CN106543246A - The separating and extracting process of gentiopicrin in Rhizoma Picrorhizae - Google Patents
The separating and extracting process of gentiopicrin in Rhizoma Picrorhizae Download PDFInfo
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- CN106543246A CN106543246A CN201610820891.4A CN201610820891A CN106543246A CN 106543246 A CN106543246 A CN 106543246A CN 201610820891 A CN201610820891 A CN 201610820891A CN 106543246 A CN106543246 A CN 106543246A
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- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
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- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C—CHEMISTRY; METALLURGY
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- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
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- C07H1/08—Separation; Purification from natural products
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Abstract
The invention belongs to chemical technology field, the separating and extracting process of gentiopicrin in specifically related to a kind of Rhizoma Picrorhizae, the method for specifically employing extraction, macroporous resin column chromatography and silica gel column chromatography, gentiopicrin is enable individually to be eluted from silica gel chromatographic column by substantial amounts of, improve the extracted amount of gentiopicrin, the gentiopicrin purity for finally giving reaches 98.7～99.3%, substantially increases the purity of gentiopicrin.Method of the present invention applied range, convenient and swift, low cost, simple to operate, fractional dose are big, are adapted to large-scale promotion application.
Description
Technical field
The invention belongs to chemical technology field, and in particular to the separation and Extraction side of gentiopicrin in a kind of Rhizoma Picrorhizae
Method.
Background technology
Rhizoma Picrorhizae also known as false Rhizoma Picrorhizae, are the dry rhizome of Scrophulariaceae Picrorrhiza herbaceos perennial, bitter in the mouth,
It is cold in nature, it is important clearind deficient heat medical material, the effects such as with reducing the asthenic fever, the infantile malnutrition with fever that disappears, heat clearing and damp drying, eliminating fire and detoxication, can be used for hectic fever due to YIN-deficiency
Consumptive fever, jaundice, cold and hot let out the diseases such as dysentery, infantile malnutrition, spontaneous perspiration, night sweat, hemorrhoid complicated by anal fistula, sore swells.Research shows, Radix Gentianae in Rhizoma Picrorhizae
The content of bitter glycosides is higher.Gentiopicrin have antiinflammatory, analgesia, liver protection, function of gallbladder promoting etc. act on, can be used for treat rheumatic arthralgia,
The diseases such as tuberculosis hectic fever, children's infantile malnutrition with fever, icterohepatitises, dysuria.
At present, gentiopicrin process for separation and purification mainly has two kinds：One kind uses Flavonoids by Macroporous Adsorption Resin, the method to separate
Amount is larger, but purity is not high enough；Another kind adopts high-speed counter-current chromatograph, and the method applied sample amount is little, is not suitable for large-tonnage product system
It is standby to use, and instrument is costly, is restricted during use.
The content of the invention
In view of this, present invention aim at providing a kind of separating and extracting process of 6-gingerol in Rhizoma Zingiberis Recenss.The method is obtained
Gentiopicrin purity it is high, applied range, convenient and swift, low cost, simple to operate, fractional dose are big, are adapted to large-scale promotion
Using.
For achieving the above object, the technical scheme is that：
In Rhizoma Picrorhizae, the separating and extracting process of gentiopicrin, specifically includes following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol extraction of 3.88～4.05 times of amounts of its quality；
B. extracting solution obtained by step A is concentrated, the purified water of equal volume amounts is added in the methanol solution after concentration, placed
Overnight, methanol is flung to, the solution for flinging to methanol is extracted with normal hexane, ethyl acetate, n-butyl alcohol successively respectively；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 20～60 mesh, with water, volume fraction is successively
10% ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, eluting
4 times for chromatographic column retention volume of volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.45～1.52
The column chromatography silica gel of times extractum quality, stirs, flings to solvent flashing, pulverize and sieve, be added to containing extractum quality 13.9
On the silica gel chromatographic column of～15.7 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 7：3 solution is eluting solvent, carries out chromatographic isolation to column chromatography,
Control is done using thin layer chromatography tracing detection with gentiopicrin sterling, gentiopicrin sterling starts to collect when single speckle is presented
Eluent, occurs again stopping collecting eluent during other speckles in eluent, the eluent of collection is volatilized solvent, dragon is obtained final product
Gallbladder hardship glycosides.
Further, ultrasonic extraction or reflux, extract, are extracted as described in step A.
Further, in step A, Rhizoma Picrorhizae dry rhizome is taken, with the methanol extraction 3 of 3.88～4.05 times of amounts of its quality
Secondary, 2 hours every time, temperature was 50～70 DEG C.
Further, in step B, the degree of the concentration is extracting solution is concentrated into total extraction volume 1/10th.
Further, in step B, normal hexane, ethyl acetate, n-butanol extraction 3 times, every time 40～50 points are used successively respectively
Clock.N-hexane extraction 3 times (every time 40～50 minutes) is first used, then is extracted with ethyl acetate 3 times (every time 40～50 minutes), most
N-butanol extraction 3 times (every time 40～50 minutes) is used afterwards.
Further, the specification of column chromatography silica gel described in step E is 100～300 mesh.
Further, pulverize and sieve in step E process screen cloth specification be 200 mesh.
Further, the blade diameter length ratio of the chromatographic column for using during pillar layer separation described in step F is 1：15.The present invention's has
Beneficial effect is：
The method of the invention enables gentiopicrin individually to be eluted from silica gel chromatographic column by substantial amounts of, improves
The extracted amount of gentiopicrin, the gentiopicrin purity for finally giving reach 98.7～99.3%, substantially increase gentiopicrin
Purity.Method of the present invention applied range, convenient and swift, low cost, simple to operate, fractional dose are big, are adapted to push away on a large scale
It is wide to apply.
Specific embodiment
It, in order to preferably illustrate to present disclosure, but is not that present disclosure is only limited that illustrated embodiment is
In illustrated embodiment.So those of ordinary skill in the art carry out nonessential change to embodiment according to foregoing invention content
Enter and adjust, still fall within protection scope of the present invention.
Embodiment 1
In Rhizoma Picrorhizae, the separating and extracting process of gentiopicrin, specifically includes following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol ultrasonic extraction of 4.05 times of its quality amount or reflux, extract, 3 times,
2 hours every time, temperature was 70 DEG C；
B., extracting solution obtained by step A is concentrated into 1/10th of total extraction volume, is added in the methanol solution after concentration
Enter the purified water of equal volume amounts, stand overnight, fling to methanol, the solution for flinging to methanol is used into normal hexane, acetic acid second successively respectively
Ester, n-butyl alcohol carry out extraction 3 times, (first use n-hexane extraction 3 times (every time 40 minutes), then use ethyl acetate within 40 minutes every time
3 times (every time 40 minutes) of extraction, finally with n-butanol extraction 3 times (every time 40 minutes))；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 20 mesh, successively with water, volume fraction be 10%
Ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, elution volume
For 4 times of chromatographic column retention volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.45 times of extractum
100 mesh column chromatography silica gel of quality, stir, fling to solvent flashing, crushed 200 mesh sieves, be added to containing extractum quality
On the silica gel chromatographic column of 15.7 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 7：3 solution is eluting solvent, carries out chromatographic isolation to column chromatography
(blade diameter length ratio of chromatographic column is 1：15) control is done using thin layer chromatography tracing detection with gentiopicrin sterling, gentiopicrin is pure
Product start to collect eluent when single speckle is presented, and occur again stopping collecting eluent during other speckles in eluent, will receive
The eluent of collection volatilizes solvent, obtains final product gentiopicrin, and in the sample for obtaining, the mass fraction of gentiopicrin is 99.2%.
Embodiment 2
In Rhizoma Picrorhizae, the separating and extracting process of gentiopicrin, specifically includes following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol ultrasonic extraction of 3.88 times of its quality amount or reflux, extract, 3 times,
2 hours every time, temperature was 50 DEG C；
B., extracting solution obtained by step A is concentrated into 1/10th of total extraction volume, is added in the methanol solution after concentration
Enter the purified water of equal volume amounts, stand overnight, fling to methanol, the solution for flinging to methanol is used into normal hexane, acetic acid second successively respectively
Ester, n-butyl alcohol carry out extraction 3 times, (first use n-hexane extraction 3 times (every time 50 minutes), then use ethyl acetate within 50 minutes every time
3 times (every time 50 minutes) of extraction, finally with n-butanol extraction 3 times (every time 50 minutes))；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 60 mesh, successively with water, volume fraction be 10%
Ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, elution volume
For 4 times of chromatographic column retention volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.52 times of extractum
300 mesh column chromatography silica gel of quality, stir, fling to solvent flashing, crushed 200 mesh sieves, be added to containing extractum quality
On the silica gel chromatographic column of 15.7 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 7：3 solution is eluting solvent, carries out chromatographic isolation to column chromatography
(blade diameter length ratio of chromatographic column is 1：15) control is done using thin layer chromatography tracing detection with gentiopicrin sterling, gentiopicrin is pure
Product start to collect eluent when single speckle is presented, and occur again stopping collecting eluent during other speckles in eluent, will receive
The eluent of collection volatilizes solvent, obtains final product gentiopicrin, and in the sample for obtaining, the mass fraction of gentiopicrin is 98.7%.
Embodiment 3
In Rhizoma Picrorhizae, the separating and extracting process of gentiopicrin, specifically includes following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol ultrasonic extraction of 3.96 times of its quality amount or reflux, extract, 3 times,
2 hours every time, temperature was 60 DEG C；
B., extracting solution obtained by step A is concentrated into 1/10th of total extraction volume, is added in the methanol solution after concentration
Enter the purified water of equal volume amounts, stand overnight, fling to methanol, the solution for flinging to methanol is used into normal hexane, acetic acid second successively respectively
Ester, n-butyl alcohol carry out extraction 3 times, (first use n-hexane extraction 3 times (every time 45 minutes), then use ethyl acetate within 45 minutes every time
3 times (every time 45 minutes) of extraction, finally with n-butanol extraction 3 times (every time 45 minutes))；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 50 mesh, successively with water, volume fraction be 10%
Ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, elution volume
For 4 times of chromatographic column retention volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.48 times of extractum
200 mesh column chromatography silica gel of quality, stir, fling to solvent flashing, crushed 200 mesh sieves, be added to containing extractum quality
On the silica gel chromatographic column of 14.6 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 7：3 solution is eluting solvent, carries out chromatographic isolation to column chromatography
(blade diameter length ratio of chromatographic column is 1：15) control is done using thin layer chromatography tracing detection with gentiopicrin sterling, gentiopicrin is pure
Product start to collect eluent when single speckle is presented, and occur again stopping collecting eluent during other speckles in eluent, will receive
The eluent of collection volatilizes solvent, obtains final product gentiopicrin, and in the sample for obtaining, the mass fraction of gentiopicrin is 99.3%.
Comparative example 1
In Rhizoma Picrorhizae, the separating and extracting process of gentiopicrin, specifically includes following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol ultrasonic extraction of 3.89 times of its quality amount or reflux, extract, 3 times,
2 hours every time, temperature was 57 DEG C；
B., extracting solution obtained by step A is concentrated into 1/10th of total extraction volume, is added in the methanol solution after concentration
Enter the purified water of equal volume amounts, stand overnight, fling to methanol, the solution for flinging to methanol is used into normal hexane, acetic acid second successively respectively
Ester, n-butyl alcohol carry out extraction 3 times, (first use n-hexane extraction 3 times (every time 40 minutes), then use ethyl acetate within 40 minutes every time
3 times (every time 40 minutes) of extraction, finally with n-butanol extraction 3 times (every time 40 minutes))；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 40 mesh, successively with water, volume fraction be 10%
Ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, elution volume
For 4 times of chromatographic column retention volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.49 times of extractum
100 mesh column chromatography silica gel of quality, stir, fling to solvent flashing, crushed 200 mesh sieves, be added to containing extractum quality
On the silica gel chromatographic column of 14.7 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 6：4 solution is eluting solvent, carries out chromatographic isolation to column chromatography
(blade diameter length ratio of chromatographic column is 1：15) control is done using thin layer chromatography tracing detection with gentiopicrin sterling, gentiopicrin is pure
Product start to collect eluent when single speckle is presented, and occur again stopping collecting eluent during other speckles in eluent, will receive
The eluent of collection volatilizes solvent, obtains final product gentiopicrin, and in the sample for obtaining, the mass fraction of gentiopicrin is 79.8%.
Comparative example 2
In Rhizoma Picrorhizae, the separating and extracting process of gentiopicrin, specifically includes following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol ultrasonic extraction of 3.97 times of its quality amount or reflux, extract, 3 times,
2 hours every time, temperature was 67 DEG C；
B., extracting solution obtained by step A is concentrated into 1/10th of total extraction volume, is added in the methanol solution after concentration
Enter the purified water of equal volume amounts, stand overnight, fling to methanol, will fling to the solution of methanol successively respectively with n-butyl alcohol, normal hexane,
Ethyl acetate carries out extraction 3 times, (first uses n-hexane extraction 3 times (every time 50 minutes), then is extracted with ethyl acetate within 50 minutes every time
3 times (every time 50 minutes) are taken, finally with n-butanol extraction 3 times (every time 50 minutes))；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 40 mesh, successively with water, volume fraction be 10%
Ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, elution volume
For 4 times of chromatographic column retention volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.51 times of extractum
200 mesh column chromatography silica gel of quality, stir, fling to solvent flashing, crushed 200 mesh sieves, be added to containing extractum quality
On the silica gel chromatographic column of 14.2 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 7：3 solution is eluting solvent, carries out chromatographic isolation to column chromatography
(blade diameter length ratio of chromatographic column is 1：15) control is done using thin layer chromatography tracing detection with gentiopicrin sterling, gentiopicrin is pure
Product start to collect eluent when single speckle is presented, and occur again stopping collecting eluent during other speckles in eluent, will receive
The eluent of collection volatilizes solvent, obtains final product gentiopicrin, and in the sample for obtaining, the mass fraction of gentiopicrin is 82.5%.
Comparative example 3
Carried with the separation that 2 methods described of application for a patent for invention embodiment of Publication No. 102675386A carries out gentiopicrin
Take, concrete grammar is：
A. weigh 250 mesh column chromatography silica gel 600g, add chloroform, methanol volume ratio for 9: 1 mixed solvent, stir to not having
Pour into after having bubble in glass chromatography column, settle, obtain silica gel column chromatography；
B. weigh Radix Gentianae crude extract 20g (Rhizoma Picrorhizae is crushed, with the volume fraction of 15 times of its quality be 70% ethanol in
40 DEG C of supersound extraction 5h, extract twice, use petroleum ether degreasing, by the Aqueous extracts after grease removal by activity after extracting solution concentrating under reduced pressure
Charcoal: the overload post of kieselguhr (1: 1), first wash removing water-solubility impurity with water, then with ethanol elution, obtain ethanol elution, return
Ethanol is received, gentiopicrin crude extract (gentiopicrin crude extract preparation method described in this application description, by Radix Gentianae Macrophyllae is obtained
Change Rhizoma Picrorhizae into)) dissolved with a small amount of ethanol, add 250 mesh silica gel of 60g to mix thoroughly, fling to solvent, dry, ground 200
Mesh sieve, is added on the silica gel column chromatography of step A；
C. eluent is done for 9: 1 mixed solvent with chloroform, methanol volume ratio, gentiopicrin sterling is compareed,
D. thin layer chromatography tracing detection, collects eluent when gentiopicrin is presented single speckle, until eluent
In stop collecting when occurring other speckles again.The eluent rotary evaporation of collection, it is concentrated to give gentiopicrin sterling, wherein Radix Gentianae
The mass fraction of bitter glycosides is 93.7%.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped
Containing an independent technical scheme, this narrating mode of description is only that those skilled in the art should for clarity
Using description as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art
Understandable other embodiment.
Claims (8)
1. in Rhizoma Picrorhizae gentiopicrin separating and extracting process, it is characterised in that comprise the following steps：
A. Rhizoma Picrorhizae dry rhizome is taken, with the methanol extraction of 3.88～4.05 times of amounts of its quality；
B. extracting solution obtained by step A is concentrated, the purified water of equal volume amounts is added in the methanol solution after concentration, was placed
At night, methanol is flung to, the solution for flinging to methanol is extracted with normal hexane, ethyl acetate, n-butyl alcohol successively respectively；
C. butanol extraction liquid is concentrated into into extractum, after flinging to n-butyl alcohol, uses purification water dissolution extractum；
D. the solution for step C being obtained carries out chromatographic isolation with the resin column of 20～60 mesh, successively with water, volume fraction be 10%
Ethanol solution, the ethanol solution that volume fraction is 30%, the ethanol solution that volume fraction is 50% carry out eluting, elution volume
For 4 times of chromatographic column retention volume；Eluent is concentrated into into extractum；
E. the extractum that step D is obtained is dissolved in methanol, after filtration, discards insoluble matter, in filtrate, add 1.45～1.52 times of leachings
The column chromatography silica gel of cream quality, stirs, flings to solvent flashing, pulverize and sieve, be added to containing extractum quality 13.9～
On the silica gel chromatographic column of 15.7 times of column chromatography silica gel；
F. with ethyl acetate：The volume ratio of methanol is 7：3 solution is eluting solvent, carries out chromatographic isolation to column chromatography, with dragon
Gallbladder hardship glycosides sterling does control using thin layer chromatography tracing detection, and gentiopicrin sterling starts to collect eluting when single speckle is presented
Liquid, occurs again stopping collecting eluent during other speckles in eluent, the eluent of collection is volatilized solvent, Radix Gentianae is obtained final product bitter
Glycosides.
2. in Rhizoma Picrorhizae according to claim 1 gentiopicrin separating and extracting process, it is characterised in that step A
It is described to be extracted as ultrasonic extraction or reflux, extract,.
3. in Rhizoma Picrorhizae according to claim 1 gentiopicrin separating and extracting process, it is characterised in that step A
In, Rhizoma Picrorhizae dry rhizome is taken, with the methanol extraction 3 times of 3.88～4.05 times of its quality amount, 2 hours every time, temperature was
50～70 DEG C.
4. in Rhizoma Picrorhizae according to claim 1 gentiopicrin separating and extracting process, it is characterised in that step B
In, the degree of the concentration is extracting solution is concentrated into total extraction volume 1/10th.
5. in Rhizoma Picrorhizae according to claim 1 gentiopicrin separating and extracting process, it is characterised in that step B
In, successively respectively with normal hexane, ethyl acetate, n-butanol extraction 3 times, every time 40～50 minutes.
6. in Rhizoma Zingiberis Recenss according to claim 1 6-gingerol separating and extracting process, it is characterised in that post color described in step E
The specification of spectrum silica gel is 100～300 mesh.
7. in Rhizoma Zingiberis Recenss according to claim 1 6-gingerol separating and extracting process, it is characterised in that crushed in step E
The specification of sieved journey screen cloth is 200 mesh.
8. in Rhizoma Zingiberis Recenss according to claim 1 6-gingerol separating and extracting process, it is characterised in that post color described in step F
The blade diameter length ratio of the chromatographic column used in spectrum separation process is 1：15.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113817007A (en) * | 2021-10-18 | 2021-12-21 | 浙江大学 | Gentiopicroside derivative and preparation and application thereof |
| CN114949063A (en) * | 2022-07-14 | 2022-08-30 | 重庆医药高等专科学校 | Preparation method and application of effective part of Dachengqi decoction with synergistic antibacterial effect |
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| CN102675386A (en) * | 2011-12-24 | 2012-09-19 | 河南科技大学 | Method for separating and purifying gentiamarin |
| CN103848875A (en) * | 2012-11-30 | 2014-06-11 | 哈尔滨誉衡药业股份有限公司 | Preparation method of gentiopicroside raw material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102675386A (en) * | 2011-12-24 | 2012-09-19 | 河南科技大学 | Method for separating and purifying gentiamarin |
| CN103848875A (en) * | 2012-11-30 | 2014-06-11 | 哈尔滨誉衡药业股份有限公司 | Preparation method of gentiopicroside raw material |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113817007A (en) * | 2021-10-18 | 2021-12-21 | 浙江大学 | Gentiopicroside derivative and preparation and application thereof |
| CN114949063A (en) * | 2022-07-14 | 2022-08-30 | 重庆医药高等专科学校 | Preparation method and application of effective part of Dachengqi decoction with synergistic antibacterial effect |
| CN114949063B (en) * | 2022-07-14 | 2023-05-16 | 重庆医药高等专科学校 | Preparation method and application of effective part with synergistic antibacterial effect |
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Application publication date: 20170329 |