CN108191933A - A kind of method that neoastilbin is prepared using smilax as raw material - Google Patents
A kind of method that neoastilbin is prepared using smilax as raw material Download PDFInfo
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- CN108191933A CN108191933A CN201711456505.9A CN201711456505A CN108191933A CN 108191933 A CN108191933 A CN 108191933A CN 201711456505 A CN201711456505 A CN 201711456505A CN 108191933 A CN108191933 A CN 108191933A
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- neoastilbin
- smilax
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- raw material
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- ZROGCCBNZBKLEL-FHXNIQKESA-N Astilbin Natural products O([C@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c(c(O)cc(O)c2)C1=O)[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O1 ZROGCCBNZBKLEL-FHXNIQKESA-N 0.000 title claims abstract description 84
- ZROGCCBNZBKLEL-AEGLVIMLSA-N Isoastibin Natural products O([C@@H]1[C@H](c2cc(O)c(O)cc2)Oc2c(c(O)cc(O)c2)C1=O)[C@H]1[C@@H](O)[C@H](O)[C@@H](O)[C@H](C)O1 ZROGCCBNZBKLEL-AEGLVIMLSA-N 0.000 title claims abstract description 54
- ZROGCCBNZBKLEL-MFSALPCASA-N neoastilbin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1C(=O)C2=C(O)C=C(O)C=C2O[C@H]1C1=CC=C(O)C(O)=C1 ZROGCCBNZBKLEL-MFSALPCASA-N 0.000 title claims abstract description 54
- ZROGCCBNZBKLEL-RMPKKLJSSA-N neoastilbin Natural products C[C@@H]1O[C@H](O[C@H]2[C@@H](Oc3cc(O)cc(O)c3C2=O)c2ccc(O)c(O)c2)[C@H](O)[C@H](O)[C@H]1O ZROGCCBNZBKLEL-RMPKKLJSSA-N 0.000 title claims abstract description 54
- 241000605422 Asparagus asparagoides Species 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000002994 raw material Substances 0.000 title claims abstract description 20
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 22
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 11
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 11
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 239000012141 concentrate Substances 0.000 claims description 14
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 8
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 239000003480 eluent Substances 0.000 claims description 6
- 238000000605 extraction Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 235000008599 Poria cocos Nutrition 0.000 claims description 5
- 241001619444 Wolfiporia cocos Species 0.000 claims description 5
- 238000004587 chromatography analysis Methods 0.000 claims description 5
- 239000000047 product Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 230000002411 adverse Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000001953 recrystallisation Methods 0.000 claims description 2
- 238000010898 silica gel chromatography Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- ZROGCCBNZBKLEL-MPRHSVQHSA-N astilbin Chemical class O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@H]1C(=O)C2=C(O)C=C(O)C=C2O[C@@H]1C1=CC=C(O)C(O)=C1 ZROGCCBNZBKLEL-MPRHSVQHSA-N 0.000 abstract description 30
- 238000006317 isomerization reaction Methods 0.000 abstract description 15
- 238000000354 decomposition reaction Methods 0.000 abstract description 6
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 abstract description 5
- 230000001131 transforming effect Effects 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000000746 purification Methods 0.000 abstract description 2
- 229930182470 glycoside Natural products 0.000 description 7
- 150000002338 glycosides Chemical class 0.000 description 7
- 241000362909 Smilax <beetle> Species 0.000 description 6
- 229930003944 flavone Natural products 0.000 description 5
- 235000011949 flavones Nutrition 0.000 description 5
- 238000004811 liquid chromatography Methods 0.000 description 4
- 239000007791 liquid phase Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 150000002212 flavone derivatives Chemical class 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002213 flavones Chemical class 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- -1 2 (R):3 (R) -3 ' Chemical compound 0.000 description 1
- HBAQYPYDRFILMT-UHFFFAOYSA-N 8-[3-(1-cyclopropylpyrazol-4-yl)-1H-pyrazolo[4,3-d]pyrimidin-5-yl]-3-methyl-3,8-diazabicyclo[3.2.1]octan-2-one Chemical class C1(CC1)N1N=CC(=C1)C1=NNC2=C1N=C(N=C2)N1C2C(N(CC1CC2)C)=O HBAQYPYDRFILMT-UHFFFAOYSA-N 0.000 description 1
- 241000123982 Astilbe chinensis Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- ZXYFGZNMDRNOGQ-UHFFFAOYSA-N ac1lawgt Chemical compound [S]O ZXYFGZNMDRNOGQ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
- C07H17/07—Benzo[b]pyran-4-ones
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention provides a kind of methods that neoastilbin is prepared using smilax as raw material.The technical solution has primarily looked in smilax and has mutually converted relationship between four kinds of isomers of astilbin, it has been surprisingly found that in the presence of ascorbic acid, specific pH and temperature condition can start isomerization reaction of the astilbin to neoastilbin, based on this beneficial discovery, the present invention, to be oriented to, has groped best reaction condition with isomerization direction, transforming degree, product degree of decomposition etc.；Under this condition, astilbin major isomer turns to neoastilbin, and decomposition rate is slower.Based on this, the present invention further devises the extracting condition of front end and subsequent purification process.Using the bright method of we, astilbin in smilax can be largely converted into neoastilbin, so as to which neoastilbin content in Rhizoma Smilacis Glabrae extract be made to improve nearly 9 times, greatly improve the efficiency that neoastilbin is isolated and purified from smilax.
Description
Technical field
The present invention relates to active components of plants extractive technique fields, and in particular to a kind of newly to be fallen by raw material preparation of smilax
The method of bride's glycosides.
Background technology
Astilbin, i.e., 2 (R):3 (R) -3 ', 4 ', 5,7-4 hydroxyl sulphur alkanone -3- α-L- rhamnopyranoses are Chinese medicine soil
The main composition of Poria cocos.There are many bioactivity, such as selective immunosupress, adjusting fat metabolism, antioxygens for astilbin
Change, liver protection effect etc..
According to astilbin molecular structure, there are stereo-isomerisms on C2 and C3, there is 2 (R) respectively:3(R)
(astilbin), 2 (S):3 (S) (neoastilbins), 2 (S):3 (R) (neoisoastilbins) and 2 (R):3 (S) (different Astilbe chinensis
Glycosides) four kinds of isomers.The isomerism of compound may influence its bioactivity, and two kinds of enantiomers of some drugs have had
Complete different pharmacological action.It is therefore desirable to be directed to the expansion research of the biological activity of its isomers.
Four kinds of isomers containing astilbin, but astilbin content highest simultaneously in smilax, other three kinds of isomeries
Body content is very low, therefore, the method routinely extracted is used to can only obtain account for the extract of ingredient big absolutely with astilbin, both can not
It realizes the separation between isomers, can not also promote the accounting of neoastilbin ingredient.Therefore it is directly separated and falls from smilax
The method of bride's glycosides is more mature at present, and the method for therefrom obtaining neoastilbin is rarely reported, even if there is researcher
Certain success is achieved, yield is also at reduced levels.This greatly hinders the property research of neoastilbin and depth
Degree application.
Invention content
The present invention is directed to be directed to the technological deficiency of the prior art, one kind is provided and prepares neoastilbin by raw material of smilax
Method, with solve lack a kind of such method in the prior art the technical issues of.
Another technical problem to be solved by the present invention is that prepared in the method for neoastilbin by raw material of smilax,
How yield is promoted.
The invention solves another technical problem be in the Rhizoma Smilacis Glabrae extract that general extraction methods are obtained, to fall new
Woman's glycosides accounts for main component, and neoastilbin accounting is very low.
For realization more than technical purpose, the present invention uses following technical scheme：
A kind of method that neoastilbin is prepared using smilax as raw material, includes the following steps：
1) fetch earth Poria cocos, smashes it through 20~40 mesh sieve, and the ethanol water of a concentration of 10~90% (v/v) is taken to be used as and is carried
Agent is taken, to be sieved through the ratio between the quality of object and the volume of the extractant as 1:20(kg:L ratio), by the sieved object and institute
Extractant mixing is stated, stirs 60min in room temperature condition, filtering takes filtrate；
2) filtrate obtained by step 1) under the conditions of 60 DEG C is concentrated in vacuo, recycles ethyl alcohol, obtain concentrate；
3) pH of concentrate obtained by step 2) is adjusted to 5~9, add in thereto ascorbic acid to final concentration of 0.1~
10mM stands 6~16h of reaction in 50~90 DEG C of environment.
Preferably, this method is further comprising the steps of 4)：Take step 3) products therefrom, using resin adsorption, recrystallization,
Silica gel column chromatography, half preparation chromatography or high speed adverse current chromatogram therefrom extract neoastilbin sterling.
Preferably, step 4) specifically includes following operation：Take step 3) products therefrom, flow through H103 macroreticular resins bed into
Row absorption, is then eluted with the ethanol solution of 4 times of bed volumes, collects eluent；It is prepared described in chromatography collection using half
Neoastilbin ingredient in eluent, freeze-drying.
Preferably, the bed volume of macroreticular resin bed described in step 4) is 160ml, column bed height is 60cm；It is described
A concentration of 50% (v/v) of ethanol solution.
Preferably, a concentration of 50% (v/v) of the step 1) ethanol water.
Preferably, the pH of concentrate is adjusted to 8.0 in step 3).
Preferably, in step 3) ascorbic acid final concentration of 1mM.
Preferably, being stood described in step 3), carried out under water bath condition.
Preferably, the temperature stood described in step 3) is 80 DEG C.
Preferably, the time stood described in step 3) is 10h.
In above technical scheme, the smilax is the Chinese medicine of entitled smilax, is in the nature liliaceous plant
The dry rhizome of smilacis glabra.The sieved object refers to using after sieve screening, and grain size is smaller thus the part that passes through sieve.
The present invention provides a kind of method that neoastilbin is prepared using smilax as raw material, which passes through first
Laboratory facilities are found, since four kinds of isomers respectively have natural contents level, and its chemical property in smilax material
It is very close, therefore it is difficult the wherein a certain isomers of orientation extraction only to improve extraction technique.In this case, this hair
It is bright to have investigated four kinds of mutual transforming relationships of isomers, it has been surprisingly found that in the presence of ascorbic acid, specific pH and temperature condition
Isomerization reaction of the astilbin to neoastilbin can be started, based on this beneficial discovery, the present invention with isomerization direction,
Transforming degree, product degree of decomposition etc. have groped best reaction condition to be oriented to；Under this condition, astilbin is mainly different
Structure turns to neoastilbin, and decomposition rate is slower.Based on this, the present invention further devises the extracting condition of front end
And subsequent purification process.Using the bright method of we, astilbin in smilax can be largely converted into neoastilbin,
So as to which neoastilbin content in Rhizoma Smilacis Glabrae extract be made to improve nearly 9 times, greatly improve and isolated and purified from smilax newly
The efficiency of astilbin.
Description of the drawings
Fig. 1 is the efficient liquid phase liquid chromatography figure of smilax extracting solution before isomerization in the specific embodiment of the invention；Figure
In：No. 1 peak is neoastilbin；No. 2 peaks are astilbin.
Fig. 2 is the efficient liquid phase liquid chromatography figure of smilax extracting solution after isomerization in the specific embodiment of the invention；Figure
In：No. 1 peak is neoastilbin；No. 2 peaks are astilbin.
Specific embodiment
The specific embodiment of the present invention will be described in detail below.In order to avoid excessive unnecessary details,
It will not be described in detail in following embodiment to belonging to well known structure or function.
Approximating language used in following embodiment can be used for quantitative expression, show in the feelings for not changing basic function
Quantity is allowed to have certain variation under condition.Therefore, it is not limited to this accurately with the modified numerical value of the language such as " about ", " left and right " institute
Numerical value is in itself.In some embodiments, the range for allowing its modified numerical value in positive and negative 10 (10%) " about " is represented
Interior variation, for example, what " about 100 " represented can be any numerical value between 90 to 110.In addition, " the about first numerical value arrives
In the statement of second value ", the first and second numerical value two values are at about corrected.In some cases, approximating language
It may be related with the precision of measuring instrument.
In addition to being defined, technical and scientific term used in following embodiment has and fields technology people of the present invention
The identical meanings that member is commonly understood by.
Test reagent consumptive material used in following embodiment is conventional biochemical reagent unless otherwise specified；The experiment
Method is conventional method unless otherwise specified；Quantitative test in following embodiment is respectively provided with three repeated experiments, as a result
It is averaged；% in following embodiment is mass percentage unless otherwise instructed.
Embodiment 1
1kg smilaxs smash it through 40 mesh sieve, add in a concentration of 50% ethanol water 20L, stir at ambient temperature
Extraction 60 minutes obtains extracting solution through conventional filtration.Fig. 1 is the high performance liquid chromatography of smilax extracting solution.Peak 1 is newly falls in figure
Bride's glycosides, peak 2 are astilbin.Through high effective liquid chromatography for measuring, astilbin content is 2.2% in smilax, is newly fallen new
Woman's glycosides content is 0.17%, i.e., contains astilbin 22g, neoastilbin 1.7g in 1kg smilaxs in total；It can be seen that in smilax
Astilbin content highest, and neoastilbin content is very low.
Smilax extracting solution is concentrated and adjusts pH to 8 after removing ethyl alcohol, adds in the ascorbic acid that ultimate density is 1mM,
It is placed in 80 degree of water-baths 10 hours and carries out isomerization reaction.Fig. 2 is the high-efficient liquid phase color of smilax extracting solution after isomerization reaction
Spectrum.Peak 1 is neoastilbin in figure, and peak 2 is astilbin.It can be seen that after isomerization reaction, astilbin content significantly reduces；
And neoastilbin content significantly increases, and becomes main flavone component.Through high effective liquid chromatography for measuring, after isomerization
Astilbin total amount is reduced to 3.9g in 1kg smilaxs, and neoastilbin total amount increases to 16.7g.Neoastilbin in smilax
Content improves 8.8 times, and substitution astilbin becomes main flavone component in extracting solution, pure subsequently to be detached from smilax
Change neoastilbin to offer convenience, and the yield of neoastilbin can be greatly improved.
Astilbin and neoastilbin comparision contents in 1kg smilaxs before and after 1 isomerization reaction of table
Experiment finds that the reduction of pH can slow down isomerization speed, and it is anti-that isomerization hardly occurs under conditions of pH3~4
It should；And pH it is excessively high (>9) and flavones can be caused unstable, astilbin and its isomers decompose rapidly.Temperature raising can be accelerated to fall
Bride's glycosides isomerization speed, but also its decomposition rate can simultaneously accelerated.Addition ascorbic acid can effectively improve neoastilbin
Conversion ratio, while improve flavones stability, reduce its decomposition rate.
Embodiment 2
(1) 1kg smilaxs is taken to crushed rear 40 mesh sieve, 60% ethanol solutions of 20L is added in, extraction is stirred at room temperature
60min obtains extracting solution after the filter-cloth filtering of 200 mesh.
(2) it is 60 degree of vacuum concentrations through temperature by extracting solution obtained by step (1), recycles ethyl alcohol, obtain concentrate 4L；Through height
Effect liquid phase chromatogram method measures, and contains astilbin 22g, neoastilbin 1.7g in concentrate in total.
(3) after concentrate obtained by step (2) being adjusted pH to 7 with 1mol/L NaOH solutions, 0.704g Vitamin Cs are added in
Acid, ascorbic acid ultimate density are 1mM, are positioned in 80 degree of water-baths 10 hours, carry out isomerization reaction.Through high performance liquid chromatography
Method measures, and contains astilbin 3.9g, neoastilbin 16.7g in concentrate in total at this time.Neoastilbin concentration improves
8.8 times, substitution astilbin becomes main flavone component in extracting solution, and purifying neoastilbin for later separation brings just
Profit.
(4) step (3) acquired solution is flowed through into H103 macroreticular resin beds, carries out adsorption operations；Bed volume is 160ml,
Column bed height is 60cm.Then elution action is carried out with 50% ethyl alcohol of 4 times of bed volumes, collects eluent.
(5) application half prepares neoastilbin component in chromatography collection step (4) eluent, is freeze-dried after concentration, altogether
Obtain the neoastilbin 16g that purity is more than 98%.
Embodiment 3
A kind of method that neoastilbin is prepared using smilax as raw material, includes the following steps：
1) fetch earth Poria cocos, smashes it through 20 mesh sieve, takes the ethanol water of a concentration of 10% (v/v) as extractant, with
It is 1 to be sieved through the ratio between the quality of object and the volume of the extractant:20(kg:L ratio), by the sieved object and the extractant
Mixing stirs 60min in room temperature condition, and filtering takes filtrate；
2) filtrate obtained by step 1) under the conditions of 60 DEG C is concentrated in vacuo, recycles ethyl alcohol, obtain concentrate；
3) pH of concentrate obtained by step 2) is adjusted to 5, adds in ascorbic acid thereto to final concentration of 0.1mM, in
Reaction 16h is stood in 50 DEG C of environment.
Embodiment 4
A kind of method that neoastilbin is prepared using smilax as raw material, includes the following steps：
1) fetch earth Poria cocos, smashes it through 40 mesh sieve, takes the ethanol water of a concentration of 90% (v/v) as extractant, with
It is 1 to be sieved through the ratio between the quality of object and the volume of the extractant:20(kg:L ratio), by the sieved object and the extractant
Mixing stirs 60min in room temperature condition, and filtering takes filtrate；
2) filtrate obtained by step 1) under the conditions of 60 DEG C is concentrated in vacuo, recycles ethyl alcohol, obtain concentrate；
3) pH of concentrate obtained by step 2) is adjusted to 9, ascorbic acid is added in thereto to final concentration of 10mM, in 90
Reaction 6h is stood in DEG C environment.
The embodiment of the present invention is described in detail above, but the content is only presently preferred embodiments of the present invention,
It is not intended to limit the invention.All all any modification, equivalent and improvement done in the application range of the present invention etc., should all
It is included within protection scope of the present invention.
Claims (10)
- A kind of 1. method that neoastilbin is prepared using smilax as raw material, it is characterised in that include the following steps：1) fetch earth Poria cocos, smashes it through 20~40 mesh sieve, takes the ethanol water of a concentration of 10~90% (v/v) as extraction Agent, to be sieved through the ratio between the quality of object and the volume of the extractant as 1:20(kg:L ratio), by the sieved object with it is described Extractant mixes, and stirs 60min in room temperature condition, filtering takes filtrate；2) filtrate obtained by step 1) under the conditions of 60 DEG C is concentrated in vacuo, recycles ethyl alcohol, obtain concentrate；3) pH of concentrate obtained by step 2) is adjusted to 5~9, adds in ascorbic acid thereto to final concentration of 0.1~10mM, 6~16h of reaction is stood in 50~90 DEG C of environment.
- 2. a kind of method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that also Include the following steps 4)：Step 3) products therefrom is taken, chromatography or height are prepared using resin adsorption, recrystallization, silica gel column chromatography, half Fast adverse current chromatogram therefrom extracts neoastilbin sterling.
- A kind of 3. method that neoastilbin is prepared using smilax as raw material according to claim 2, it is characterised in that step It is rapid 4) to specifically include following operation：Step 3) products therefrom is taken, H103 macroreticular resin beds is flowed through and is adsorbed, then with 4 times of columns The ethanol solution of bed volume is eluted, and collects eluent；Chromatography, which is prepared, using half collects neoastilbin in the eluent Ingredient, freeze-drying.
- A kind of 4. method that neoastilbin is prepared using smilax as raw material according to claim 3, it is characterised in that step It is rapid 4) described in macroreticular resin bed bed volume for 160ml, column bed height is 60cm；A concentration of the 50% of the ethanol solution (v/v)。
- A kind of 5. method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that step A concentration of 50% (v/v) of rapid 1) described ethanol water.
- A kind of 6. method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that step It is rapid 3) in the pH of concentrate be adjusted to 8.0.
- A kind of 7. method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that step It is rapid 3) in ascorbic acid final concentration of 1mM.
- A kind of 8. method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that step It is rapid 3) described in stand, carried out under water bath condition.
- A kind of 9. method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that step It is rapid 3) described in the temperature that stands be 80 DEG C.
- A kind of 10. method that neoastilbin is prepared using smilax as raw material according to claim 1, it is characterised in that step It is rapid 3) described in time for standing be 10h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711456505.9A CN108191933B (en) | 2017-12-28 | 2017-12-28 | Method for preparing new astilbin by taking rhizoma smilacis glabrae as raw material |
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| CN114452261A (en) * | 2021-12-31 | 2022-05-10 | 湖南茯神科技有限公司 | Preparation method and application of rhizoma smilacis glabrae alcohol extract oral tablet |
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| CN114452261A (en) * | 2021-12-31 | 2022-05-10 | 湖南茯神科技有限公司 | Preparation method and application of rhizoma smilacis glabrae alcohol extract oral tablet |
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Effective date of registration: 20231208 Address after: 343000 Chengbei Industrial Park, Yongfeng County, Ji'an City, Jiangxi Province Patentee after: WENIR NUTRITION HIGH-TECH CO.,LTD. Address before: 330045 Jiangxi Agricultural University, Changbei Economic and Technological Development Zone, Nanchang City, Jiangxi Province Patentee before: JIANGXI AGRICULTURAL University |