CN108047289A - A kind of extraction for preparing high-purity gardenoside and process for purification - Google Patents
A kind of extraction for preparing high-purity gardenoside and process for purification Download PDFInfo
- Publication number
- CN108047289A CN108047289A CN201711494766.XA CN201711494766A CN108047289A CN 108047289 A CN108047289 A CN 108047289A CN 201711494766 A CN201711494766 A CN 201711494766A CN 108047289 A CN108047289 A CN 108047289A
- Authority
- CN
- China
- Prior art keywords
- gardenoside
- extraction
- purity
- gained
- concentrated
- 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
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
-
- 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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The present invention relates to a kind of extraction for preparing high-purity gardenoside and process for purification, the method is：Using cape jasmine fruit phytoclasts as raw material, with 60% ethanol water heating and refluxing extraction, after extraction, gained mixed liquor is through removing ethyl alcohol and being concentrated to give Gardenoside crude extract medicinal extract；Gained Gardenoside crude extract medicinal extract addition deionized water is made into Gardenoside crude extract medicinal extract aqueous solution, it crosses macroporous resin column HPD100A, after end of the sample, is eluted using 20% ethanol solution as eluant, eluent, the eluent of 20% ethanol solution is collected, is concentrated to give Gardenoside concentrate；Excessive settling agent is added in into gained concentrate, sediment is precipitated in adjustment pH value to 9~14, and removal precipitation obtains high-purity gardenoside.This experimental implementation is simple, and material is cheap and easy to get, Gardenoside high income, lost in separation process it is small, purity be more than 95%, without cumbersome column chromatography for separation, be very suitable for industrializing, advantageously reduce enterprise production cost.
Description
Technical field：
The present invention relates to a kind of extraction for preparing high-purity gardenoside and process for purification.Height is refined especially by the precipitation method
The method of purity Gardenoside.
Background technology：
China's cape jasmine resource is very abundant, occupies first place in the world, is distributed mainly on southern each province.Cape jasmine is madder wort Cape jasmine
The dry mature fruit of son, oblong or ellipse, in peony or yellowish red color.Effective component in cape jasmine is Gardenoside,
Content of the Gardenoside in cape jasmine is also quite high, generally 3%--5%.Gardenoside has hepatic cholagogic, anti-inflammatory, antioxygen
Change and the effect for the treatment of diabetes B etc..In addition, Gardenoside is also production gardenia blue, the effective monomer of gardenia red.Not only such as
This, Gardenoside can be hydrolyzed to Geniposide under enzymatic catalysis, Geniposide as a kind of excellent collagen, gelatin, protein and
The genipin of chitosan has the characteristics that toxicity is low.Geniposide may be also used on the materials such as artifical bone and wound dressing.
But due to existing separation and refining method deficiency, commercial product is mostly without refined Gardenoside crude product, and content is only 60%
Left and right, not only limits the application of Gardenoside, low-purity Gardenoside can also influence downstream product Geniposide and gardenia blue pigment
Quality, causes that Geniposide yield is relatively low and cyanine color value is unstable.
Isolating and purifying the method for Gardenoside from cape jasmine at present mainly has (1) column chromatography (CN102212091A, Chinese medicine
Material, 2011,34 (09):1442-1446)：Using silica gel, modified silica-gel or aluminium oxide separate Gardenoside as sorbing material, can
To obtain the preferable Gardenoside of purity, but it is high there are equipment requirement, and fractional dose is small, refines the problems such as yield is relatively low, is difficult at present
It realizes industrialization, and is needed during Gardenoside isolates and purifies using a large amount of poisonous and hazardous solvents, such as ether, chloroform, third
Ketone, lead salt etc. do not meet the production specification of food and medicine.(2) macroreticular resin absorbing method (CN1706859；CN102212091A)：
For the Gardenoside isolation and purification method used at present, but it is complicated for operation, and solvent-oil ratio is big, and product purity is difficult to control
System.(3) other methods such as aqueous two-phase system (CN105037461A), ultrafiltration (the ultrafiltration such as Rao Shuanchao, Shi Zhaohua, Huang Zhi army
Gardenoside technical study [J] medicine Leaders, 2007,26 (5) in method Purification of Fructus Gardeniae:464-466), lead salt precipitation (Yan Y
H.Simple separation method of geniposide in Gardemia jasminoides Ellis[J]
.Chin J Pharm Anal,1998,4(4):227-229), the supercritical fluid extraction (such as Yu Shunhuo, Li Xianxiang, riding track honor
Supercritical carbon dioxide extraction separates technical study [J] processings of farm products of high-purity gardenoside:Academic periodical, 2008,2008 (12):
64-66), (the high speed adverse current chromatogram separation such as Qian Hua, Lu Wei, Zhao Baitao prepares Gardenoside [C] // the Changjiang river to high-speed countercurrent chromatography
Delta Area botany seminar .2009) etc. be also used for the separation of Gardenoside with it is refined in, but equipment requirement is high or not
Meet food development principle, therefore be not used to actual production.
The content of the invention：
For overcome the deficiencies in the prior art, the present invention provides a kind of side extracted by cape jasmine and prepare high-purity gardenoside
Method.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of extraction for preparing high-purity gardenoside and process for purification, it is characterised in that：The method is specifically according to such as
Lower step carries out：
(1) using cape jasmine fruit phytoclasts as raw material, with 60% ethanol water heating and refluxing extraction, extraction finishes
Afterwards, gained mixed liquor is through removing ethyl alcohol and being concentrated to give Gardenoside crude extract medicinal extract；
(2) Gardenoside crude extract medicinal extract obtained by step (1) is added in into the Gardenoside crude extract that deionized water is configured to 10g/L
Medicinal extract aqueous solution crosses macroporous resin column HPD100A, after end of the sample, is eluted using 20% ethanol solution as eluant, eluent, collection
20% ethanol solution eluent, is concentrated to give Gardenoside concentrate；
(3) settling agent is added in into concentrate obtained by step (2), sediment is precipitated in adjustment pH value to 9-14, and removal is heavy
It forms sediment, remaining reaction mixture is post-treated to obtain high-purity gardenoside；The settling agent for magnesia, alkali alumina,
In calcium oxide, calcium carbonate, sodium carbonate, sodium acid carbonate, potassium carbonate, saleratus, lithium hydroxide, sodium hydroxide, potassium hydroxide
A kind of or arbitrary several combination (is preferably that mass ratio is 1:1 sodium hydroxide and the mixture of calcium oxide).
Further, in step (1), the cape jasmine fruit phytoclasts, which are pulverized and sieved by cape jasmine fruit to 40 mesh, to be obtained.
Further, in step (1), the extraction at a reflux temperature repeat extraction 3 times, every time 3 it is small when, merge 3 times
Extracting solution be mixed liquor.
Further, in step (1), after extraction, gained mixed liquor is filtered, collects filtrate, gained filter cake is used again
60% ethyl alcohol continues extraction 3 times, merges all filtrates and is concentrated into no alcohol taste, obtains Gardenoside crude extract medicinal extract.
Further, in step (1), the addition of the ethanol water is added in the cape jasmine fruit phytoclasts
The quality of amount is calculated as 10~30ml/g, preferably 20ml/g.
Further, in step (2), the relative density of the Gardenoside concentrate is 0.92~1.01.
Further, in step (3), the post-processing approach of the reaction mixture is：After reaction, gained reaction is mixed
It closes the filtrate that object is obtained by filtration and extracts 1~9 time (being preferably 3 times) with isometric organic solvent, combining extraction liquid extracts gained
Liquid concentration, bleaching agent bleaching, are dried under reduced pressure, and the solid of gained is recrystallized, dry, obtain high-purity gardenoside；Described has
Solvent is C3-5Aliphatic monobasic alcohol (preferably n-butanol).
Further, in step (3), the decolorising agent is the mixture of activated carbon and additional adsorbents arbitrary proportion,
The activated carbon character is graininess, powdery or column, preferably granular active carbon；The additional adsorbents are neutral oxygen
Change one or more of aluminium, alkali alumina, silica gel, diatomite or Emathlite (preferably alkali alumina).
Further, in step (3), the gross mass of the decolorising agent is calculated as 0.1- with the destainer volume
0.2mg/L。
In the decolorising agent, the amount ratio 1 of the activated carbon and aided bleaching agent：0.1-5.
Further, in step (3), the recrystallization process is：The solid is dissolved in mixing at 50-70 DEG C
Solvent, then stood still for crystals at -18-5 DEG C 24 it is small when, filtering, gained filter cake through mixed solvent wash 2~4 times, be dried under reduced pressure
Obtain high-purity gardenoside；The mixed solvent is methanol, ethyl alcohol, isopropanol, normal propyl alcohol, n-butanol, methyl acetate, second
The combination of arbitrary two kinds of organic solvents in acetoacetic ester, acetone or dichloromethane；The addition of the mixed solvent is with described
The quality of solid be calculated as 2-10ml/g.
Further, in step (3), the mixed solvent is methanol, ethyl alcohol, isopropanol, normal propyl alcohol, n-butanol, second
Arbitrary two kinds in sour methyl esters, ethyl acetate, acetone or dichloromethane are 10 by volume:1-1:20 ratio mixes organic
The combination of solvent is preferably that volume ratio is 1：20 methanol and the mixed solvent of ethyl acetate.
Compared with prior art, the present invention has the following advantages：
1. by using settling agent, the impurity such as polysaccharide contained in gardenia extract, phenols, organic acid, a side can be removed
Face improves the purity of Gardenoside in solution, on the other hand alleviates emulsification problem present in extraction process, and mitigation refined
Loss in journey.Make contamination precipitation, greatly improve the purity of Gardenoside.
2. settling agent is cheap and easily-available, particle is big, good impurity removing effect, is easy to later stage filtration treatment.
3. the use of aided bleaching agent, can the foreign pigment being tightly held by activated carbon further be difficult in adsorbing and extracting liquid,
The character of Gardenoside crude product can significantly be improved, while aided bleaching agent is seldom to the absorption of Gardenoside, will not cause effectively
The loss of ingredient, is greatly saved production cost.
4. experimental implementation is simple, material is cheap and easy to get, Gardenoside high income, loses small in separation process, and purity is more than
95%, it without cumbersome column chromatography for separation, is very suitable for industrializing, advantageously reduces the cost of enterprise's production.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
The cape jasmine fruit that 500g is taken to dry, mechanical grinding is into fine powder, and with 60% ethanol solutions of 10L, 70 DEG C are heated to reflux
Filtrate is collected in 3h, filtering, and filter cake continues to extract, be repeated 3 times with 60% ethyl alcohol of 10L, and merging filtrate is simultaneously concentrated into no alcohol taste, adds
Deionized water is diluted to 2L, and the concentration of Gardenoside is 10g/L.The Gardenoside aqueous solution obtained will be extracted, cross macroporous resin column
HPD100A after end of the sample, is eluted using 20% ethanol solution, is collected 20% ethanol eluate, be concentrated to 250ml or so.It presses
The amount of 2ml/g adds in alkali alumina solid, there is a large amount of precipitation generations, filtering, the isometric water-saturated n-butanol extraction 3 of filtrate
It is secondary, combining extraction liquid.Extract liquor is concentrated into 100ml, adds in 4g activated carbons and 4g alkali aluminas, 90 DEG C of heating stirrings 10 minutes
It decolourizes, filters, be concentrated under reduced pressure, obtain flaxen Gardenoside crude product 13.4g, purity 83.2%.
Above-mentioned obtained Gardenoside crude product 13.4g being dissolved in 53.6ml ethyl alcohol, 50 DEG C of heating stirrings are completely dissolved,
134ml ethyl acetate is added in, stirs evenly, is cooled to room temperature, when placement 12 is small in refrigerator, mass crystallization precipitation to be had.Filtering,
Filter cake is washed 2--4 times with the ethyl acetate of ice, drying, you can obtains the Gardenoside 11.6g that purity is 93.2%, yield is
54.1%.
Embodiment 2
The cape jasmine fruit that 500g is taken to dry, mechanical grinding is into fine powder, and with 60% ethanol solutions of 10L, 70 DEG C are heated to reflux
Filtrate is collected in 3h, filtering, and filter cake continues to extract, be repeated 3 times with 60% ethyl alcohol of 10L, and merging filtrate is simultaneously concentrated into no alcohol taste, adds
Deionized water is diluted to 2L, and the concentration of Gardenoside is 10g/L.The Gardenoside aqueous solution obtained will be extracted, cross macroporous resin column
HPD100A after end of the sample, is eluted using 20% ethanol solution, is collected 20% ethanol eluate, be concentrated to 250ml or so.It presses
The amount of 2ml/g adds in magnesia solid, there is a large amount of precipitation generations, filtering, and the isometric water-saturated n-butanol of filtrate extracts 3 times,
Combining extraction liquid.Extract liquor is concentrated into 100ml, adds in 4g activated carbons and 4g alkali aluminas, 90 DEG C of heating stirrings 10 minutes into
Row decoloration, filtering are concentrated under reduced pressure, obtain flaxen Gardenoside crude product 17.5g, purity 82.6%.
Above-mentioned obtained Gardenoside crude product 17.5g is dissolved in 70ml ethyl alcohol, 50 DEG C of heating stirrings are completely dissolved, and are added
Enter 175ml ethyl acetate, stir evenly, be cooled to room temperature, when placement 12 is small in refrigerator, mass crystallization precipitation to be had.Filtering, filter
Cake is washed 2--4 times with the ethyl acetate of ice, drying, you can obtains the Gardenoside 15.0g that purity is 92.8%, yield is
69.6%.
Embodiment 3
The cape jasmine fruit that 500g is taken to dry, mechanical grinding is into fine powder, and with 60% ethanol solutions of 10L, 70 DEG C are heated to reflux
Filtrate is collected in 3h, filtering, and filter cake continues to extract, be repeated 3 times with 60% ethyl alcohol of 10L, and merging filtrate is simultaneously concentrated into no alcohol taste, adds
Deionized water is diluted to 2L, and the concentration of Gardenoside is 10g/L.The Gardenoside aqueous solution obtained will be extracted, cross macroporous resin column
HPD100A after end of the sample, is eluted using 20% ethanol solution, is collected 20% ethanol eluate, be concentrated to 250ml or so.It presses
The amount of 2ml/g adds in sodium hydrate solid, there is a large amount of precipitation generations, filtering, the isometric water-saturated n-butanol extraction 3 of filtrate
It is secondary, combining extraction liquid.Extract liquor is concentrated into 100ml, adds in 4g activated carbons and 4g alkali aluminas, 90 DEG C of heating stirrings 10 minutes
It decolourizes, filters, be concentrated under reduced pressure, obtain flaxen Gardenoside crude product 18.9g, purity 85.2%.
Above-mentioned obtained Gardenoside crude product 18.9g being dissolved in 37.8ml methanol, 50 DEG C of heating stirrings are completely dissolved,
189ml ethyl acetate is added in, stirs evenly, is cooled to room temperature, when placement 12 is small in refrigerator, mass crystallization precipitation to be had.Filtering,
Filter cake is washed 2--4 times with the ethyl acetate of ice, drying, you can obtains the Gardenoside 16.2g that purity is 95.6%, yield is
77.4%.
Embodiment 4
The cape jasmine fruit that 500g is taken to dry, mechanical grinding is into fine powder, and with 60% ethanol solutions of 10L, 70 DEG C are heated to reflux
Filtrate is collected in 3h, filtering, and filter cake continues to extract, be repeated 3 times with 60% ethyl alcohol of 10L, and merging filtrate is simultaneously concentrated into no alcohol taste, adds
Deionized water is diluted to 2L, and the concentration of Gardenoside is 10g/L.The Gardenoside aqueous solution obtained will be extracted, cross macroporous resin column
HPD100A after end of the sample, is eluted using 20% ethanol solution, is collected 20% ethanol eluate, be concentrated to 250ml or so.It presses
The amount of 2ml/g adds in calcium oxide and sodium hydroxide grade ratio mixture, there is a large amount of precipitation generations, filtering, and the isometric water of filtrate is satisfied
With extracting n-butyl alcohol 3 times, combining extraction liquid.Extract liquor is concentrated into 100ml, adds in 4g activated carbons and 4g alkali aluminas, 90 DEG C
Heating stirring is decolourized for 10 minutes, and filtering is concentrated under reduced pressure, obtains flaxen Gardenoside crude product 19.6g, purity is
84.8%.
Above-mentioned obtained Gardenoside crude product 19.6g being dissolved in 78.4ml ethyl alcohol, 50 DEG C of heating stirrings are completely dissolved,
196ml ethyl acetate is added in, stirs evenly, is cooled to room temperature, when placement 12 is small in refrigerator, mass crystallization precipitation to be had.Filtering,
Filter cake is washed 2--4 times with the ethyl acetate of ice, drying, you can obtains the Gardenoside 17.0g that purity is 95.2%, yield is
80.9%.
Embodiment 5
The cape jasmine fruit that 500g is taken to dry, mechanical grinding is into fine powder, and with 60% ethanol solutions of 10L, 70 DEG C are heated to reflux
Filtrate is collected in 3h, filtering, and filter cake continues to extract, be repeated 3 times with 60% ethyl alcohol of 10L, and merging filtrate is simultaneously concentrated into no alcohol taste, adds
Deionized water is diluted to 2L, and the concentration of Gardenoside is 10g/L.The Gardenoside aqueous solution obtained will be extracted, cross macroporous resin column
HPD100A after end of the sample, is eluted using 20% ethanol solution, is collected 20% ethanol eluate, be concentrated to 250ml or so.It presses
The amount of 2ml/g adds in calcium oxide and sodium hydroxide grade ratio mixture solid, there is a large amount of precipitation generations, filtering, and filtrate is isometric
Water-saturated n-butanol extracts 3 times, combining extraction liquid.Extract liquor is concentrated into 100ml, adds in 4g activated carbons and 4g alkali aluminas,
90 DEG C of heating stirrings are decolourized for 10 minutes, and filtering is concentrated under reduced pressure, obtains flaxen Gardenoside crude product 19.6g, purity is
84.8%.
Above-mentioned obtained Gardenoside crude product 19.6g being dissolved in 39.2ml methanol, 50 DEG C of heating stirrings are completely dissolved,
196ml ethyl acetate is added in, stirs evenly, is cooled to room temperature, when placement 12 is small in refrigerator, mass crystallization precipitation to be had.Filtering,
Filter cake is washed 2--4 times with the methyl acetate of ice, drying, you can obtains the Gardenoside 17.2g that purity is 95.6%, yield is
82.2%.
Embodiment 5
Help influence of the precipitating reagent for Gardenoside yield and purity.Change settling agent species in embodiment 3, other conditions are not
Become, experimental result is as shown in table 1, wherein it is 1 that mixing, which helps the ratio of precipitating reagent,：1g/g.
Influence of 1 settling agent of table to 3 products obtained therefrom of Gardenoside purification step
By result of the test as can be seen that with sodium hydroxide and calcium oxide (1：It is 1g/g) settling agent, the yield of Gardenoside
And purity is preferable, up to 84.8%, acquisition product purity is significantly better than the macroreticular resin used at present and refines purity after recrystallization
Method.
Embodiment 6
Influence of the recrystallization solvent for Gardenoside yield and purity, preferably sodium hydroxide and calcium oxide (1：It is 1g/g) to help
Heavy agent, condition changes the species of recrystallization solvent with reference to described in embodiment 3, and other conditions are constant, the product that experimental result obtains
Data are as shown in table 2
Influence of the selection of 2 recrystallization solvent of table to final Gardenoside quality
By result of the test as can be seen that using volume ratio as 1：20 methanol and the mixed solvent of ethyl acetate are recrystallization
Solvent, the purity of Gardenoside is preferable, and purity is up to 95.6% after recrystallization.Have the time short compared with existing process for purification, imitate
The advantages of rate is high, and product purity is high.
Claims (10)
1. a kind of extraction for preparing high-purity gardenoside and process for purification, it is characterised in that：The method is specifically according to as follows
Step carries out：
(1) using cape jasmine fruit phytoclasts as raw material, with 60% ethanol water heating and refluxing extraction, after extraction, institute
Mixed liquor is obtained through removing ethyl alcohol and being concentrated to give Gardenoside crude extract medicinal extract；
(2) Gardenoside crude extract medicinal extract obtained by step (1) is added in into the Gardenoside crude extract medicinal extract that deionized water is configured to 10g/L
Aqueous solution crosses macroporous resin column HPD100A, after end of the sample, is eluted using 20% ethanol solution as eluant, eluent, collection 20%
The eluent of ethanol solution is concentrated to give Gardenoside concentrate；
(3) excessive settling agent is added in into concentrate obtained by step (2), sediment is precipitated in adjustment pH value to 9~14, and removal is heavy
It forms sediment, remaining reaction mixture is post-treated to obtain high-purity gardenoside；The settling agent for magnesia, alkali alumina,
In calcium oxide, calcium carbonate, sodium carbonate, sodium acid carbonate, potassium carbonate, saleratus, lithium hydroxide, sodium hydroxide, potassium hydroxide
A kind of or arbitrary several combination.
2. the method as described in claim 1, it is characterised in that：In step (1), the extraction repeats to carry at a reflux temperature
Take 3 times, every time 3 it is small when, merge the extracting solution of 3 times for mixed liquor, after extraction, gained mixed liquor filtered, collect filtrate,
Gained filter cake continues extraction 3 times with 60% ethyl alcohol again, merges all filtrates and is concentrated into no alcohol taste, obtains the leaching of Gardenoside crude extract
Cream.,
3. the method as described in claim 1, it is characterised in that：In step (1), the addition of the ethanol water is with institute
The quality for the cape jasmine fruit phytoclasts addition stated is calculated as 20ml/g.
4. the method as described in claim 1, it is characterised in that：In step (2), the relative density of the Gardenoside concentrate
For 0.92~1.01.
5. the method as described in claim 1, it is characterised in that：In step (3), the post-processing approach of the reaction mixture
For：After reaction, the filtrate that gained reaction mixture is obtained by filtration is extracted 1~9 time with isometric organic solvent, merges extraction
Liquid by the concentration of gained extract liquor, bleaching agent bleaching, is dried under reduced pressure, the solid of gained is recrystallized, dry, obtains high-purity Cape jasmine
Sub- glycosides；The organic solvent is C3-5Aliphatic monobasic alcohol.
6. method as claimed in claim 5, it is characterised in that：In step (3), the decolorising agent is inhaled for activated carbon and auxiliary
The mixture of attached dose of arbitrary proportion, the activated carbon shape is graininess, powdery or column, during the additional adsorbents are
One or more of property aluminium oxide, alkali alumina, silica gel, diatomite or Emathlite；It is described in the decolorising agent
Activated carbon and the amount ratio of aided bleaching agent 1：0.1-5.
7. the method as described in claim 1, it is characterised in that：In step (3), the settling agent is that mass ratio is 1:1
The mixture of sodium hydroxide and calcium oxide.
8. method as claimed in claim 5, it is characterised in that：In step (3), the recrystallization process is：It will be described
Solid is dissolved in mixed solvent at 50-70 DEG C, then stood still for crystals at -18-5 DEG C 24 it is small when, filtering, gained filter cake through mixing
Solvent washs 2~4 times, is dried under reduced pressure and obtains high-purity gardenoside；The mixed solvent is methanol, ethyl alcohol, isopropanol, just
The combination of arbitrary two kinds of organic solvents in propyl alcohol, n-butanol, methyl acetate, ethyl acetate, acetone or dichloromethane；Described
The addition of mixed solvent is calculated as 2-10ml/g with the quality of the solid.
9. method as claimed in claim 8, it is characterised in that：In step (3), the mixed solvent is methanol, ethyl alcohol, different
Arbitrary two kinds in propyl alcohol, normal propyl alcohol, n-butanol, methyl acetate, ethyl acetate, acetone or dichloromethane are 10 by volume:
1-1:The combination of the organic solvent of 20 ratio mixing.
10. method as claimed in claim 9, it is characterised in that：In step (3), the mixed solvent is that volume ratio is 1：
20 methanol and the mixed solvent of ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711494766.XA CN108047289A (en) | 2017-12-31 | 2017-12-31 | A kind of extraction for preparing high-purity gardenoside and process for purification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711494766.XA CN108047289A (en) | 2017-12-31 | 2017-12-31 | A kind of extraction for preparing high-purity gardenoside and process for purification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108047289A true CN108047289A (en) | 2018-05-18 |
Family
ID=62129491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711494766.XA Pending CN108047289A (en) | 2017-12-31 | 2017-12-31 | A kind of extraction for preparing high-purity gardenoside and process for purification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108047289A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115813829A (en) * | 2022-12-29 | 2023-03-21 | 云南云科特色植物提取实验室有限公司 | Preparation method and application of gardenia extract |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1706859A (en) * | 2005-05-24 | 2005-12-14 | 中国人民解放军第二军医大学 | Process of preparing high-purity jasminodin with Cape jasmine fruit |
| CN101880300A (en) * | 2010-04-27 | 2010-11-10 | 南京泽朗农业发展有限公司 | Purification process of geniposide |
| CN102212092A (en) * | 2011-05-31 | 2011-10-12 | 广西大学 | Preparation method for high-purity jasminoidin |
| CN102212091A (en) * | 2011-04-19 | 2011-10-12 | 肖文辉 | High-purity geniposide as well as preparation and clinical application of preparations thereof |
| CN102344692A (en) * | 2011-08-10 | 2012-02-08 | 浙江工业大学 | Method for extracting gardenia yellow pigment from gardeniae longicarpae fruit |
| CN102399251A (en) * | 2011-12-20 | 2012-04-04 | 广西大学 | Method for preparing high-purity geniposide |
| CN104497076A (en) * | 2014-11-05 | 2015-04-08 | 潜江市绿海宝生物技术有限公司 | Preparation purification method for high-purity geniposide |
| CN105273014A (en) * | 2015-11-12 | 2016-01-27 | 云南麦瑞科生物科技有限公司 | Preparation method of high-content geniposide crystals |
-
2017
- 2017-12-31 CN CN201711494766.XA patent/CN108047289A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1706859A (en) * | 2005-05-24 | 2005-12-14 | 中国人民解放军第二军医大学 | Process of preparing high-purity jasminodin with Cape jasmine fruit |
| CN101880300A (en) * | 2010-04-27 | 2010-11-10 | 南京泽朗农业发展有限公司 | Purification process of geniposide |
| CN102212091A (en) * | 2011-04-19 | 2011-10-12 | 肖文辉 | High-purity geniposide as well as preparation and clinical application of preparations thereof |
| CN102212092A (en) * | 2011-05-31 | 2011-10-12 | 广西大学 | Preparation method for high-purity jasminoidin |
| CN102344692A (en) * | 2011-08-10 | 2012-02-08 | 浙江工业大学 | Method for extracting gardenia yellow pigment from gardeniae longicarpae fruit |
| CN102399251A (en) * | 2011-12-20 | 2012-04-04 | 广西大学 | Method for preparing high-purity geniposide |
| CN104497076A (en) * | 2014-11-05 | 2015-04-08 | 潜江市绿海宝生物技术有限公司 | Preparation purification method for high-purity geniposide |
| CN105273014A (en) * | 2015-11-12 | 2016-01-27 | 云南麦瑞科生物科技有限公司 | Preparation method of high-content geniposide crystals |
Non-Patent Citations (6)
| Title |
|---|
| 卓家雄: "栀子中栀子苷的高效分离方法研究", 《中国优秀博硕士学位论文全文数据库（硕士）工程科技Ⅰ辑》 * |
| 史高杨: "《有机化学实验》", 31 August 2016 * |
| 吴梧桐: "《生物制药工艺学》", 31 August 2015 * |
| 张丽茹等: "栀子中京尼平苷的分离及其含量测定", 《中草药》 * |
| 李丽华等: "《天然药物化学实验教程》", 30 June 2017, 中国医药科技出版社 * |
| 王永敏等: "《生物化学》", 28 February 2017, 中国轻工业出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115813829A (en) * | 2022-12-29 | 2023-03-21 | 云南云科特色植物提取实验室有限公司 | Preparation method and application of gardenia extract |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108516997A (en) | A method of extracting Rubusoside from sweet tea | |
| CN105294790A (en) | Method for extracting high-purity steviol glycosides from stevia rebaudiana | |
| CN108752231B (en) | Method for extracting theanine from sweet tea and simultaneously extracting rubusoside and tea polyphenol | |
| CN102423329B (en) | A kind of discoloration method of panax notoginsenoside extract | |
| CN103951718A (en) | Method used for preparing high-purity gardenoside and crocin from gardenia jasminoides ellis | |
| CN110407890A (en) | The preparation method of sapindoside | |
| CN109180755A (en) | A method of extracting Rubusoside from sweet tea | |
| CN109134560A (en) | A method of extracting anthocyanin from Roselle calyx | |
| WO2022057603A1 (en) | Method for extracting coenzyme q10 from fermentation broth of coenzyme q10 | |
| CN103058871B (en) | Separation and purification method of tobacco chlorogenic acid | |
| CN101732398A (en) | Method for extracting gypenosides | |
| CN106832037A (en) | A kind of notoginseng polysaccharide extracting method rapidly and efficiently | |
| CN108047289A (en) | A kind of extraction for preparing high-purity gardenoside and process for purification | |
| CN112266399B (en) | High-purity separation and extraction method of epimedium extract | |
| CN108822164A (en) | The preparation process of high quality monosialotetrahexose ganglioside sodium | |
| CN107011405B (en) | A kind of preparation method of Panaxatriol saponin | |
| CN104788509B (en) | A kind of technique extracting preparation high-purity Raffinose from defatted wheat germ | |
| CN111072747A (en) | Ginsenoside and ultrasonic extraction method thereof | |
| CN109400566A (en) | A method of extracting separating high-purity amentoflavone from Rock lily plant | |
| CN108586440A (en) | The purification process of Puerarin | |
| CN108976193A (en) | A kind of Osthole extracting method | |
| CN105418708B (en) | A kind of method that residual abamectin B1a is extracted in the primary crystallization mother liquor from Avermectin B1a | |
| CN108341846A (en) | A kind of technique of the separation and Extraction arctiin from great burdock achene | |
| CN113861248A (en) | Method for treating heavy metals in pomegranate peel extracting solution and purifying punicalagin | |
| CN102898864B (en) | Method for refining gardenia yellow pigment by adopting solvent crystallization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180518 |
|
| RJ01 | Rejection of invention patent application after publication |