohol-water solution, the active ingredient of the figwort root extract comprises angoroside C; when eluted with a high concentration of an aqueous alcohol solution, the active ingredients of the radix scrophulariae extract include angoroside C, harpagoside and cinnamic acid.
10. Use of the figwort extract according to claim 9 in skin care products or in the preparation of oral care products.
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Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20000010275A (en) * | 1998-07-31 | 2000-02-15 | 성재갑 | Composition for skin whitening |
| KR20040074697A (en) * | 2003-02-18 | 2004-08-26 | 학교법인 한림대학교 | Scrophularia buergeriana extract with preventing or improving activity of skin wrinkle and a composition containing the extract |
| CN1679810A (en) * | 2005-02-02 | 2005-10-12 | 深圳市凯尔腾科技有限公司 | A kind of Scrophulariaceae total glycosides extract, its preparation method and its application in pharmacy |
| CN1931868A (en) * | 2006-09-29 | 2007-03-21 | 张惠东 | Figwort total phenyl glycoside and its prepn process and application |
| CN101167733A (en) * | 2006-10-23 | 2008-04-30 | 杨泗兴 | Venous injection powder injection for preventing and treating ischemic cerebral apoplexy and preparation method thereof |
| CN101744937A (en) * | 2009-12-31 | 2010-06-23 | 浙江中医药大学 | Method for extracting effective components of figwort for resisting cerebral ischemia and method for preparing dropping pills |
| CN104327127A (en) * | 2014-09-30 | 2015-02-04 | 浙江工业大学 | Method for preparing angroside C, aucubin and harpagide through separation and purification by high-speed countercurrent chromatography |
| CN105287885A (en) * | 2015-11-06 | 2016-02-03 | 贵州天豪民族药业有限公司 | Method for extracting radix scrophulariae saponin from radix scrophulariae leftovers |
| CN105362462A (en) * | 2014-08-28 | 2016-03-02 | 贵州天豪民族药业有限公司 | Comprehensive extraction technology for radix scrophulariae stem leaf bioactive components |
| CN105707489A (en) * | 2016-03-22 | 2016-06-29 | 吴正锋 | Traditional Chinese medicine scrophularia ningpoensis extract for improving productivity and muscle quality of pork pigs |
| KR20160119548A (en) * | 2015-04-06 | 2016-10-14 | 연세대학교 원주산학협력단 | Skin whitening composition comprising Scrophularia buergeriana hot water extract as an active ingredient |
| CN108440612A (en) * | 2018-06-26 | 2018-08-24 | 西南大学 | The isolation and purification method of three kinds of iridoid constituents in a kind of radix scrophulariae |
| CN109709249A (en) * | 2018-12-27 | 2019-05-03 | 药圣堂（湖南）制药有限公司 | A kind of Quality evaluation method based on the more active component detections of radix scrophulariae |
| CN111616995A (en) * | 2020-04-14 | 2020-09-04 | 云南英格生物技术有限公司 | Coffee silverskin extract and preparation method and application thereof |
| CN112362792A (en) * | 2020-12-15 | 2021-02-12 | 北京中医药大学 | Radix scrophulariae iridoid control extract and preparation method and application thereof |
| CN113476356A (en) * | 2021-04-30 | 2021-10-08 | 云南英格生物技术有限公司 | Preparation method and application of pyracantha fortuneana fruit extract |
-
2022
- 2022-11-17 CN CN202211437085.0A patent/CN115487242A/en active Pending
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20000010275A (en) * | 1998-07-31 | 2000-02-15 | 성재갑 | Composition for skin whitening |
| KR20040074697A (en) * | 2003-02-18 | 2004-08-26 | 학교법인 한림대학교 | Scrophularia buergeriana extract with preventing or improving activity of skin wrinkle and a composition containing the extract |
| CN1679810A (en) * | 2005-02-02 | 2005-10-12 | 深圳市凯尔腾科技有限公司 | A kind of Scrophulariaceae total glycosides extract, its preparation method and its application in pharmacy |
| CN1931868A (en) * | 2006-09-29 | 2007-03-21 | 张惠东 | Figwort total phenyl glycoside and its prepn process and application |
| CN101167733A (en) * | 2006-10-23 | 2008-04-30 | 杨泗兴 | Venous injection powder injection for preventing and treating ischemic cerebral apoplexy and preparation method thereof |
| CN101744937A (en) * | 2009-12-31 | 2010-06-23 | 浙江中医药大学 | Method for extracting effective components of figwort for resisting cerebral ischemia and method for preparing dropping pills |
| CN105362462A (en) * | 2014-08-28 | 2016-03-02 | 贵州天豪民族药业有限公司 | Comprehensive extraction technology for radix scrophulariae stem leaf bioactive components |
| CN104327127A (en) * | 2014-09-30 | 2015-02-04 | 浙江工业大学 | Method for preparing angroside C, aucubin and harpagide through separation and purification by high-speed countercurrent chromatography |
| KR20160119548A (en) * | 2015-04-06 | 2016-10-14 | 연세대학교 원주산학협력단 | Skin whitening composition comprising Scrophularia buergeriana hot water extract as an active ingredient |
| CN105287885A (en) * | 2015-11-06 | 2016-02-03 | 贵州天豪民族药业有限公司 | Method for extracting radix scrophulariae saponin from radix scrophulariae leftovers |
| CN105707489A (en) * | 2016-03-22 | 2016-06-29 | 吴正锋 | Traditional Chinese medicine scrophularia ningpoensis extract for improving productivity and muscle quality of pork pigs |
| CN108440612A (en) * | 2018-06-26 | 2018-08-24 | 西南大学 | The isolation and purification method of three kinds of iridoid constituents in a kind of radix scrophulariae |
| CN109709249A (en) * | 2018-12-27 | 2019-05-03 | 药圣堂（湖南）制药有限公司 | A kind of Quality evaluation method based on the more active component detections of radix scrophulariae |
| CN111616995A (en) * | 2020-04-14 | 2020-09-04 | 云南英格生物技术有限公司 | Coffee silverskin extract and preparation method and application thereof |
| CN112362792A (en) * | 2020-12-15 | 2021-02-12 | 北京中医药大学 | Radix scrophulariae iridoid control extract and preparation method and application thereof |
| CN113476356A (en) * | 2021-04-30 | 2021-10-08 | 云南英格生物技术有限公司 | Preparation method and application of pyracantha fortuneana fruit extract |
Non-Patent Citations (4)
| Title |
|---|
| 叶孝兆，等: "富含苯丙烯酸的天然植物提取物对酪氨酸酶活性的影响", 《广东化工》 * |
| 李祚丹，等: "玄参中环烯醚萜类物质的分离纯化工艺", 《中成药》 * |
| 田金凤，等: "玄参中化学成分的分离鉴定及其降糖活性研究", 《食品工业科技》 * |
| 韩龙，等: "玄参提取物对动物复发性口腔溃疡组织中转化生长因子-β_1表达的影响", 《齐齐哈尔医学院学报》 * |
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