CN102389456A - Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A - Google Patents
Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A Download PDFInfo
- Publication number
- CN102389456A CN102389456A CN2011103871284A CN201110387128A CN102389456A CN 102389456 A CN102389456 A CN 102389456A CN 2011103871284 A CN2011103871284 A CN 2011103871284A CN 201110387128 A CN201110387128 A CN 201110387128A CN 102389456 A CN102389456 A CN 102389456A
- Authority
- CN
- China
- Prior art keywords
- rabdosia japonica
- extract
- diterpene
- extraction
- glaucocalyxin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention belongs to the field of traditional Chinese medicine extraction and discloses a method for preparing isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A. The method provided by the invention comprises extraction, elution and decolouring steps and specifically comprises the following steps of: crushing the upper portion of the medicinal material isodon japonica var.galaucocalyx vegetable plot, refluxing by using an ethanol aqueous solution at normal pressure to extract for 1-3 times, merging extracts, reducing pressure and recovering a solvent to obtain a condensed extract; loading the condensed extract into a processed macroporous adsorption resin, eluting pigment by 50 column volumes of water, eluting impurities by 25-time column of 30% ethanol, eluting by 30 column volumes of 60% ethanol, collecting the eluted portion, and recovering a solvent to obtain an isodon japonica var.galaucocalyx diterpenoid extract product; dissolving the isodon japonica var.galaucocalyx diterpenoid extract product into ethanol, adding active carbon for decolouring, recovering a solvent, drying to obtain the isodon japonica var.galaucocalyx total diterpenoids, and crystallizing ethanol to prepare Glaucocalyxin A. By the adoption of the preparation method provided by the invention, the content of the isodon japonica var.galaucocalyx total diterpenoids is high, the purity of Glaucocalyxin A is more than 90%, and the yield is over 7%.
Description
Technical field
The invention belongs to the Chinese medicine extraction field, relating to a kind of is the method for raw material preparing Rabdosia japonica total diterpene or glaucocalyxin with the medical material Rabdosia japonica.
Background technology
Rabdosia japonica (
Isodon japonicaVar glaucocalyx (Maxim) Hara) is Labiatae Rabdosia plant, extensively is distributed in the northeast of China, North China, areas such as East China; Have be good for the stomach, heat-clearing and toxic substances removing, invigorate blood circulation, the anti-inflammation isoreactivity, be used to treat gastritis, abdominal distention, hepatitis initial stage, cold, fever, mastitis, arthralgia etc.Rabdosia japonica mainly contains glaucocalyxin, Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element, glaucocalyxin F, glaucocalyxin X; Deng mapping-Kaurane diterpine (referring to Zhao Bao Xiang; Et al. Two new diterpenoids from Rabdosia japonica var. glaucocalyx. Chinese Chemical Letters. 2008,19:852, Cao Luye etc.; The Rabdosia japonica progress; Yunnan Chinese medicine magazine, 2004,25 (3): 42.).Diterpenes composition in the Rabdosia japonica is its main active substances, and the rabbit platelet that glaucocalyxin can suppress calcimycin and stimulate generates platelet activating factor, and the rabbit platelet thromboxane A2 that can suppress arachidonic acid-induction generates; And the PGE2 that raises simultaneously, can significantly suppress ADP, AA; Inductive rabbit platelet such as PAF is assembled, and cAMP level in the remarkable increased platelets counts (referring to: Zhang B, Long K. Effects of glaucocalyxin A on aggtegation and cAMP levels of rabbit platelets in vitro. Acta Pharmacologica Sinica 1993; 14 (4): 347.) glaucocalyxin has certain inhibitory action to ehrlich carcinoma, in the body S180 solid tumor suppression ratio is reached 30.4% (10mg/kg, 7 days); (referring to: Zhang Shuxiang etc.; Glaucocalyxin external to DNA, the biosynthetic influence of RNA and protein, pharmacy Intelligence Newsletter; 1990,8 (3): 238.).Glaucocalyxin, Glaucocalyxin B, Glaucocalyxin D, blue calyx penta element, the own element of blue calyx have stronger cytotoxic activity to A549 (human lung carcinoma cell), LOVO (people's colon-cancer cell), 6T-CEM (human T cell leukemia cell), HL-60 (human leukemia cell); Can be used for preparing cancer therapy drug (referring to Chen Haisheng etc.; The application of diterpene-kind compound in the preparation cancer therapy drug in the Rabdosia japonica, the patent No. is 200910044882.0 Chinese invention patent); Glaucocalyxin B, blue calyx third element, Glaucocalyxin D, blue calyx penta element and the own element of blue calyx have carried out anti-hepatitis B surface antigen and HBcAg test; The result finds; They have significant anti-hepatitis B activity; Can be used for preparing the medicine (referring to Chen Haisheng etc., the application of diterpene-kind compound in the preparation anti-hepatitis virus medicament in the Rabdosia japonica, the patent No. is 200910044883.5 Chinese invention patent) of anti-hepatitis virus.
In the prior art, the method for from the medical material Rabdosia japonica, extracting glaucocalyxin is complex steps not only, and yield is on the low side; Generally be lower than 10%; And because employing has toxic solvent to organism, residual toxic solvent does not meet the pharmacopeia requirement, specifically may further comprise the steps:
The purity that adopts technique scheme gained glaucocalyxin is generally more than 90%; But yield is generally 7% ~ 9%, and has used deleterious solvent in the process, chloroform, methanol; And residual toxic solvent can influence the use of glaucocalyxin as medicine, does not meet the pharmacopeia requirement.
Publication number is the method for distilling that the Chinese invention patent application of CN 101914002 discloses a kind of glaucocalyxin, and extraction, silica gel column chromatography eluting pigment and impurity, purification step specifically may further comprise the steps:
Wherein, said eluent A is the mixture of petroleum ether and ethyl acetate, and by volume, Shi You Mi ︰ ethyl acetate=8 ︰ 1; Said eluent B is the mixture of petroleum ether and ethyl acetate, and by volume, Shi You Mi ︰ ethyl acetate=4 ︰ 1; Said eluent C is the mixture of petroleum ether and ethyl acetate, and by volume, Shi You Mi ︰ ethyl acetate=2 ︰ 1;
The purity of the glaucocalyxin that obtains through said method is 95 ~ 100%, and purity is high, is suitable for preparing various dosage forms; Yield is more than 10%, and yield is high, and the repeatability of method is strong; Measure according to organic solvent residual assay method in 2010 editions pharmacopeia appendix; Organic solvent-free is residual, and the organic solvent avirulence that is suitable for, and meets 2010 editions pharmacopeia requirements.
Macroporous adsorbent resin be one type not with the porous cross linked polymer of ion-exchange group, have the polymeric sorbent of macroporous structure.Physicochemical properties are stable, and specific surface area is big, and adsorption capacity is big, and selectivity is good; Adsorption rate is fast, and desorption condition is gentle, and is good to the Organic substance selectivity, the influence that not existed by inorganic salts and other strong ions, low molecule; Help absorption, wide in variety, the adsorbable multiple organic compound of different cultivars; Fluid resistance is less, and decoloring ability is high, and Regeneration Treatment is convenient, life cycle is long, be suitable for formation closed cycle, cost saving; Also can reduce the moisture absorption of product simultaneously, effectively remove heavy metal, solve the difficult problem of Chinese medicine heavy metals exceeding standard.Be mainly used in the separation and purification of Chinese herbal medicine at present, as to the medical material The pretreatment, to the separation and purification of single medicinal material extract and the separation and purification of centering recurrence due to taking drug formula extraction, the realization suitability for industrialized production that has has vast potential for future development.(referring to: Liu Shuaiying etc., the purification with macroreticular resin of peoniflorin research in the Radix Paeoniae Rubra, Chinese herbal medicine, 2010,41 (9): 1480.)
Silica gel is not re-usable column packing, Chemical Decomposition purification glaucocalyxin, and the silica gel consumption is big, and cost is higher, and macroporous resin is reusable column chromatography filler, and can suitability for industrialized production, can reduce cost greatly.
Glaucocalyxin and diterpene have significant pharmacologically active in the Rabdosia japonica, but do not see that the macroporous resin of bibliographical information glaucocalyxin and total diterpene method for preparing is arranged, and are necessary to carry out preparation technology's investigation.
Summary of the invention
Goal of the invention of the present invention provides a kind of method of extracting the Rabdosia japonica total diterpene.
For reaching the foregoing invention purpose, the technical scheme that the present invention adopts is: a kind of method of extracting the Rabdosia japonica total diterpene, comprise extraction, eluting, decolouring step, wherein,
Said extraction step is: medical material Rabdosia japonica aerial parts is pulverized, used the ethanol water reflux, extract,, obtain extracting solution, decompression and solvent recovery gets concentrated extracting solution, contains crude drug 0.5-1g in said every milliliter of concentrated extracting solution;
Said elution step is: the gained concentrated extracting solution is crossed macroporous adsorbent resin; With 50 times of column volume water elution pigments; 25 times of column volume 30% ethanol water eluting impurity, 30 times of column volume 60% ethanol water eluting are collected this eluting part; Reclaim solvent, obtain the Rabdosia japonica diterpene extract.
Said decolouring step is: the Rabdosia japonica diterpene extract is dissolved in the ethanol, adds activated carbon decolorizing then, reclaim solvent, drying obtains the Rabdosia japonica total diterpene.
In the technique scheme, the decolouring step is in order to remove pigment such as chlorophyll, to improve yield.
In the technique scheme, use the method for ethanol water reflux, extract, to be: under normal pressure, with percentage by volume 55-70% ethanol water reflux, extract, 1 ~ 3 time, reflux, extract, is 1 ~ 3 hour at every turn, merge extractive liquid.
In the technique scheme; Said macroporous adsorbent resin is the macroporous adsorbent resin of nonpolar or low pole; Comprise AB-8 type, D101 type, HPD-100, HPD-200A, HPD-200B, HPD-300, HPD-700, HPD-722 type, handle by prior art before use.
In the technique scheme, in the elution step, the macroporous resin quality: quality of medicinal material is 1: 1.0-2.7.
In the technique scheme, in the elution step, the macroporous resin column diameter: the post height is 1: 4-9.
In the technique scheme, in the elution step, the macroporous resin quality: column volume is 1mg: 1mL.
In the technique scheme, in the decolouring step, the quality of Rabdosia japonica diterpene extract and alcoholic acid volume ratio are 1: 250-300.
In the technique scheme, in the decolouring step, the quality of active carbon is 1～5% of a Rabdosia japonica diterpene extract quality.
Further in the technical scheme, get above-mentioned Rabdosia japonica total diterpene, alcohol crystal prepares glaucocalyxin, and purity is more than 90%, and yield is more than 7%.
Therefore, the present invention requires a kind of method of extracting glaucocalyxin of protection simultaneously again.
The glaucocalyxin and the total diterpene that adopt method for preparing according to the invention to prepare can be used to process dosage forms such as tablet, capsule, pill, are applied to compound recipe or single preparations of ephedrine.
Because the technique scheme utilization, the present invention compared with prior art has advantage:
The Rabdosia japonica total diterpene content that adopts method for preparing according to the invention to obtain is high, and glaucocalyxin purity is more than 90%, and yield is more than 7%, and this technological operation is simple, and is pollution-free, but suitability for industrialized production.
Description of drawings
Fig. 1 is the purity analysis chromatogram of glaucocalyxin among the embodiment one;
Fig. 2 is the purity analysis chromatogram of glaucocalyxin among the embodiment two;
Fig. 3 is the purity analysis chromatogram of glaucocalyxin among the embodiment three;
Fig. 4 is the hydrogen analysis of spectrum figure of glaucocalyxin among the embodiment five;
Fig. 5 is the carbon analysis of spectrum figure of glaucocalyxin among the embodiment five.
The specific embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is further described:
Embodiment one:
Get Rabdosia japonica aerial parts 100 gram, through pulverizing, in the atmospheric pressure reflux extraction element, with volume fraction 55% ethanol water reflux, extract, 2 times, reflux, extract, is 2 hours at every turn, merge extractive liquid,, and decompression and solvent recovery is to 200 milliliters; Through 80 gram HPD-100 type macroporous adsorbent resins (macroporous resin column is high 13 centimetres for 80 milliliters of column volumes, 2.8 centimetres of macroporous resin column diameters); With 50 times of water elution pigments; 25 times of volume fraction 30% ethanol water eluting impurity, 30 times of 60% volume fraction ethanol water eluting collected this eluting part; Reclaim solvent, obtain Rabdosia japonica diterpene extract 1.65 grams.The Rabdosia japonica diterpene extract is dissolved in 430 milliliters of ethanol, adds 0.08 gram activated carbon decolorizing element, drying to this solution; Obtain Rabdosia japonica total diterpene 1.08 grams, 41.3%, 2 milliliter of alcohol crystal of content; Get glaucocalyxin 0.02 gram, its purity is 95.6%, yield 8%.
In the technique scheme, the glaucocalyxin method for detecting purity is: 2 milligrams of glaucocalyxin, and dissolve with methanol standardize solution to 10 milliliter, chromatographic column is Sweden Kromasil C18 (4.6 mm * 250 mm, 5 μ m); Mobile phase: methanol: 0.1% phosphoric acid (70:30); Flow velocity: 1 mL/min; Detect wavelength: 231 nm; Sample size: 20 μ L; Column temperature: 30 ℃, detect gained figure shown in liquid chromatograph Fig. 1, data see the following form:
| Peak (Peak) | Retention time | Area | Highly | Area % | Tailing |
| 1 | 2.726 | 114372 | 7462 | 2.098 | 1.165 |
| 2 | 3.613 | 105597 | 4615 | 1.937 | 0.959 |
| 3 | 5.127 | 5209313 | 423492 | 95.573 | 1.048 |
| 4 | 8.247 | 21349 | 1323 | 0.392 | 0.735 |
| Summation | ? | 5450631 | 436892 | 100.000 | ? |
Embodiment two:
Get Rabdosia japonica aerial parts 1000 gram, through pulverizing, in the atmospheric pressure reflux extraction element, with 60% alcohol reflux 2 times; Each reflux, extract, 3 hours, merge extractive liquid,, decompression and solvent recovery is to 1500 milliliters; Through 600 gram D101 type macroporous adsorbent resins (macroporous resin column is high 26 centimetres for 600 milliliters of column volumes, 5.5 centimetres of macroporous resin column diameters); With 50 times of water elution pigments, 25 times of 30% ethanol elution impurity, 30 times of 60% ethanol elution; Collect this eluting part, reclaim solvent, obtain Rabdosia japonica diterpene extract 16.72 grams.The Rabdosia japonica diterpene extract is dissolved in 4190 milliliters of ethanol, adds 0.60 gram activated carbon decolorizing element, drying to this solution; Obtain Rabdosia japonica total diterpene 10.16 grams, 42.0%, 35 milliliter of alcohol crystal of content; Get glaucocalyxin 0.25 gram, its purity is 95.0%, yield 9%.
In the technique scheme, the glaucocalyxin method for detecting purity is: 2 milligrams of glaucocalyxin, and dissolve with methanol standardize solution to 10 milliliter, chromatographic column is Sweden Kromasil C18 (4.6 mm * 250 mm, 5 μ m); Mobile phase: methanol: 0.1% phosphoric acid (70:30); Flow velocity: 1 mL/min; Detect wavelength: 231 nm; Sample size: 20 μ L; Column temperature: 30 ℃, detect gained figure shown in liquid chromatograph Fig. 2, data see the following form:
| Peak (Peak) | Retention time | Area | Highly | Area % | Tailing |
| 1 | 2.688 | 137605 | 9202 | 3.026 | 1.425 |
| 2 | 3.526 | 76711 | 4157 | 1.687 | 1.028 |
| 3 | 4.988 | 4320503 | 389744 | 95.018 | 1.128 |
| 4 | 6.616 | 12219 | 1312 | 0.269 | 1.062 |
| Summation | ? | 4547037 | 404415 | 100.000 | ? |
Embodiment three:
Get Rabdosia japonica aerial parts 10000 gram, through pulverizing, in the atmospheric pressure reflux extraction element, with 70% alcohol reflux 2 times; Each reflux, extract, 2 hours, merge extractive liquid,, decompression and solvent recovery is to 16000 milliliters; Through 6000 gram AB-8 type macroporous adsorbent resins (macroporous resin column is high 77 centimetres for 6000 milliliters of column volumes, 10 centimetres of macroporous resin column diameters); With 50 times of water elution pigments, 25 times of 30% ethanol elution impurity, 30 times of 60% ethanol elution; Collect this eluting part, reclaim solvent, obtain Rabdosia japonica diterpene extract 170.20 grams.The Rabdosia japonica diterpene extract is dissolved in 4190 milliliters of ethanol, adds 5.98 gram activated carbon decolorizings elements, drying to this solution; Obtain Rabdosia japonica total diterpene 121.83 grams, 43.2%, 50 milliliter of alcohol crystal of content; Get glaucocalyxin 2.48 grams, its purity is 96.0%, yield 8%.
In the technique scheme, the glaucocalyxin method for detecting purity is: 2 milligrams of glaucocalyxin, and dissolve with methanol standardize solution to 10 milliliter, chromatographic column is Sweden Kromasil C18 (4.6 mm * 250 mm, 5 μ m); Mobile phase: methanol: 0.1% phosphoric acid (70:30); Flow velocity: 1 mL/min; Detect wavelength: 231 nm; Sample size: 20 μ L; Column temperature: 30 ℃, detect gained figure shown in liquid chromatograph Fig. 3, data see the following form:
| Peak (Peak) | Retention time | Area | Highly | Area | Tailing factor | |
| 1 | 2.648 | 92322 | 5999 | 1.810 | 1.159 | |
| 2 | 3.440 | 97539 | 4940 | 1.913 | 1.022 | |
| 3 | 4.833 | 4897540 | 415590 | 96.035 | 1.040 | |
| 4 | 6.404 | 12360 | 1286 | 0.242 | 1.018 | |
| Summation | ? | 5099761 | 427815 | 100.000 | ? |
Embodiment four: diterpene content in the Rabdosia japonica
Get purity and be 6 parts of 96.6% glaucocalyxin, dissolve with methanol, standardize solution are to 25ml, and 230nm surveys absorbance as absorbing wavelength.With the glaucocalyxin quality is abscissa, and absorbance is a vertical coordinate, tries to achieve regression equation Y=0.001X+1.9856, R
2=0.9997 explanation is linear good, and glaucocalyxin is good in 4.376-21.996 mg scope internal linear relation.
Get Rabdosia japonica total diterpene 0.25 gram respectively, dissolve with methanol, standardize solution to 250 milliliter under the 230nm wavelength, is surveyed absorbance, does parallel sample three times, calculates the average content of Rabdosia japonica total diterpene.(list of references: the assay of total diterpene in the Rabdosia rubescens, but treasure etc., the time precious traditional Chinese medical science traditional Chinese medicines, 2010,21 (4): 828-829.)
| Sequence number | Rabdosia japonica total diterpene quality (gram) | Rabdosia japonica total diterpene |
| 1 | 1.08 | 41.3 |
| 2 | 10.16 | 42.0 |
| 3 | 121.83 | 43.2 |
Embodiment five:
The glaucocalyxin structure is identified: colourless block crystallization (ethanol), mp 220.0-222.0 ℃; Be soluble in organic solvents such as chloroform, ethyl acetate, acetone, methanol.
Simultaneously embodiment gained glaucocalyxin is carried out hydrogen spectrum and carbon analysis of spectrum, the result is referring to Fig. 4,5, and concrete data are as follows:
1H?NMR?(400MHz,?DMSO-
d 6)?δ：6.00?and?5.46?(each?1H,?brs,?17-H
a/b)，4.75?(1H,brs,?H-14α)，4.09?(1H,?m,?7β-H)，3.00?(1H,?brs,?13α-H)，1.08?(3H,?s)，1.04(3H,?s)，1.02?(3H,?s)。
13C?NMR?(100MHz,?DMSO-
d 6)?δ：37.9?(1-C)，33.9?(2-C)，216.5?(3-C)，46.5?(4-C)，50.6?(5-C)，30.9?(6-C)，73.0?(7-C)，60.7?(8-C)，52.8?(9-C)，38.6?(10-C)，18.1?(11-C)，30.3?(12-C)，46.1?(13-C)，74.6?(14-C)，207.0?(15-C)，148.8?(16-C)，116.9?(17-C)，27.4?(18-C)，21.1?(19-C)，18.1?(20-C)。POP data and document (Kim Yong Il etc., Rabdosia japonica root chemical constitution study, CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2000,25 (11): 38-39.) unanimity is accredited as glaucocalyxin.
Claims (10)
1. a method of extracting the Rabdosia japonica total diterpene comprises extraction, eluting, decolouring step, it is characterized in that:
Said extraction step is: medical material Rabdosia japonica aerial parts is pulverized, used the ethanol water reflux, extract,, obtain extracting solution, decompression and solvent recovery gets concentrated extracting solution, contains crude drug 0.5-1g in every milliliter of concentrated extracting solution;
Said elution step is: the gained concentrated extracting solution is crossed macroporous adsorbent resin; With 50 times of column volume water elution pigments; The concentration of 25 times of column volumes is percentage by volume 30% ethanol water eluting impurity, and the concentration of 30 times of column volumes is percentage by volume 60% ethanol water eluting, collects this eluting part; Reclaim solvent, obtain the Rabdosia japonica diterpene extract;
Said decolouring step is: the Rabdosia japonica diterpene extract is dissolved in the ethanol, adds activated carbon decolorizing then, reclaim solvent, drying obtains the Rabdosia japonica total diterpene.
2. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene; It is characterized in that, use the method for ethanol water reflux, extract, to be: under normal pressure, with percentage by volume 55-70% ethanol water reflux, extract, 1 ~ 3 time; Each reflux, extract, 1 ~ 3 hour, merge extractive liquid.
3. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that said macroporous adsorbent resin is the macroporous adsorbent resin of nonpolar or low pole.
4. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that said macroporous adsorbent resin comprises AB-8 type, D101 type, HPD-100, HPD-200A, HPD-200B, HPD-300, HPD-700, HPD-722 type.
5. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that in the elution step, the macroporous resin quality: quality of medicinal material is 1: 1.0-2.7.
6. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that in the elution step, the macroporous resin column diameter: the post height is 1: 4-9.
7. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that in the elution step, the macroporous resin quality: column volume is 1mg: 1mL.
8. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that in the decolouring step, the quality of Rabdosia japonica diterpene extract and alcoholic acid volume ratio are 1: 250-300.
9. according to the method for the said extraction Rabdosia japonica of claim 1 total diterpene, it is characterized in that in the decolouring step, the quality of active carbon is 1～5% of a Rabdosia japonica diterpene extract quality.
10. a method of extracting glaucocalyxin is characterized in that, adopts the method for the said extraction Rabdosia japonica of claim 1 total diterpene to prepare the Rabdosia japonica total diterpene, and alcohol crystal prepares glaucocalyxin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103871284A CN102389456A (en) | 2011-11-29 | 2011-11-29 | Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103871284A CN102389456A (en) | 2011-11-29 | 2011-11-29 | Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102389456A true CN102389456A (en) | 2012-03-28 |
Family
ID=45856921
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103871284A Pending CN102389456A (en) | 2011-11-29 | 2011-11-29 | Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102389456A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103405497A (en) * | 2013-04-08 | 2013-11-27 | 河南中医学院 | Preparation method of isodon excisoides total diterpenoid extractive |
| CN103989740A (en) * | 2014-05-04 | 2014-08-20 | 苏州大学 | Application of rabdosia japonica in preparing anti-acute lung injury drugs |
| CN104069145A (en) * | 2014-06-04 | 2014-10-01 | 苏州大学 | Application of lindley eupatorium herb in preparing anti-hepatitis B virus medicaments |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101914002A (en) * | 2010-08-27 | 2010-12-15 | 苏州大学 | Method for extracting glaucocalyxin A |
| CN101940615A (en) * | 2010-08-25 | 2011-01-12 | 吉林天药药物研发有限公司 | New preparation method of Isodon excisa total diterpene |
-
2011
- 2011-11-29 CN CN2011103871284A patent/CN102389456A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101940615A (en) * | 2010-08-25 | 2011-01-12 | 吉林天药药物研发有限公司 | New preparation method of Isodon excisa total diterpene |
| CN101914002A (en) * | 2010-08-27 | 2010-12-15 | 苏州大学 | Method for extracting glaucocalyxin A |
Non-Patent Citations (4)
| Title |
|---|
| 林朝展等: "大孔树脂富集纯化狭基线纹香茶菜总三萜酸工艺研究", 《中成药》 * |
| 沈晓丹等: "蓝萼香茶菜中蓝萼甲素提取工艺研究", 《抗感染药学》 * |
| 王雪: "《尾叶香茶菜萜类成分的研究》", 《中国优秀硕士学位论文集》 * |
| 聂仁强: "《大孔树脂在中药提取工艺中的应用》", 《基层中药杂志》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103405497A (en) * | 2013-04-08 | 2013-11-27 | 河南中医学院 | Preparation method of isodon excisoides total diterpenoid extractive |
| CN103989740A (en) * | 2014-05-04 | 2014-08-20 | 苏州大学 | Application of rabdosia japonica in preparing anti-acute lung injury drugs |
| CN103989740B (en) * | 2014-05-04 | 2017-06-06 | 苏州大学 | Application of the rabdosia japonica in resisting acute lung injury medicine is prepared |
| CN104069145A (en) * | 2014-06-04 | 2014-10-01 | 苏州大学 | Application of lindley eupatorium herb in preparing anti-hepatitis B virus medicaments |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102976909B (en) | Method for extracting and purifying 6-gingerol from ginger | |
| CN103304613B (en) | A kind of method of separation and purification 4 kinds of ucleosides chemical compositions from Snakegourd Peel | |
| CN105294623B (en) | A kind of Sesquiterpene lactones compound, its preparation method and application | |
| CN101921277B (en) | Method for simultaneously preparing vasicine and vasicinone from peganum harmala | |
| CN109879919B (en) | Method for separating and preparing three flavonoid glycosides from spina date seeds | |
| CN103113433B (en) | A kind of method extracting Oleuropein from Syringa pubescens | |
| CN101348474A (en) | Method for preparing salvianolic acid B and tanshinol from Salvia miltiorrhiza stem | |
| CN103180334B (en) | Prepare the method for lactone glucoside of Radix Paeoniae and peoniflorin | |
| CN110092767A (en) | A method of Sync enrichment purification of paclitaxel and 10-DAB III from Chinese yew | |
| CN102389456A (en) | Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A | |
| CN103665079A (en) | Separation and purification method of pachymic acid monomer | |
| CN103304490A (en) | Method for separating and purifying five purine and pyrimidine bases from trichosanthes bark | |
| CN101084967A (en) | Extracting and purifying technology for safflower flavonoids | |
| CN113264974A (en) | Preparation of type B cardiac glycoside and anti-angiogenesis application thereof | |
| CN106496292A (en) | A kind of method for preparing 6 iridoid glycoside constituents from Fructus Gardeniae simultaneously | |
| CN105175426B (en) | A kind of method of the extraction purification Bergenin from treebine stem | |
| CN101531721B (en) | Industrial preparation method for triterpenoid saponin monomer | |
| CN106674312A (en) | Separation and purification method for high-purity monomer sweroside series components | |
| CN104027403B (en) | A kind of preparation method of Radix Polygalae sugar ester effective site | |
| Hou et al. | Preparative purification of corilagin from Phyllanthus by combining ionic liquid extraction, prep-HPLC, and precipitation | |
| CN107721857A (en) | A kind of method that high-purity chlorogenic acid is prepared from Gynura procumbens (Lour.) Merr | |
| CN110240585B (en) | Preparation method of agilawood tetraol | |
| CN101940615A (en) | New preparation method of Isodon excisa total diterpene | |
| CN111675741A (en) | Separation method for simultaneously obtaining four kinds of epimedium rare flavone by using preparative liquid phase method | |
| CN107074798B (en) | Method for extracting phytoxin from rhodiola rosea |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20120328 |