CN107663201A - A kind of method that silymarin is extracted using ethanol - Google Patents
A kind of method that silymarin is extracted using ethanol Download PDFInfo
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- CN107663201A CN107663201A CN201610609946.7A CN201610609946A CN107663201A CN 107663201 A CN107663201 A CN 107663201A CN 201610609946 A CN201610609946 A CN 201610609946A CN 107663201 A CN107663201 A CN 107663201A
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- ethanol
- silybum marianum
- extracting method
- marianum seed
- milk thistle
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- 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
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- Medicines Containing Plant Substances (AREA)
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Abstract
The application is related to a kind of extracting method of silymarin, it is characterised in that comprises the following steps：Silybum marianum seed is soaked into the scheduled time in ethanol；Silybum marianum seed is taken out from ethanol, hulling machine is added, silybum marianum seed is shelled；Milk thistle shell is loaded into rotocel extractor, ethanol and diluent are added into rotocel extractor；Extract and 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 process for eliminating softening and immersion using application scheme, improves the whole efficiency of extraction silymarin, 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 ethanol, extract solution passes through supercritical CO2Abstraction impurity removal matter, and then obtain milk thistle
Element.The problem of this method, is after crushing silybum marianum seed, thoroughly can not extract wherein grease, follow-up silymarin will be carried
Purity is taken to produce certain influence；Another technology is after silybum marianum seed is first shelled, then enters and enter water-filling using milk thistle shell
Fly the extraction of silibin, avoid the grease in silybum marianum seed from influenceing, but this method needs individually shelling, then milk thistle shell will
The program such as softening, immersion can just carry out the extraction of silymarin, great increased abstraction process, increased extraction time cost
And financial cost.
The content of the invention
The invention provides a kind of extracting method of silymarin, and grease in silybum marianum seed can be avoided to carry silymarin
The influence taken, while the step of softening milk thistle shell can be removed from, 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 is soaked into the scheduled time in ethanol；
Silybum marianum seed is taken out from ethanol, hulling machine is added, silybum marianum seed is shelled；
Milk thistle shell is loaded into rotocel extractor, ethanol and diluent are added into rotocel extractor；
Extract and 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, the volume of the aqueous alkali is 3-10 times of the volume of concentrate, and the species of the aqueous alkali is
One or more combination in potassium hydroxide, sodium hydroxide, saleratus and sodium acid carbonate, the concentration of the aqueous alkali are
0.3%-1.0%, drying temperature are 50-70 DEG C, and drying time is 7-12 hours.
Wherein, by silybum marianum seed and 98% ethanol according to weight 1:The proportioning mixing immersion 1-2 hours of (0.8-1.2), make
Milk thistle shell fully softens and separated with silybum marianum seed.
Preferably, silybum marianum seed and ethanol are according to weight 1:1 proportioning mixing, soak time are 1 hour.
Using filter by silybum marianum seed and separation of ethanol, the silybum marianum seed of epidermis softening is sent into hulling machine and taken off
Shell, the operating ambient temperature of hulling machine is 20-50 DEG C, and humidity is more than 70%.
It is collected into the 40-50% of the weight of milk thistle shell than generally accounting for silybum marianum seed weight before shelling.
Ethanol and diluent agent are added into rotocel extractor, the wherein concentration of the ethanol in rotocel extractor is 70%-90%.
Preferred concentration is 75%-80%, and diluent is distilled water.
The temperature of the rotocel extractor is 50-60 DEG C, rotating speed 10-40r/min, continuous spray extraction 4-6 hours, is obtained
To extract solution, then concentrated step obtains silymarin concentrate.
Wherein, the volume of the aqueous alkali is 5-7 times of the volume of concentrate.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, silybum marianum seed can be soaked first, make fine grinding
Ji shell is softened and fully contacted with ethanol in advance, then carries out the extraction of silymarin, because ethanol is immiscible with grease,
Silybum marianum seed can equally carry out the extraction of grease after immersion, and milk thistle shell has been had ethanol to soften and contact, and is eliminated
Softening and the process of immersion, improve the whole efficiency of extraction silymarin.
【Brief description of the drawings】
Fig. 1 is the flow chart of present invention extraction silymarin.
Fig. 2 is present invention extraction silymarin and the data comparison figure of prior art.
【Embodiment】
For problems of the prior art, a kind of extracting method of silymarin, grease pair in silybum marianum seed can be avoided
The influence of silymarin extraction, while the step of softening milk thistle shell can be removed from, it not only ensure that DNA purity but also that improves carry
Take efficiency.
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 is soaked into the scheduled time in ethanol；In this step, by silybum marianum seed and 98% second
Alcohol is according to weight 1:The proportioning mixing immersion 1-2 hours of (0.8-1.2), milk thistle shell is set fully to soften and divide with silybum marianum seed
From preferable silybum marianum seed is with ethanol according to weight 1:1 proportioning mixing, soak time are 1 hour.Due in advance by milk thistle
Seed contacts with ethanol, avoids follow-up the step of individually softening milk thistle shell, while milk thistle shell can be made fully to be connect with ethanol
Touch.
Step S20, silybum marianum seed is taken out from ethanol, adds hulling machine, silybum marianum seed is shelled；In the step, lead to
Filter is crossed by silybum marianum seed and separation of ethanol, ethanol is collected into containers for future use, the silybum marianum seed of epidermis softening is sent into
Hulling machine is shelled, and collects milk thistle shell.Because milk thistle shell has softened, therefore the process that shells also is relatively easy to.Wherein receive
Collect the 40-50% of the weight of milk thistle shell than generally accounting for silybum marianum seed weight before shelling, the working environment of shelling maintains the temperature at
20-50 DEG C, humidity is maintained at more than 70%, to ensure the soft state of milk thistle shell.
Step S30, milk thistle shell is loaded into rotocel extractor, ethanol and diluent is added into rotocel extractor；By step
Ethanol is collected in S20 and diluent adds rotocel extractor, while in order to ensure the concentration of ethanol according to last concentration and matter
Ratio requirement is measured, a certain amount of ethanol can be also individually added on the basis of S20 is collected into ethanol, is wherein passed through in rotocel extractor
The concentration requirement of ethanol after dilution is 70%-90%, and preferred concentration 75%-80%, diluent is distilled water.Due to making water in advance
Fly Ji shell to contact with ethanol, therefore concentration of alcohol need not use the ethanol of 95% concentrations above in rotocel extractor, save extraction
The dosage of organic solvent, has saved extraction cost.
Step S40, extract and be concentrated to give milk thistle concentrate；In this step, the temperature of the rotocel extractor is adjusted
Spend for 50-60 DEG C, rotating speed 10-40r/min, continuous spray, extract 4-6 hours, obtain extract solution.Then negative pressure rectifying is passed through
The methods of extract solution is concentrated, obtain silymarin concentrate.
Step S50, aqueous alkali is added into the concentrate, stirs, staticly settles；In this step, the buck
The volume of solution is 3-10 times of the volume of concentrate；Preferably 5-7 times, the species of the aqueous alkali is potassium hydroxide,
One or more combination in sodium hydroxide, saleratus and sodium acid carbonate；The concentration of the aqueous alkali is 0.3%-
1.0%, preferred concentration 0.46%.
Step S60, the precipitation is filtered, dry, pulverize sieving.
Drying temperature in the step S60 is 50-70 DEG C, and drying time is 7-12 hours.
Based on above-mentioned extracting method, relevant comparative's embodiment of actual feed operation is as follows：
100 tons of milk thistle seeds are after ethanol soaks 1 hour, hulling machine shelling, 65.5 tons of the milk thistle shell softened.Flat turn
Infuser extracts, and charge is the 70% of material lattice, and 80% ethanol is as extractant, 55-60 DEG C of temperature, rotating speed 30r/min, continuously
Spray, extract 4-6 hours.Extract solution is concentrated into 50m3, add 50 DEG C of 0.3% potassium hydroxide aqueous solution 300m3, quickly stir 0.5
Hour, it is washed to neutrality after settling centrifugation in 0.5 hour, 70 DEG C of dryings 10 hours, pulverizes and sieves.Obtain 3.9 tons of silymarin.
If using the present invention first silybum marianum seed shells, then soften the mode extracted again, be equally 100 tons of fine grindings
Ji seed, softening milk thistle shell need 1 hour, and the extraction time in rotocel extractor is usually 6-10 hours, during concentrate drying
Between it is identical, finally give silymarin as 3.95 tons.
As shown in Fig. 2 in the case where materials and output silymarin are essentially identical, the present invention uses specific data comparison
Extracting method can great less extraction time, so that 100 tons of milk thistle seeds extract as an example, each extraction process about may be used
3-5 hours are saved, greatly improve production efficiency, simultaneously because reducing the process of softening milk thistle shell, reduces electric energy and disappears
Consumption, while reduce the consumption of ethanol, it is seen that extraction scheme of the invention can reduce energy consumption, meet energy-conservation at present and subtract
The national policy of row.
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 (10)
- A kind of 1. extracting method of silymarin, it is characterised in that including：Step S10, silybum marianum seed is soaked into the scheduled time in ethanol；Step S20, silybum marianum seed is taken out from ethanol, adds hulling machine, silybum marianum seed is shelled；Step S30, milk thistle shell is loaded into rotocel extractor, ethanol and diluent is added into rotocel extractor；Step S40, extract and be concentrated to give milk thistle concentrate；Step S50, aqueous alkali is added into the concentrate, stirs, staticly settles；Step S60, the precipitation is filtered, dry, pulverize sieving；Wherein, the volume of aqueous alkali described in step S50 is 3-10 times of the volume of concentrate, the kind of the aqueous alkali Class be potassium hydroxide, sodium hydroxide, saleratus and sodium acid carbonate in one or more combination, the concentration of the aqueous alkali For 0.3%-1.0%；Drying temperature is 50-70 DEG C in step S60, and drying time is 7-12 hours.
- 2. extracting method according to claim 1, it is characterised in that step S10 is specifically, by silybum marianum seed and 98% Ethanol is according to weight 1:The proportioning mixing immersion 1-2 hours of (0.8-1.2), milk thistle shell is set fully to soften and divide with silybum marianum seed From.
- 3. extracting method according to claim 2, it is characterised in that silybum marianum seed is with ethanol according to weight 1:1 proportioning Mixing, soak time are 1 hour.
- 4. extracting method according to claim 1, it is characterised in that step S20 is specifically, using filter by milk thistle Seed and separation of ethanol, the silybum marianum seed of epidermis softening is sent into hulling machine and shelled, the operating ambient temperature of hulling machine is 20- 50 DEG C, humidity is more than 70%.
- 5. extracting method according to claim 4, it is characterised in that the weight for being collected into milk thistle shell than generally accounts for shelling The 40-50% of preceding silybum marianum seed weight.
- 6. extracting method according to claim 1, it is characterised in that step S30 is specifically, ethanol and diluent are added The concentration of ethanol in rotocel extractor, wherein rotocel extractor is 70%-90%.
- 7. extracting method according to claim 6, it is characterised in that the concentration of the ethanol in rotocel extractor is 75%- 80%, diluent is distilled water.
- 8. extracting method according to claim 1, it is characterised in that step S40 is specifically, the temperature of the rotocel extractor Spend for 50-60 DEG C, rotating speed 10-40r/min, continuous spray extraction 4-6 hours, obtain extract solution, then concentrated step obtains To silymarin concentrate.
- 9. extracting method according to claim 1, it is characterised in that the volume of the aqueous alkali is the concentrated liquid Long-pending 5-7 times.
- 10. extracting method according to claim 9, it is characterised in that the concentration of the aqueous alkali is 0.46%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610609946.7A CN107663201A (en) | 2016-07-29 | 2016-07-29 | A kind of method that silymarin is extracted using ethanol |
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| CN201610609946.7A CN107663201A (en) | 2016-07-29 | 2016-07-29 | A kind of method that silymarin is extracted using ethanol |
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| CN107663201A true CN107663201A (en) | 2018-02-06 |
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| CN201610609946.7A Pending CN107663201A (en) | 2016-07-29 | 2016-07-29 | A kind of method that silymarin is extracted using ethanol |
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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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079745A (en) * | 2009-12-01 | 2011-06-01 | 白心亮 | Production method of silymarin |
-
2016
- 2016-07-29 CN CN201610609946.7A patent/CN107663201A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079745A (en) * | 2009-12-01 | 2011-06-01 | 白心亮 | Production method of silymarin |
Non-Patent Citations (2)
| Title |
|---|
| 叶定江，等: "《中药炮制学辞典》", 30 June 2005, 上海科学技术出版社 * |
| 吴建华: "《中药炮制学实验指导》", 30 September 2014, 陕西科学技术出版社 * |
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 |
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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. |
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Application publication date: 20180206 |