CN100422199C - Extractive from specific part of skullcap, preparation method and application - Google Patents
Extractive from specific part of skullcap, preparation method and application Download PDFInfo
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- CN100422199C CN100422199C CNB2005100314527A CN200510031452A CN100422199C CN 100422199 C CN100422199 C CN 100422199C CN B2005100314527 A CNB2005100314527 A CN B2005100314527A CN 200510031452 A CN200510031452 A CN 200510031452A CN 100422199 C CN100422199 C CN 100422199C
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Abstract
The present invention relates to a specific position of baikal skullcap root. The present invention is characterized in that the specific position of the labiate baikal skullcap root is from 4 to 6cm close to ground surface and from 1 to 2cm close to under ground in a figure 1. The extract of the specific position of the baikal skullcap root is prepared by extraction. The extract of the specific position of the baikal skullcap root has the following characteristics: the extract of the specific position of the baikal skullcap root is measured by a high efficiency liquid phase method, and the content of baicalin is not less than 70.0 wt. %; the content of scutellarin is not less than 5.0 wt. %, and the content of total minor flavone is not less than 10.0 wt. %; the three components are not less than 85.0 wt. %. The extract of the specific position of the baikal skullcap root has anti-inflammatory activity. The present invention relates to the application of cosmetics, health care products and medicine containing the components with the purpose of anti-inflammatory activity.
Description
Technical field
The present invention relates to new extractive from specific part of skullcap and preparation method thereof and application.
Background technology
The root of large-flowered skullcap (Scutellaria Baicalensis Georgi) is one of conventional Chinese medicine, and the root of large-flowered skullcap that Chinese Pharmacopoeia records is the root of the labiate root of large-flowered skullcap, has effects such as heat-clearing and damp-drying drug, eliminating fire and detoxication, arresting bleeding and miscarriage prevention.Its main effective constituent is flavonoid compound, mainly contain: baicaline, scutellarin, demethyl wogonin-7-glycoside acid, the acid of QIANCENGZHI-7 glycoside, the acid of wogonin-7 glycoside, scutellarin, wogonin and chrysin etc. (Lee makes equality. foreign medical science plant amedica fascicle .1994,9 (4): 147), see Table one.
Table one, main component structure
Glucuronosyl: glucoside acidic group; Gluronosyl: glucosyl group.
Modern pharmacological research proof root of large-flowered skullcap over-ground part has antianaphylaxis, anti-oxidant, carcinogenesis and effect such as antiviral, also has a certain protection effect to cardiovascular.The root of large-flowered skullcap is that use range is wider in the traditional Chinese medicine, a kind of medicinal herbs most in use that usage quantity is bigger, and the growth cultivated area is very big, follows gathering of scutellariae,radix every year, produce a large amount of root of large-flowered skullcap dis-medicinal part plant materialss.Therefore, the development and use to the dis-medicinal part of the root of large-flowered skullcap are of great value work.
A lot of Chinese medicines for a long time only with a certain position of plant materials as medicinal, other parts are then underused, and have caused the waste of resource.Hu Zhixiang etc. (medicinal plant different sites development and use overview. the time precious traditional Chinese medical science traditional Chinese medicines, 1998,9 (6): 581) development and use of pointing out the medicinal plant different sites have prospect very much, not only can enlarge the resource of Chinese medicine, also can therefrom find purposes or new function that some are new simultaneously.
Research to root of large-flowered skullcap dis-medicinal part at present mainly concentrates on Caulis et Folium Scutellariae.Patent 98126822.6 (application number) discloses the pharmaceutical use and the new purposes of Caulis et Folium Scutellariae, confirms that the Caulis et Folium Scutellariae ingredient has analgesia, anti-inflammatory, effect such as analgesic.Meng Yanbin etc. (assay of total flavones and scutellarin [J] in the different growing stages Caulis et Folium Scutellariae. Chengde Medical College's journal, 2003,20 (3): 259) composition of having studied the Caulis et Folium Scutellariae that different times is gathered in a year changes, and finds that the best collecting season of Caulis et Folium Scutellariae should be in the fall.
At present the patent relevant with the present invention is: 98126822.6,03138015.8,01110843.6,200410024693.4,200310109290.5 (application numbers) etc., related to scutellariae,radix, and Caulis et Folium Scutellariae is the composition extraction and the related application of raw material.
Summary of the invention
The present invention relates generally to two aspects to the exploitation of root of large-flowered skullcap dis-medicinal part: utilize the dis-medicinal part exploitation of the root of large-flowered skullcap can substitute the product of scutellariae,radix purposes; Or find new purposes.
The object of the present invention is to provide a kind of clear and definite extractive from specific part of skullcap of content that extracts with root of large-flowered skullcap privileged site raw material.
Another object of the present invention provides the preparation method of above-mentioned root of large-flowered skullcap specific extraction thing.
An also purpose of the present invention provides the application of above-mentioned extractive from specific part of skullcap.
The objective of the invention is to realize by following manner:
Raw material used in the present invention is the dis-medicinal part of the labiate root of large-flowered skullcap.
Raw material used in the present invention is: the privileged site of the root of large-flowered skullcap promptly refers to 1-2cm part under the 4-6cm near the ground of the labiate root of large-flowered skullcap and the near-earth; Another raw material that extractive from specific part relates to is the labiate root of large-flowered skullcap top branches and leaves of gathering autumn, and extract the clear and definite extractive from specific part of skullcap of content and be characterized as: be characterized by with the high performance liquid phase method: baicalin content is not less than 70.0%; Scutellarin content is not less than 5.0%; Total less important flavones content is not less than 10.0%, and above-mentioned three kinds of component sums are not less than 85.0%, by weight.
The root of large-flowered skullcap privileged site of indication of the present invention refers to 1-2cm part under the 4-6cm near the ground of the labiate root of large-flowered skullcap and the near-earth, as shown in Figure 1; Another raw material that extractive from specific part relates to is the labiate root of large-flowered skullcap top branches and leaves of gathering autumn, also as shown in Figure 1.
The present invention is to be parent with traditional conventional Chinese medicine root of large-flowered skullcap; with modern analysis measuring technology and drug screening technology is means; dis-medicinal part to the traditional Chinese medicine root of large-flowered skullcap is studied screening, can effectively reduce the blindness and the risk of exploitation, also helps and makes full use of natural resources of Chinese medicinal materials and environment protection.Part is national in the world at present, such as, Brazil, Japan etc., strict use position and the use range that limits some traditional herbal medicines, the use people from field of herbal medicine is for dwindling.Therefore, the dis-medicinal part of traditional herbal medicines is developed, seeking substitute also is a kind of disadvantageous policy barrier of avoiding, and widens the available strategy of the world market of China's tcm product.Then a kind of so just product of the present invention can play to a great extent avoids disadvantageous policy barrier, enlarges the use field, promotes the smooth circulation of root of large-flowered skullcap product in the world market.
The present invention provides for the first time the mixture that extractive from specific part of skullcap can clear and definite content clearly.And Radix Scutellariae extract in the past all is to set about from raw material, and do not know the content of its composition, let alone more accurately show this mixture and obviously different from the past the feeding intake with starting material of extractive from specific part of skullcap provided by the present invention calculated or with the radix scutellariae medicinal materials or the extract of single component explanation, be a kind of new Radix Scutellariae extract that can accurately explain its component content.And extract of the present invention can prepare well, and can be with simple and means science are carried out quality control.Thereby on behalf of the tcm product of China, product of the present invention also can obtain the recognition and acceptance of international community.The present invention realizes that for tcm product the modernization of Chinese medicine provides a kind of implementation.
The preparation method of another object of the present invention extractive from specific part of skullcap is:
The extractive from specific part of skullcap extraction process
Can adopt ethanol-extracted technology:
(1) root of large-flowered skullcap privileged site, promptly 1-2cm part under the 4-6cm near the ground of the root of large-flowered skullcap and the near-earth is ground into meal, extracts secondary, adds 4-8 for the first time and doubly measures alcohol reflux 1.5-3 hour of 80-95%; Add for the second time 2-4 and doubly measure alcohol reflux 1-2 hour of 80-95%, filter;
(2) filtrate is concentrated into nothing alcohol flavor;
(3) with 20-50%NaOH or KOH solution concentrated solution pH value is transferred to pH7-9.5;
(4) leave standstill 1-4 hour, solution is collected in centrifugal or filtration;
(5) when solution temperature during at 40 ℃-50 ℃, with the concentrated hydrochloric acid or the vitriol oil centrifugate pH value is transferred to pH1.5-3, ℃ of-90 ℃ insulations of reheat to 75 30-40 minute are filtered or centrifugal, the collecting precipitation thing;
(6) will precipitate 60-80 ℃ of hot water wash of usefulness to neutral, the dry dry powder that gets;
(7) after gained dry powder is pulverized, is sieved dry powder A.
Or employing water extraction process:
(1) root of large-flowered skullcap privileged site, promptly 1-2cm part under the 4-6cm near the ground of the root of large-flowered skullcap and the near-earth is ground into meal, extracts secondary, adds the poach that 6-10 doubly measures for the first time and carries 1.5-3 hour.Add for the second time 3-6 times of water gaging and boil and carry 1-2 hour, filter or centrifugal, collect extracting solution;
(2) extracting solution is inserted the 1/2-1/3 that is concentrated to original volume in the thickener;
(3) with 20-50%NaOH or KOH solution concentrated solution pH value is transferred to pH 7-9.5;
(4) leave standstill 1-4 hour, solution is collected in centrifugal or filtration;
(5) when solution temperature at 40 ℃ more than-50 ℃ the time, with concentrated hydrochloric acid or concentrated sulfuric acid solution centrifugate pH value is transferred to pH1.5-3, reheat is to 75-90 ℃ of insulation 20-40 minute, filters or centrifugal the collecting precipitation thing;
(6) will precipitate 40-80 ℃ of hot water wash of usefulness to neutral, the dry dry powder that gets;
(7) after gained dry powder is pulverized, is sieved dry powder B.
Two, root of large-flowered skullcap branches and leaves extraction process
(1) root of large-flowered skullcap branches and leaves that will gather autumn are ground into meal, drop in the extraction equipment, extract secondary, add 4-8 for the first time and doubly measure alcohol reflux 1-2 hour of 70-80%.Add for the second time 2-4 and doubly measure alcohol reflux 1-1.5 hour of 70-80%, filter;
(2) filtrate is concentrated into the 15-25 Baume;
(3) dry, pulverize, sieve, after dry powder C.
Three, extractive from specific part of skullcap preparation
(1) obtain dry powder D by A and C allotment, described dry powder D is extractive from specific part of skullcap.
(2) obtain dry powder E by B and C allotment, described dry powder E also is an extractive from specific part of skullcap.
The extractive from specific part of skullcap of above-mentioned preparation and the makeup with anti-inflammatory action, protective foods and the medicine that contain this extract are not seen announcement at home and abroad, and this extract feature sees Table two.
Characterize with the high performance liquid phase method, content by weight, this extract feature sees Table two and accompanying drawing (as Fig. 1, Fig. 2, Fig. 3, shown in Figure 4).
The feature of table two, extractive from specific part of skullcap
Annotate: total less important flavones comprises described in the table: Norwogonin-7-Glucuronide; Oroxylin-7-Glucuronide; Wogonin-7-0-glucosiduronate; Scutellarin; Wogonin; Chrysin.
Another object of the present invention relate to will contain this extract makeup, protective foods and pharmaceutical applications in the anti-inflammatory activity direction.
Extract of the present invention can be applicable to the medicine of various formulations, comprises capsule, tablet, oral liquid, injection, pill etc.
With rational extraction process root of large-flowered skullcap privileged site is extracted, the gained extractive from specific part makes up the composition that can have anti-inflammatory activity, can will contain makeup, protective foods and the pharmaceutical applications of this composition in the anti-inflammatory activity direction.
The present invention relates to the production and the application of extractive from specific part of skullcap, the present invention has improved the utilization ratio of plant resources, can obtain good economic benefits and social benefit.Extract of the present invention can use in some is not suitable for field that scutellariae,radix uses, such as in Brazil, closing rules and regulations: the herbal medicine that uses as medicine must not use as the raw material of food or foodstuff production, and just can avoid this disadvantageous policy barrier from the extractive from specific part of root of large-flowered skullcap dis-medicinal part, promote of the smooth circulation of root of large-flowered skullcap product in the world market.Therefore the utilization of this Products Development is the breakthrough to the traditional developing thought and the field of use.Technology used in the present invention has simple, lower-cost advantage, and the qualitative characteristics of products obtained therefrom is clearly reasonable, the characterization method science, the quality of product is controlled fully.Extractive from specific part of the present invention has better anti-inflammatory activity, and the makeup, protective foods and the medicine that contain this extractive from specific part can be applicable to the anti-inflammatory activity direction.
In order better to understand essence of the present invention, below with example explanation more specifically.
Test
The root of large-flowered skullcap privileged site composition of the present invention's preparation is to the anti-inflammatory action of inflammatory animal model.
1, experiment material
Animal: mouse, Kunming kind; Rat, the Wistar strain provides by Hunan College of Traditional Chinese Medicine's Experimental Animal Center.
Medicine: root of large-flowered skullcap privileged site composition, prepared of the present invention.
Hydrocortisone: Henan Lihua Pharmaceutical Co., Ltd. produces, lot number: 031204.
More than the equal room temperature preservation of the medicine of Shi Yonging is mixed with the proper concn soup with physiological saline during experiment and uses.
2, method and result
2.1 p-Xylol causes the influence of mice auricle swelling reaction.Kunming mouse, male, 26～30g by the body weight layering, is divided into 5 groups of blanks, hydrocortisone, the large, medium and small dosage of baikal skullcap root composition, 12 every group at random.Each organizes mouse by 20ml/kg volume gastric infusion, and the 12h administration is 3 times at interval.60min is with dimethylbenzene contact auris dextra 5s after the last administration, and 15min takes off cervical vertebra and puts to death mouse, uses the punch tool of diameter 6mm that ears are downcut with the position homalographic, takes by weighing left and right sides auricle weight, calculates auricle edema rate (%) and inhibitory rate of intumesce (%).Experimental result sees Table three.
Table three p-Xylol causes the acutely inflamed restraining effect of Mice Auricle (x ± s)
Annotate: 1. baikal skullcap root composition fingerprint characteristic extract calculates by pure product, down together; 2. relatively t check between organizing is compared * P＜0.05 with the blank group, * * P＜0.01, down together.
2.2 egg white is caused the influence of rat paw edema reaction.The Wistar rat, 180～220g, male and female half and half by the body weight layering, are divided into 5 groups of blanks, hydrocortisone, the large, medium and small dosage of baikal skullcap root composition, 12 every group at random.Each organizes rat by 10ml/kg volume gastric infusion, gives physiological saline, hydrocortisone 20mg/kg, baikal skullcap root composition fingerprint characteristic extract 30,60,120mg/kg respectively, and the 12h administration is 3 times at interval.30min after the last administration is injected in the subcutaneous inflammation that causes of the left back sufficient sole of the foot of rat with fresh albumen 0.1ml.Volumetric method is measured rat and is caused the volume that following position, scorching sufficient external malleolus highlight plane causes before the inflammation and causes scorching back 0.5,1.0,2.0,4.0 and 6.0h, calculating rat paw edema value.Experimental result sees Table four.
Table four pair egg white causes the influence (x ± s) of rat paw edema value
2.3 to the swollen influence that forms of rat granuloma.The Wistar rat, male, 135～165g by the body weight layering, is divided into 5 groups of blanks, hydrocortisone, the large, medium and small dosage of baikal skullcap root composition, 12 every group at random.Each organizes rat with 3% vetanarcol 30mg/kg intraperitoneal injection of anesthesia, aseptic condition cuts abdomen center skin down after the cropping, long incision 1cm, to the aseptic dry cotton balls of the subcutaneous implantation of bilateral inguinal region 10mg, sew up the incision, postoperative was subjected to the reagent thing, every day 1 time, continuous 7 days by 10ml/kg volume filling stomach the same day; Postoperative vetanarcol anesthetized rat on the 8th, cotton balls is taken out in operation, picks most fatty tissue, and 60 ℃ of oven dry postoperative cotton balls of weighing subtracts the raw cotton ball weight, represents that with mg/100g granuloma is heavy, calculates inflammation inhibiting rate (%).Experimental result sees Table five.
The swollen restraining effect that forms of table five pair rat granuloma (x ± s)
2.4 histamine is caused the influence that the rat skin capillary permeability increases reaction.The Wistar rat, male and female half and half, 180～220g by the body weight layering, is divided into 5 groups of blanks, hydrocortisone, the large, medium and small dosage of baikal skullcap root composition, 12 every group at random.Each organizes rat by 10ml/kg volume gastric infusion, and the 12h administration is 3 times at interval.60min after the last administration, each mouse back intradermal injection 0.01% histamine normal saline solution 0.1ml, tail vein injection 1% Evans Blue normal saline solution 0.4ml/100g immediately, take off cervical vertebra behind the 30min and put to death rat, diameter 1.5cm punch tool downcuts back indigo plant and dyes skin graft, shreds rearmounted 7: 3 acetone normal saline solution 5ml, 45 ℃ are soaked 96h until the blue completely dissolve of skin, the centrifugal 15min of 1500rpm gets supernatant liquor and measures the A620nm value, calculates and oozes out inhibiting rate (%).Experimental result sees Table six.
The restraining effect that the rat skin capillary permeability that causes table six pair histamine increases (x ± s)
3, result and conclusion
Experimental result shows, root of large-flowered skullcap privileged site composition p-Xylol causes mice auricle swelling, egg white and causes the swollen formation of rat paw edema, rat granuloma and histamine and cause the rat skin capillary permeability and increase and all have than the obvious suppression effect, but inflammation-inhibiting acute phase pathology and inflammation later stage reticular tissue generate.
Description of drawings
Fig. 1 refers to 1-2cm part under the 4-6cm near the ground of the root of large-flowered skullcap and the near-earth for root of large-flowered skullcap privileged site, and the synoptic diagram of root of large-flowered skullcap top branches and leaves.
Fig. 2 embodiment 1 extractive from specific part of skullcap color atlas.
Fig. 3 embodiment 2 extractive from specific part of skullcap color atlass.
Fig. 4 embodiment 3 extractive from specific part of skullcap color atlass.
Fig. 5 embodiment 4 extractive from specific part of skullcap color atlass.
Embodiment
For better understanding essence of the present invention, below with the preparation method of the explanation of example more specifically extractive from specific part of skullcap.
(1) root of large-flowered skullcap privileged site (1-2cm part under 4-6cm near the ground and the near-earth) is ground into meal, drops in the extractor, extracts secondary, adds the alcohol reflux 1.5 hours of 4 times of amounts 95% for the first time.Add for the second time the alcohol reflux 2 hours of 4 times of amounts 90%, filter.
(2) filtrate is concentrated into nothing alcohol flavor.
(3) with 30%NaOH solution concentrated solution pH value is transferred to pH9.5.
(4) leave standstill 1 hour, the centrifugal centrifugate that gets.
(5) when centrifugate temperature during, centrifugate pH value is transferred to pH1.5 with concentrated hydrochloric acid at 40 ℃, reheat to 80 ℃ insulation 20 minutes, filter throw out.
(6) will precipitate with 60 ℃ of hot water injections to neutral, vacuum-drying gets dry powder.
(7) after gained dry powder is pulverized, is sieved dry powder A1.
The root of large-flowered skullcap branches and leaves of (8) gathering autumn are ground into meal, drop in the extractor, extract secondary, add 8 times of amount 70% ethanol for the first time, refluxing extraction 2 hours.Add for the second time 4 times of amount 70% ethanol, refluxing extraction 1.5 hours is filtered; Filtrate is concentrated into about 20 Baumes; Vacuum-drying, after pulverizing, sieving dry powder C1.
Mixed to obtain dry powder D1 by dry powder A1 and dry powder C1 allotment, described D1 is extractive from specific part of skullcap.
(9) extractive from specific part of skullcap characteristic present: adopting HPLC (high performance liquid chromatography), under certain separation condition, is the correlation factor that standard substance calculate each less important flavones with external standard method or with the baicaline, and each peak is carried out quantitatively; Baicaline directly carries out quantitatively with the baicaline standard substance, and scutellarin directly carries out quantitatively with the scutellarin standard substance.
The feature of extractive from specific part of skullcap D1 sees Table eight and Fig. 2.
The feature of table eight, extractive from specific part of skullcap D1
Annotate: total less important flavones comprises described in the table: Norwogonin-7-Glucuronide; Oroxylin-7-Glucuronide; Wogonin-7-O-glucosiduronate; Scutellarin; Wogonin; Chrysin.
Embodiment 2
(1) root of large-flowered skullcap privileged site (1-2cm part under 4-6cm near the ground and the near-earth) is ground into meal, drops in the extractor, boils and carries secondary, and the poach that adds 6 times of amounts is for the first time carried 3 hours.Add for the second time 6 times of water gagings and boil and carry 2 hours, filter.
(2) with 40%NaOH solution concentrated solution pH value is transferred to pH9.
(4) leave standstill 4 hours, the centrifugal centrifugate that gets.
(5) when centrifugate temperature during, centrifugate pH value is transferred to pH2 with the vitriol oil at 40 ℃, reheat to 80 ℃ insulation 40 minutes, filter throw out.
(6) will precipitate with 80 ℃ of hot water wash to neutral, vacuum-drying gets dry powder.
(7) after gained dry powder is pulverized, is sieved B1.
The root of large-flowered skullcap branches and leaves of (8) gathering autumn are ground into meal, drop in the extractor, extract secondary, add 8 times of amount 70% ethanol for the first time, refluxing extraction 2 hours.Add for the second time 4 times of amount 70% ethanol, refluxing extraction 1.5 hours is filtered.Filtrate is concentrated into about 22 Baumes.Vacuum-drying, after pulverizing, sieving C2.
By dry powder B1 and dry powder C2 allocate dry powder E1, described E1 is extractive from specific part of skullcap.
The feature of extractive from specific part of skullcap E1 sees Table nine and Fig. 3.
The feature of table nine, root of large-flowered skullcap specific extraction thing E1
Annotate: total less important flavones comprises described in the table: Norwogonin-7-Glucuronide; Oroxylin-7-Glucuronide; Wogonin-7-O-glucosiduronate; Scutellarin; Wogonin; Chrysin.
(1) root of large-flowered skullcap privileged site (1-2cm part under 4-6cm near the ground and the near-earth) is ground into meal, drops in the extraction equipment, extracts secondary, adds the alcohol reflux 1.5 hours of 4 times of amounts 90% for the first time.Add for the second time the alcohol reflux 2 hours of 4 times of amounts 90%, filter.
(2) filtrate is concentrated into nothing alcohol flavor.
(3) with 30%KOH solution concentrated solution pH value is transferred to pH8.
(4) leave standstill 1 hour, the centrifugal centrifugate that gets.
(5) when centrifugate temperature during, with the vitriol oil centrifugate pH value is transferred to pH2, reheat to 80 ℃ insulation 30 minutes at 45 ℃.Filter throw out.
(6) will precipitate with 60 ℃ of hot water injections, vacuum-drying gets dry powder.
(7) after gained dry powder is pulverized, is sieved A2.
The root of large-flowered skullcap branches and leaves of (8) gathering autumn are ground into meal, drop in the extraction equipment, extract secondary, add the alcohol reflux 2 hours of 7 times of amounts 75% for the first time.Add for the second time the alcohol reflux 1 hour of 4 times of amounts 75%, filter, filtrate is concentrated into 22 Baumes.With medicinal extract vacuum-drying, after pulverizing, sieving C3.
By dry powder A2 and dry powder C2 allocate dry powder D2, described D2 is extractive from specific part of skullcap.
The feature of extractive from specific part of skullcap D2 sees Table ten and Fig. 4.
The feature of table ten, root of large-flowered skullcap specific extraction thing D2
Annotate: total less important flavones comprises described in the table: Norwogonin-7-Glucuronide; Oroxylin-7-Glucuronide: wogonin-7-O-glucosiduronate; Scutellarin; Wogonin; Chrysin.
(1) root of large-flowered skullcap privileged site (1-2cm part under 4-6cm near the ground and the near-earth) is ground into meal, drops in the extractor, boils and carries secondary, and the poach that adds 6 times of amounts is for the first time carried 3 hours.Add for the second time 6 times of water gagings and boil and carry 2 hours, filter.
(2) with 40%NaOH solution concentrated solution pH value is transferred to pH9.5.
(4) leave standstill 4 hours, the centrifugal centrifugate that gets.
(5) when centrifugate temperature during, centrifugate pH value is transferred to pH 2 with the vitriol oil at 40 ℃, reheat to 80 ℃ insulation 40 minutes, filter throw out.
(6) will precipitate with 80 ℃ of hot water wash to neutral, vacuum-drying gets dry powder.
(7) after gained dry powder is pulverized, is sieved B2.
The root of large-flowered skullcap branches and leaves of (8) gathering autumn are ground into meal, drop in the extractor, extract secondary, add 8 times of amount 80% ethanol for the first time, refluxing extraction 2 hours.Add for the second time 4 times of amount 80% ethanol, refluxing extraction 1.5 hours is filtered; With filtrate be concentrated into about 20 Baumes medicinal extract, vacuum-drying, after pulverizing, sieving C4.
By dry powder B2 and dry powder C4 allocate dry powder E2, described E2 is extractive from specific part of skullcap.
The feature of extractive from specific part of skullcap E2 sees Table 11 and Fig. 5.
The feature of table ten one, root of large-flowered skullcap specific extraction thing E2
Annotate: total less important flavones comprises described in the table: Norwogonin-7-Glucuronide; Oroxylin-7-Glucuronide; Wogonin-7-O-glucosiduronate; Scutellarin; Wogonin; Chrysin.
Get extractive from specific part of skullcap 100g of the present invention, mix, with 85% ethanol system softwood with 50g dextrin and Icing Sugar 20g, granulate 55-60 ℃ of vacuum-drying, the whole grain of 20 mesh sieves with 16 order nylon screens, select capsule shell for use No. 2, be filled to 1000 with Autocapsulefillingmachine or craft, polishing promptly.Every contains composition 100mg.This product has anti-inflammatory activity, becomes human oral every day 2-3 time, at every turn the 1-2 grain.
Get 1 part of extractive from specific part of skullcap of the present invention, 3 parts of tea-polyphenol, 10 parts of Icing Sugar, 2 parts in dextrin, be weight part, cross 80 mesh sieves, mix, add 8% starch slurry and make softwood, granulate 55-60 ℃ of vacuum-drying with 12 order nylon screens, the whole grain of 14 mesh sieves, packing promptly, every bag weight 6g.This granule has anti-inflammatory activity, becomes human oral every day 2-3 time, and each 1 wraps.
Prescription: 0.2 part of extractive from specific part of skullcap of the present invention, 15.0 parts of stearic acid, 1.0 parts of single stearic acid glycerine lipoproteins, 1.0 parts of white oils, 1.0 parts of hexadecanols, 10.0 parts of propylene glycol, 0.6 part in potassium hydroxide, 0.05 part in sodium hydroxide, by weight, essence, sanitas are an amount of, and adding water is 100 parts to gross weight.
Preparation: press amount difference weighing scutellariae,radix fingerprint characteristic extract, stearic acid, single stearic acid glycerine lipoprotein, white oil, hexadecanol and propylene glycol in the prescription, load weighted raw material is added in the 250ml beaker, water and alkali are weighed in another 250ml beaker of back adding.Be heated to 90 ℃ respectively, make material melting, dissolving evenly.The beaker of dress water keeps the 20min sterilization down at 90 ℃.Under agitation water is slowly joined in the grease then, continue to stir, when temperature is reduced to 50 ℃, add sanitas.After being cooled to 40 ℃, add essence, stir.Leave standstill, be cooled to room temperature.Adjust the pH of lotion, make it in the scope that requires.This vanishing cream has certain anti-inflammatory activity.
Claims (2)
1. prepare the production technique of extractive from specific part of skullcap, it is characterized in that:
The ethanol-extracted technology of root of large-flowered skullcap privileged site:
(1) root of large-flowered skullcap privileged site, it is 1-2cm part under the 4-6cm near the ground of the labiate root of large-flowered skullcap and the near-earth, be ground into meal, extract secondary, add for the first time 4-8 and doubly measure alcohol reflux 1.5-3 hour of 80-95%, add for the second time 2-4 and doubly measure alcohol reflux 1-2 hour of 80-95%, filter;
(2) filtrate is concentrated into nothing alcohol flavor;
(3) with 20-50%NaOH or KOH solution concentrated solution pH value is transferred to pH 7-9.5;
(4) leave standstill 1-4 hour, solution is collected in centrifugal or filtration;
(5) when solution temperature during at 40 ℃-50 ℃, with the concentrated hydrochloric acid or the vitriol oil centrifugate pH value is transferred to pH1.5-3, ℃ of-90 ℃ insulations of reheat to 75 30-40 minute are filtered or centrifugal, the collecting precipitation thing;
(6) will precipitate 60-80 ℃ of hot water wash of usefulness to neutral, the dry dry powder that gets;
(7) after gained dry powder is pulverized, is sieved dry powder A;
Root of large-flowered skullcap branches and leaves extraction process
(1) root of large-flowered skullcap branches and leaves that will gather autumn are ground into meal, drop in the extraction equipment, extract secondary, add 4-8 for the first time and doubly measure 70 one 80% alcohol reflux 1-2 hour.Add for the second time 2-4 and doubly measure alcohol reflux 1-1.5 hour of 70-80%, filter;
(2) filtrate is concentrated into the 15-25 Baume;
(3) dry, pulverize, sieve, after dry powder C;
Mixed to obtain dry powder D by A and C allotment, described dry powder D is extractive from specific part of skullcap.
2. prepare the production technique of extractive from specific part of skullcap, it is characterized in that:
The water extraction process of root of large-flowered skullcap privileged site:
(1) root of large-flowered skullcap privileged site, promptly 1-2cm part under the 4-6cm near the ground of the labiate root of large-flowered skullcap and the near-earth is ground into meal, extract secondary, add the poach that 6-10 doubly measures for the first time and carry 1.5-3 hour, add 3-6 times of water gaging for the second time and boil and carry 1-2 hour, extracting solution is collected in filtration or centrifugal;
(2) extracting solution is inserted the 1/2-1/3 that is concentrated to original volume in the thickener;
(3) with 20-50%NaOH or KOH solution concentrated solution pH value is transferred to pH 7-9.5;
(4) leave standstill 1-4 hour, solution is collected in centrifugal or filtration;
(5) when solution temperature during at 40 ℃-50 ℃, with concentrated hydrochloric acid or concentrated sulfuric acid solution centrifugate pH value is transferred to pH 1.5-3, ℃ of-90 ℃ insulations of reheat to 75 20-40 minute are filtered or centrifugal, the collecting precipitation thing;
(6) will precipitate with 40 ℃ of-80 ℃ of hot water wash to neutral dry dry powder;
(7) after gained dry powder is pulverized, is sieved dry powder B;
Root of large-flowered skullcap branches and leaves extraction process
(1) root of large-flowered skullcap branches and leaves that will gather autumn are ground into meal, drop in the extraction equipment, extract secondary, add 4-8 for the first time and doubly measure alcohol reflux 1-2 hour of 70-80%.Add for the second time 2-4 and doubly measure alcohol reflux 1-1.5 hour of 70-80%, filter;
(2) filtrate is concentrated into the 15-25 Baume;
(3) dry, pulverize, sieve, after dry powder C;
Mixed to obtain dry powder E by B and C allotment, described dry powder E also is an extractive from specific part of skullcap.
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101003529B (en) * | 2007-01-17 | 2010-05-19 | 河南中医学院 | Method for separating component in flavonoid from root of large-flowered skullcap |
| CN104610401B (en) * | 2015-02-25 | 2017-03-15 | 山东省中医药研究院 | A kind of method for extracting baicalin, baicalin and wogonin from Radix Scutellariae simultaneously |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260189A (en) * | 1998-12-31 | 2000-07-19 | 承德医学院中药研究所 | Application of radix scutellariae stem and leaf to pharmaceutical industry |
| CN1383818A (en) * | 2002-01-05 | 2002-12-11 | 承德医学院中药研究所 | Application of skullcap stem and leaf general flavone and wild baicalin in preparing dementia resisting medicine |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1260189A (en) * | 1998-12-31 | 2000-07-19 | 承德医学院中药研究所 | Application of radix scutellariae stem and leaf to pharmaceutical industry |
| CN1383818A (en) * | 2002-01-05 | 2002-12-11 | 承德医学院中药研究所 | Application of skullcap stem and leaf general flavone and wild baicalin in preparing dementia resisting medicine |
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| 中草药. 黎万寿，107－108，黄芩苷提取工艺研究. 2000 * |
| 内蒙古大学学报（自然科学版）. 唐海燕 等，355－357，黄芩中黄芩甙的提取工艺研究. 2004 * |
| 承德医学院学报. 孟艳彬 等，258－259，不同生长期黄芩茎叶中总黄酮及野黄芩苷的含量测定. 2003 内蒙古大学学报（自然科学版）. 唐海燕 等，355－357，黄芩中黄芩甙的提取工艺研究. 2004 深圳中西医结合杂志. 胡应权，21－22，黄芩甙提取工艺的改进. 1999 中草药. 黎万寿，107－108，黄芩苷提取工艺研究. 2000 |
| 承德医学院学报. 孟艳彬 等，258－259，不同生长期黄芩茎叶中总黄酮及野黄芩苷的含量测定. 2003 * |
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