CN107663200A - A kind of silymarin gradient extracting method using ethyl acetate - Google Patents
A kind of silymarin gradient extracting method using ethyl acetate Download PDFInfo
- Publication number
- CN107663200A CN107663200A CN201610609494.2A CN201610609494A CN107663200A CN 107663200 A CN107663200 A CN 107663200A CN 201610609494 A CN201610609494 A CN 201610609494A CN 107663200 A CN107663200 A CN 107663200A
- Authority
- CN
- China
- Prior art keywords
- extractor
- extraction
- extract solution
- ethyl acetate
- silymarin
- 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
- C07D—HETEROCYCLIC COMPOUNDS
- C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
- C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
- C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
Itself relate to a kind of extracting method of silymarin, it is characterised in that including：Silybum marianum seed addition hulling machine is shelled；Milk thistle shell and ethyl acetate are loaded into pot group type gradient extraction equipment；Gradient extraction is carried out to milk thistle shell, obtains the first extract solution of silymarin；First extract solution is carried out to be concentrated to give milk thistle concentrate；Aqueous alkali is added into the concentrate, stirs, staticly settles；The precipitation is filtered, dry, pulverize sieving, and then obtain silymarin.The mode of gradient extraction has been used using application scheme, the recovery rate of extraction silymarin has been improved, reduces energy consumption and production cost.
Description
Technical field
The present embodiments relate to a kind of production method, more particularly to a kind of production method of silymarin.
Background technology
Silymarin is the mixture of flavanolignan's class compound, and source is composite family Silybum plant milk thistle
The seed of (Silybum marianum).Its main component includes legalon, Isosilybin, dehydro-silibinin, fine grinding
The Flavonoid substances such as Ji booth and silydianin.Silymarin has hepatic cholagogic effect, is mainly used in the treatment of hepatopathy.Secondly,
It also has obvious anti peroxidation of lipid, radioresistance, removes the effect such as free radical, anti-gastric-ulcer.In reducing blood lipid, preventing and treating artery congee
Sample hardening, prevention cerebral ischemia, anti-platelet aggregation etc. have good effect.It is nontoxic, without teratogenesis and mutagenesis.
The extracting method of silymarin mainly has two kinds at present, and one kind is organic solvent extraction, and one kind is that alkali carries acid is heavy
Method.Wherein in the prior art, the step of organic solvent extraction generally use is first to crush silybum marianum seed, by overcritical
After fluid extraction proposes grease, then extracted with ethyl acetate, extract solution passes through supercritical CO2Abstraction impurity removal matter, and then obtain water
Fly silibin.The problem of this method, is after crushing silybum marianum seed, thoroughly can not extract wherein grease, will be to follow-up silymarin
DNA purity produce certain influence；Another technology is after silybum marianum seed is first shelled, then enters and entered using milk thistle shell
The extraction of row silymarin, the grease in silybum marianum seed is avoided to influence, but this method needs individually shelling, in extraction process
Middle extraction is not thorough, containing the silymarin not extracted thoroughly in the milk thistle dregs of rice, when obtaining same amount of silymarin, increases
The extraction time cost and financial cost added.
The content of the invention
The invention provides a kind of extracting method of silymarin, silymarin that can be in milk thistle shell is repeatedly carried
Take, improve the recovery rate of silymarin, the extraction efficiency that not only ensure that DNA purity but also improved.
The extracting method of silymarin of the present invention is specific as follows：
A kind of extracting method of silymarin, it is characterised in that including：
Silybum marianum seed addition hulling machine is shelled；
Milk thistle shell and ethyl acetate are loaded into pot group type gradient extraction equipment；
Gradient extraction is carried out to milk thistle shell, obtains the first extract solution of silymarin；
First extract solution is carried out to be concentrated to give milk thistle concentrate；
Aqueous alkali is added into the concentrate, stirs, staticly settles；
The precipitation is filtered, dry, pulverize sieving；
Wherein pot group type gradient extraction equipment includes the first extractor, the second extractor and the 3rd extractor, in each extractor
For Steam pressure control in 0.1-0.18Mpa, Extracting temperature is 40-65 DEG C, and gradient extraction includes the extraction of first order gradient and second
Gradient extracts two subgradient extraction process.
The extraction of two subgradients specifically includes：
First order gradient extraction step, the mixture of milk thistle shell and ethyl acetate is separately added into the first extractor, second carried
Take tank and the 3rd extractor；Standby after the filtering of first extractor first time extract solution, second of extract solution of the first extractor adds
Enter water or ethyl acetate；Then the solvent the second extract solution of the first extractor extracted as the first time of the second extractor,
The first extract solution filtering of second extractor is standby；The third time extract solution of first extractor is added into water or ethyl acetate, made
For the solvent of second of the second extractor extraction, water or ethyl acetate conduct are added in second of extract solution of the second extractor
The solvent of the first time extraction of 3rd extractor, the first extract solution filtering of the 3rd extractor are standby；
Second level gradient extraction step, merge the first extractor, the second extractor and the 3rd extraction in the extraction of first order gradient
Then the first extract solution in tank adds water or ethyl acetate carries out first time extraction into the 3rd extractor；By the 3rd extraction
Tank the first extract solution filtering after it is standby, by the second extract solution of the 3rd extractor into the second extractor, then add water or
Ethyl acetate carries out first time extraction, will be standby after the first extract solution filtering of the second extractor, by the 3rd of the 3rd extractor the
Secondary extract solution adds water or ethyl acetate, as the solvent of second of extraction of the second extractor, then by the second extractor
Second extract solution adds water or ethyl acetate, as the extractant of the first extractor extraction for the first time, by the of the first extractor
It is standby after the filtering of one extract solution.
The first extract solution in the first extractor, the second extractor and the 3rd extractor in merging second circulation, is obtained
First extract；
Reclaim ethyl acetate, the Extraction solvent as subsequent extracted；
Drying or natural drying carry out the milk thistle shell after gradient extraction, make its drying.
In the extraction of first order gradient, the water or the volume of ethyl acetate that add in extractor are the 3- of this extracting liquid volume
4 times.
In the gradient extraction of the second level, the water or the volume of ethyl acetate that add in extractor are the 2- of this extracting liquid volume
3 times.
The volume of the aqueous alkali is 3-10 times of the volume of concentrate, and the species of the aqueous alkali is hydroxide
One or more combination in potassium, sodium hydroxide, saleratus and sodium acid carbonate, the concentration of the aqueous alkali is 0.3%-
1.0%；Drying temperature is 50-70 DEG C in step S60, and drying time is 7-12 hours.
Preferably, the volume of the aqueous alkali is 5-7 times of the volume of concentrate, and the concentration of the aqueous alkali is
0.46%。
It is can be seen that from above-mentioned introduction using the method for the invention, the side of multistage gradient extraction carried out to milk thistle shell
Formula, the silymarin in milk thistle shell is sufficiently extracted, due to being to take multistage extracting mode, can parallel work-flow, and
Extraction time will not be extended, therefore this programme improves the whole efficiency and DNA purity of extraction silymarin.
【Brief description of the drawings】
Fig. 1 is the flow chart of present invention extraction silymarin.
Fig. 2 is step S30 specific execution flow chart.
Fig. 3 is present invention extraction silymarin and the data comparison figure of prior art.
【Embodiment】
For problems of the prior art, the extracting method of silymarin of the invention, gradient is used in extraction process
The mode of extraction, parallel multiple extraction is carried out to milk thistle shell, the recovery rate of silymarin can be improved, both ensure that extraction
The extraction efficiency that purity improves again.
In order that the object, technical solutions and advantages of the present invention are clearer, below in conjunction with the accompanying drawings with specific embodiment pair
The present invention is described in detail.
Fig. 1 is the flow chart of present invention extraction silymarin, as shown in figure 1, including implementation in detail below.
Step S10, silybum marianum seed addition hulling machine is shelled；
Silybum marianum seed is sent into hulling machine and shelled, and silybum marianum seed and milk thistle shell are separated, and collects milk thistle shell.Silybum marianum seed
For oil expression etc., milk thistle shell is used for the extraction of silymarin.
Step S20, milk thistle shell and ethyl acetate are loaded into pot group type gradient extraction equipment；
The concentration requirement of the ethyl acetate of addition is 75%-95%, and preferred concentration 80%-90%, ethyl acetate diluent is distillation
Water, ethyl acetate dosage are 3-5 times of milk thistle shell volume.Due to use gradient extracting mode, ethyl acetate is dense in the step
Degree need not use the ethyl acetate of 95% concentrations above, saved the dosage of extraction organic solvent, saved extraction cost,
Step S30, gradient extraction is carried out to milk thistle shell, obtains the first extract solution of silymarin；
Wherein pot group type gradient extraction equipment includes the first extractor, the second extractor and the 3rd extractor, in each extractor
For Steam pressure control in 0.1-0.18Mpa, Extracting temperature is 40-65 DEG C, and gradient extraction includes the extraction of first order gradient and second
Gradient extracts two subgradient extraction process.
This step is extracted using second order gradient, i.e., milk thistle shell is carried out twice in extractor group, it is noted that this
Invention is illustrated with second order gradient extraction, in actual extracting operation, can be selected according to specific extraction of substance and technological process
Select the extraction of one-level gradient or multistage gradient extraction.
Step S40, first extract solution is carried out being concentrated to give milk thistle concentrate；
The step is concentrated extract solution using the methods of negative pressure rectifying, obtains silymarin concentrate.
Step S50, aqueous alkali is added into the concentrate, stirs, staticly settles；
In this step, the volume of the aqueous alkali is 3-10 times of the volume of concentrate；Preferably 5-7 times, the alkali
The species of the aqueous solution is the one or more combination in potassium hydroxide, sodium hydroxide, saleratus and sodium acid carbonate；The buck
The concentration of solution is 0.3%-1.0%, preferred concentration 0.46%.
Step S60, the precipitation is filtered, dry, pulverize sieving；
Drying temperature in the step is 50-70 DEG C, and drying time is 7-12 hours.
Second order gradient extraction step in wherein step S30 as shown in Fig. 2
Comprise the following steps that：
Step S31, first order gradient extraction step, the mixture of milk thistle shell and ethyl acetate is separately added into the first extraction
Tank, the second extractor and the 3rd extractor；It is standby after the filtering of first extractor first time extract solution, second of the first extractor
Extract solution adds water or ethyl acetate；Then extracted the second extract solution of the first extractor as the first time of the second extractor
Solvent, the second extractor the first extract solution filtering it is standby；The third time extract solution of first extractor is added into water or acetic acid
Ethyl ester, as the solvent of second of extraction of the second extractor, water or acetic acid are added in second of extract solution of the second extractor
The solvent that ethyl ester extracts as the first time of the 3rd extractor, the first extract solution filtering of the 3rd extractor are standby；
The water or the volume of ethyl acetate that wherein add three times in extractor are 3-4 times that works as time extracting liquid volume
Step S32, second level gradient extraction step, merge the first extractor in the extraction of first order gradient, the second extractor and
Then the first extract solution in 3rd extractor adds water or ethyl acetate carries out first time extraction into the 3rd extractor；Will
It is standby after the first extract solution filtering of 3rd extractor, by the second extract solution of the 3rd extractor into the second extractor, then
Add water or ethyl acetate carries out first time extraction, will be standby after the first extract solution filtering of the second extractor, by the 3rd extraction
The third time extract solution of tank adds water or ethyl acetate, as the solvent of second of extraction of the second extractor, then by second
Second extract solution of extractor adds water or ethyl acetate, and as the extractant of the first extractor extraction for the first time, first is carried
Take the first extract solution of tank standby after filtering.
The volume for adding the water added three times in extractor or ethyl acetate is work as time extracting liquid volume 2-3 times
Step S33, the first extract solution in the first extractor in merging second circulation, the second extractor and the 3rd extractor,
Obtain first extract；
Step S34, ethyl acetate, the Extraction solvent as subsequent extracted are reclaimed；
Step S35, drying or natural drying carry out the milk thistle shell after gradient extraction, make its drying.
Wherein dried milk thistle shell may be used as him and use, and such as produce feed.
Based on above-mentioned extracting method, relevant comparative's embodiment of actual feed operation is as follows：
100 tons of milk thistle seeds shell through hulling machine, using common extracting mode, can obtain 3.92 tons of silymarin, usage time
For 13.5 hours.
Equally it is 100 tons of milk thistle seeds if the mode extracted using the gradient in the present invention, extraction time is 14 small
When or so, the concentrate drying time is identical, finally gives silymarin as 4.39 tons.
As shown in figure 3, in the case where materials and output silymarin are essentially identical, the present invention uses specific data comparison
Gradient extracting method can greatly improve extraction sales volume, so that 100 tons of milk thistle seeds extract as an example, each extraction process is big
Consumption of making an appointment is substantially the same, but is improved in unit mass milk thistle seed, the extracted amount of silymarin, is reduced simultaneously
Power consumption, the consumption of ethyl acetate is reduced, therefore the solution of the present invention greatly improves production efficiency, reduces simultaneously
The energy consumption of specific yield, meet the national policy of current energy-saving and emission-reduction.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God any modification, equivalent substitution and improvements done etc., should be included within the scope of protection of the invention with principle.
Claims (7)
- A kind of 1. extracting method of silymarin, it is characterised in that including：Step S10, silybum marianum seed addition hulling machine is shelled；Step S20, milk thistle shell and ethyl acetate are loaded into pot group type gradient extraction equipment；Step S30, gradient extraction is carried out to milk thistle shell, obtains the first extract solution of silymarin；Step S40, first extract solution is carried out being concentrated to give silymarin concentrate；Step S50, aqueous alkali is added into the concentrate, stirs, staticly settles；Step S60, the precipitation is filtered, dry, pulverize sieving；In wherein step S30, pot group type gradient extraction equipment includes the first extractor, the second extractor and the 3rd extractor, often For Steam pressure control in 0.1-0.18Mpa, Extracting temperature is 40-65 DEG C in individual extractor, and gradient extraction includes first order gradient Extraction and the second gradient extract two subgradient extraction process.
- 2. extracting method according to claim 1, it is characterised in that step S30 two subgradients extraction specifically includes：Step S31, first order gradient extraction step, the mixture of milk thistle shell and ethyl acetate is separately added into the first extraction Tank, the second extractor and the 3rd extractor；It is standby after the filtering of first extractor first time extract solution, second of the first extractor Extract solution adds water or ethyl acetate；Then extracted the second extract solution of the first extractor as the first time of the second extractor Solvent, the second extractor the first extract solution filtering it is standby；The third time extract solution of first extractor is added into water or acetic acid Ethyl ester, as the solvent of second of extraction of the second extractor, water or acetic acid are added in second of extract solution of the second extractor The solvent that ethyl ester extracts as the first time of the 3rd extractor, the first extract solution filtering of the 3rd extractor are standby；Step S32, second level gradient extraction step, merge the first extractor in the extraction of first order gradient, the second extractor and Then the first extract solution in 3rd extractor adds water or ethyl acetate carries out first time extraction into the 3rd extractor；Will It is standby after the first extract solution filtering of 3rd extractor, by the second extract solution of the 3rd extractor into the second extractor, then Add water or ethyl acetate carries out first time extraction, will be standby after the first extract solution filtering of the second extractor, by the 3rd extraction The third time extract solution of tank adds water or ethyl acetate, as the solvent of second of extraction of the second extractor, then by second Second extract solution of extractor adds water or ethyl acetate, and as the extractant of the first extractor extraction for the first time, first is carried Take the first extract solution of tank standby after filtering.
- 3. extracting method according to claim 2, it is characterised in that after step S32, in addition to：Step S33, the first extract solution in the first extractor in merging second circulation, the second extractor and the 3rd extractor, Obtain silymarin first extract；Step S34, ethyl acetate, the Extraction solvent as subsequent extracted are reclaimed；Step S35, drying or natural drying carry out the milk thistle shell after gradient extraction, make its drying.
- 4. the extracting method according to Claims 2 or 3, it is characterised in that in step S31, add extractor in water or The volume of ethyl acetate is 3-4 times of this extracting liquid volume.
- 5. the extracting method according to Claims 2 or 3, it is characterised in that in step S32, add extractor in water or The volume of ethyl acetate is 2-3 times of this extracting liquid volume.
- 6. extracting method according to claim 1, it is characterised in that the volume of aqueous alkali described in step S50 is institute State the volume of concentrate 3-10 times, the species of the aqueous alkali is potassium hydroxide, sodium hydroxide, saleratus and sodium acid carbonate In one or more combination, the concentration of the aqueous alkali is 0.3%-1.0%；Drying temperature is 50-70 in step S60 DEG C, drying time is 7-12 hours.
- 7. extracting method according to claim 6, it is characterised in that the volume of the aqueous alkali is the concentrated liquid Long-pending 5-7 times, the concentration of the aqueous alkali is 0.46%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610609494.2A CN107663200A (en) | 2016-07-29 | 2016-07-29 | A kind of silymarin gradient extracting method using ethyl acetate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610609494.2A CN107663200A (en) | 2016-07-29 | 2016-07-29 | A kind of silymarin gradient extracting method using ethyl acetate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107663200A true CN107663200A (en) | 2018-02-06 |
Family
ID=61114535
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610609494.2A Pending CN107663200A (en) | 2016-07-29 | 2016-07-29 | A kind of silymarin gradient extracting method using ethyl acetate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107663200A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020535132A (en) * | 2017-09-22 | 2020-12-03 | エウロメッド・エセ・ア | Oazami extract with improved solubility |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079745A (en) * | 2009-12-01 | 2011-06-01 | 白心亮 | Production method of silymarin |
| CN102816155A (en) * | 2012-07-27 | 2012-12-12 | 宁波立华植物提取技术有限公司 | Preparation method of silymarin |
| CN102924438A (en) * | 2012-10-30 | 2013-02-13 | 晨光生物科技集团股份有限公司 | Method for extracting silymarin and silybum mariamum oil from silybum mariamum seed |
| CN104650051A (en) * | 2014-01-17 | 2015-05-27 | 吴长军 | Method for extracting silymarin by using ethyl acetate as extraction solvent |
-
2016
- 2016-07-29 CN CN201610609494.2A patent/CN107663200A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079745A (en) * | 2009-12-01 | 2011-06-01 | 白心亮 | Production method of silymarin |
| CN102816155A (en) * | 2012-07-27 | 2012-12-12 | 宁波立华植物提取技术有限公司 | Preparation method of silymarin |
| CN102924438A (en) * | 2012-10-30 | 2013-02-13 | 晨光生物科技集团股份有限公司 | Method for extracting silymarin and silybum mariamum oil from silybum mariamum seed |
| CN104650051A (en) * | 2014-01-17 | 2015-05-27 | 吴长军 | Method for extracting silymarin by using ethyl acetate as extraction solvent |
Non-Patent Citations (2)
| Title |
|---|
| 李玉山，等: "水飞蓟素提取纯化工艺研究", 《化学工程师》 * |
| 王沛: "《药物制剂设备》", 31 January 2016, 中国医药科技出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2020535132A (en) * | 2017-09-22 | 2020-12-03 | エウロメッド・エセ・ア | Oazami extract with improved solubility |
| US11819528B2 (en) | 2017-09-22 | 2023-11-21 | Euromed, S.A. | Enhanced solubility of milk thistle extract |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104530173B (en) | A kind of extract the technique of tea saponin in cake of camellia oleifera seeds | |
| CN102060728A (en) | Method for extracting capsorubin and capsaicin from chillies | |
| CN105903227B (en) | lavender absolute oil and preparation method thereof | |
| CN108741078A (en) | The processing method for preparing the method and linseed of flaxseed gum, flax lignan, flax dietary fiber and flax protein powder | |
| CN103461645A (en) | Preparation method of cottonseed protein | |
| CN104726197B (en) | The method of extracting cigarette seed oil is discarded in cigarette seed using homogenate extraction technology from Turkish tobaccos | |
| CN107663200A (en) | A kind of silymarin gradient extracting method using ethyl acetate | |
| CN107698572A (en) | A kind of extracting method of silymarin | |
| CN104606288B (en) | The preparation method of Scullcap total-flavonoid aglycone extract | |
| CN104292294B (en) | A kind of method of purification of sapindust saponin | |
| CN103783255A (en) | Method for extracting protein from byproduct of oil extraction of snakegourd fruit seeds | |
| CN103621688A (en) | Rice bran oil with effects of promoting blood circulation and bodybuilding | |
| CN102326669A (en) | Process for preparing white fish meal by dehydrating and degreasing at low temperature at one time | |
| CN106188020A (en) | A kind of silymarin gradient extracting method using ethanol | |
| CN104370992B (en) | A kind of from Glossy Privet Fruit, extract ursolic acid and the method for Oleanolic Acid mixture | |
| CN106243095A (en) | A kind of method using ethyl acetate to extract silymarin | |
| CN107663201A (en) | A kind of method that silymarin is extracted using ethanol | |
| CN106008484B (en) | A kind of extracting method of silymarin | |
| CN103829123A (en) | Method for producing hypoglycemic hypolipemic product by using tartary buckwheat | |
| CN105859699A (en) | Preparation method of silymarin | |
| CN105748570A (en) | Ultrasonic-assisted method for extracting total flavonoid in alfalfa | |
| CN107115488A (en) | Preparation containing curcumin and preparation method thereof | |
| CN105801665B (en) | A kind of method that protodioscin is extracted in the plant from Chinese yam | |
| CN109721666A (en) | A kind of ultrasonic auxiliary extraction method of Sphallerocerpus gracilis polysaccharide | |
| CN107964453A (en) | The method for preparing grease again from the dry shrimp slag of krill degreasing |
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 | ||
| CB02 | Change of applicant information |
Address after: 028400 no.0427, Dongjiao Industrial Park, Kailu Town, Kailu County, Tongliao City, Inner Mongolia Autonomous Region Applicant after: Inner Mongolia Changhui Biotechnology Co., Ltd. Address before: 011517 the Inner Mongolia Autonomous Region Helingeer County of Hohhot city Shengle Economic Zone Applicant before: Inner Mongolia Changhui Biotechnology Co., Ltd. |
|
| CB02 | Change of applicant information | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180206 |
|
| RJ01 | Rejection of invention patent application after publication |