CN105859699A - Preparation method of silymarin - Google Patents
Preparation method of silymarin Download PDFInfo
- Publication number
- CN105859699A CN105859699A CN201610218798.6A CN201610218798A CN105859699A CN 105859699 A CN105859699 A CN 105859699A CN 201610218798 A CN201610218798 A CN 201610218798A CN 105859699 A CN105859699 A CN 105859699A
- Authority
- CN
- China
- Prior art keywords
- silymarin
- ethanol
- described step
- entering
- preparation
- 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)
Abstract
The invention discloses a preparation method of silymarin. The method comprises the following steps: a) squeezing and oil removal; b) extraction: performing pretreatment of grinding, filtering and impurity removal of a silybum marianum slag cake obtained in the step a), putting the pretreated silybum marianum slag cake into an extraction tank, adding an ethanol extraction solution and performing repeated extraction to obtain a mixed solution of ethanol and silymarin; c) concentration; d) separation of residual ethanol: adding the rough silymarin obtained in the step c) into pure water and heating so that residual ethanol in the rough silymarin is dissolved in the pure water; and e) secondary concentration. In the invention, by adopting ultrasonic-assisted extraction in the silymarin extraction process, the extraction efficiency of silymarin is increased; and by adding the step of residual ethanol separation, the organic solvent residue in the silymarin is effectively reduced.
Description
[technical field]
The technical field of silymarin of the present invention, the technical field of the preparation method of a kind of silymarin.
[background technology]
Silymarin is antioxidant, refines from a kind of entitled Silybum marianum Gaertn plant and forms.Silymarin can stablize liver
Cell membrane, maintains the integrity of hepatocyte, makes toxin cannot penetrate destruction liver, and can accelerate to synthesize liver
The DNA (deoxyribonucleic) of cell, can prevent the diseases such as liver cirrhosis, fatty liver, cholangitis, psoriasis,
There is growth and the differentiation inhibitory action of hepatocarcinoma, carcinoma of prostate, breast carcinoma and cervical cancer cell simultaneously.It it is mesh
Found on former world that the flavonoid of most liver disease curative effect, the preparation of existing silymarin usually use organic
Solvent carries out extracting, and owing to existing silymarin is in preparation process, simply have employed simple true
Sky is dried the organic solvent removing in silymarin, there is organic solvent in therefore obtained silymarin,
These organic solvents are the most harmful, and these organic solvents also affect the drug effect of silymarin.
[summary of the invention]
The purpose of the present invention solves the problems of the prior art exactly, proposes the preparation method of a kind of silymarin,
The present invention is by using ultrasonic assistant to extract during extracting at silymarin, thus adds silymarin
Extraction efficiency, the present invention, also by increasing the step that residual ethanol separates, thus is effectively reduced water and flies
Determination of Residual Organic Solvents in silibin.
For achieving the above object, the present invention proposes the preparation method of a kind of silymarin, it is characterised in that
Comprise the steps:
A) squeezing oil removing: by the fruit of Herba Silybi mariani, carries out squeezing oil removing, thus obtains Silybum Marianum Gaertn Seed Oil and water flies
A Ji blob of slag；
B) extract: first carry out the Herba Silybi mariani blob of slag that step a) obtains pulverizing the early stage process filtering roguing,
Then the Herba Silybi mariani blob of slag after early stage being processed is put in extraction pot, subsequently adds ethanol extraction solution and carries out
Repeatedly extract, thus obtain the mixed solution of ethanol and silymarin；
C) concentrate: the ethanol that step b) is obtained and the mixed solution of silymarin, carry out vacuum drying and concentrate,
Thus obtain rough silymarin；
D) residual ethanol separates: the rough silymarin obtained by step c) rejoins in pure water, then
Heat temperature raising, so that the ethanol of residual dissolves in pure water in rough silymarin；
E) secondary concentration；The silymarin being settled out in step d) pure water is carried out secondary vacuum and is dried concentration,
Thus obtain silymarin finished product.
As preferably, described step b), when entering shape and extracting, uses the mode being heated to reflux and extracts
, described step b) additionally uses ultrasonic assistant and extracts when entering and extracting.
As preferably, the described step b) heating-up temperature when entering shape and extracting every time is 60 DEG C-80 DEG C, described
Step b) enters the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ when extracting entering shape every time.
As preferably, the described step b) constant temperature time when entering shape and extracting every time is 1h-1.5h, described step
Rapid b) when entering shape and extracting every time, add 6-7 times that weight is Herba Silybi mariani blob of slag weight of ethanol.
As preferably, the described step d) heating-up temperature when carrying out residual ethanol and separating is 50 DEG C-60 DEG C,
It is auxiliary that constant temperature persistent period 0.5h-1h, described step d) also use ultrasound wave when carrying out residual ethanol and separating
Hydrotropy solution.
As preferably, the auxiliary ultrasonic that described step d) is used when carrying out residual ethanol and separating is
The ultrasound wave of 35KHZ-40KHZ, described step d to step e can be with repetitive operation, until making silymarin
In ethanol be totally separated.
[detailed description of the invention]
The preparation method of a kind of silymarin of the present invention, it is characterised in that comprise the steps: a) squeeze oil removing:
By the fruit of Herba Silybi mariani, carry out squeezing oil removing, thus obtain Silybum Marianum Gaertn Seed Oil and a Herba Silybi mariani blob of slag；B) extract: first
First carry out the Herba Silybi mariani blob of slag that step a) obtains pulverizing the early stage process filtering roguing, then early stage is processed
After a Herba Silybi mariani blob of slag put in extraction pot, subsequently add ethanol extraction solution repeatedly extract, thus
Obtain the mixed solution of ethanol and silymarin；C) concentrate: ethanol that step b) is obtained and silymarin
Mixed solution, carries out vacuum drying and concentrates, thus obtain rough silymarin；D) residual ethanol separates: will step
Rapid rough silymarin c) obtained rejoins in pure water, and then heat temperature raising, so that rough water flies
In silibin, the ethanol of residual dissolves in pure water；E) secondary concentration；To the water being settled out in step d) pure water
Flying silibin to carry out secondary vacuum and be dried concentration, thus obtain silymarin finished product, described step b) carries entering shape
When taking, using what the mode being heated to reflux carried out extracting, described step b) additionally uses when entering and extracting
Ultrasonic assistant extracts, and the described step b) heating-up temperature when entering shape and extracting every time is 60 DEG C-80 DEG C, institute
State step b) and enter the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ when extracting entering shape every time, described
The step b) the constant temperature time when entering shape and extracting every time is 1h-1.5h, and described step b) extracts entering shape every time
Time, adding 6-7 times that weight is Herba Silybi mariani blob of slag weight of ethanol, described step d) is carrying out residual ethanol
Heating-up temperature during separation is 50 DEG C-60 DEG C, constant temperature persistent period 0.5h-1h, and described step d) is being carried out
Residual ethanol also uses ultrasonic assistant and dissolves when separating, described step d) is when carrying out residual ethanol and separating
The auxiliary ultrasonic used is the ultrasound wave of 35KHZ-40KHZ, and described step d to step e can repeat
Operation, until making the ethanol in silymarin be totally separated.
The present invention is by using ultrasonic assistant to extract during extracting at silymarin, thus adds water and fly
The extraction efficiency of silibin, the present invention is also by increasing the step that residual ethanol separates, thus is effectively reduced
Determination of Residual Organic Solvents in silymarin.
Above-described embodiment is the description of the invention, is not limitation of the invention, any simple to the present invention
Scheme after conversion belongs to protection scope of the present invention.
Claims (6)
1. the preparation method of a silymarin, it is characterised in that comprise the steps:
A) squeezing oil removing: by the fruit of Herba Silybi mariani, carries out squeezing oil removing, thus obtains Silybum Marianum Gaertn Seed Oil and Herba Silybi mariani
A blob of slag；
B) extract: first carry out the Herba Silybi mariani blob of slag that step a) obtains pulverizing the early stage process filtering roguing,
Then the Herba Silybi mariani blob of slag after early stage being processed is put in extraction pot, subsequently adds ethanol extraction solution and carries out
Repeatedly extract, thus obtain the mixed solution of ethanol and silymarin；
C) concentrate: the ethanol that step b) is obtained and the mixed solution of silymarin, carry out vacuum drying and concentrate,
Thus obtain rough silymarin；
D) residual ethanol separates: the rough silymarin obtained by step c) rejoins in pure water, then
Heat temperature raising, so that the ethanol of residual dissolves in pure water in rough silymarin；
E) secondary concentration；The silymarin being settled out in step d) pure water is carried out secondary vacuum and is dried concentration,
Thus obtain silymarin finished product.
The preparation method of a kind of silymarin the most as claimed in claim 1, it is characterised in that: described step b) is entering
When shape is extracted, using what the mode being heated to reflux carried out extracting, described step b) also adopts when entering and extracting
With ultrasonic assistant extraction.
The preparation method of a kind of silymarin the most as claimed in claim 1, it is characterised in that: described step b) is entering
Heating-up temperature when shape is extracted every time is 60 DEG C-80 DEG C, and described step b) is auxiliary enter that shape enters when extracting every time
The ultrasound wave helping ultrasound wave to be 35KHZ-40KHZ.
The preparation method of a kind of silymarin the most as claimed in claim 1, it is characterised in that: described step b) is entering
Constant temperature time when shape is extracted every time is 1h-1.5h, and described step b), when entering shape and extracting every time, adds second
The weight of alcohol is 6-7 times of Herba Silybi mariani blob of slag weight.
The preparation method of a kind of silymarin the most as claimed in claim 1, it is characterised in that: described step d) is entering
The heating-up temperature that row residual ethanol separates is 50 DEG C-60 DEG C, constant temperature persistent period 0.5h-1h, described step d)
Also use ultrasonic assistant when carrying out residual ethanol and separating to dissolve.
The preparation method of a kind of silymarin the most as claimed in claim 1, it is characterised in that: described step d) is entering
Row residual ethanol separates the ultrasound wave that auxiliary ultrasonic is 35KHZ-40KHZ used, described step d
Can be with repetitive operation to step e, until making the ethanol in silymarin be totally separated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610218798.6A CN105859699A (en) | 2016-04-08 | 2016-04-08 | Preparation method of silymarin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610218798.6A CN105859699A (en) | 2016-04-08 | 2016-04-08 | Preparation method of silymarin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105859699A true CN105859699A (en) | 2016-08-17 |
Family
ID=56637251
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610218798.6A Pending CN105859699A (en) | 2016-04-08 | 2016-04-08 | Preparation method of silymarin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105859699A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285443A (en) * | 2017-01-09 | 2018-07-17 | 天津天士力圣特制药有限公司 | A kind of process for purification of silibinin |
| CN109362966A (en) * | 2018-11-05 | 2019-02-22 | 华中农业大学 | A kind of plant extract feed additive and application for improving sow milk performance |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Extraction process of silymarin using ethanol as a single organic solvent |
| 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 |
| CN103509647A (en) * | 2013-09-27 | 2014-01-15 | 宁波市北仑玉健医药科技有限公司 | Method for preparing silybum marianum oil rich in silymarin |
| CN104673486A (en) * | 2015-02-13 | 2015-06-03 | 安徽嘉旗粮油工程技术有限公司 | Method for simultaneously extracting silybum marianum oil and silymarin from silybum marianum cake |
-
2016
- 2016-04-08 CN CN201610218798.6A patent/CN105859699A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Extraction process of silymarin using ethanol as a single organic solvent |
| 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 |
| CN103509647A (en) * | 2013-09-27 | 2014-01-15 | 宁波市北仑玉健医药科技有限公司 | Method for preparing silybum marianum oil rich in silymarin |
| CN104673486A (en) * | 2015-02-13 | 2015-06-03 | 安徽嘉旗粮油工程技术有限公司 | Method for simultaneously extracting silybum marianum oil and silymarin from silybum marianum cake |
Non-Patent Citations (3)
| Title |
|---|
| 任冰如等: "水飞蓟素提取和水飞蓟宾纯化的研究", 《时珍国医国药》 * |
| 张淑丽等: "水飞蓟有效成分及其提取方法研究进展", 《人参研究》 * |
| 董岩等: "水飞蓟有效成分的提取研究", 《中成药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285443A (en) * | 2017-01-09 | 2018-07-17 | 天津天士力圣特制药有限公司 | A kind of process for purification of silibinin |
| CN108285443B (en) * | 2017-01-09 | 2023-05-23 | 江苏天士力帝益药业有限公司 | Refining method of silybin |
| CN109362966A (en) * | 2018-11-05 | 2019-02-22 | 华中农业大学 | A kind of plant extract feed additive and application for improving sow milk performance |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104946383B (en) | A kind of supercritical CO2The method that composite microwave auxiliary extraction prepares ganoderma lucidum spore oil | |
| CN102558264A (en) | Method for extracting cordycepin and cordyceps polysaccharide from cordyceps militaris | |
| CN106046194A (en) | Extraction method of dendrobium huoshanense polysaccharide | |
| CN106187977A (en) | A kind of method extracting Garcinia mangostana shell procyanidins | |
| CN105859601A (en) | Method for extracting astaxanthin from haematococcus pluvialis | |
| CN102388987B (en) | Ultrasound-assisted tea oil extraction method | |
| CN101993775B (en) | Method for preparing oil by whole peanut kernels | |
| CN103613624B (en) | The process for purification of a kind of Avrmectin | |
| CN105884754A (en) | Fine extraction method of silibinin | |
| CN105461778A (en) | Method for extracting tea saponin from sasangua cake | |
| CN105859699A (en) | Preparation method of silymarin | |
| CN101851268A (en) | Process for directly preparing soybean concentrated protein by wet soybean meal | |
| CN103349850B (en) | A kind of method for extracting active ingredient in wax-apple | |
| CN104906259A (en) | Preparation method of wolfberry extract | |
| CN102180921A (en) | Method for extracting high-purity rutin from boxthorn leaves | |
| CN113413403A (en) | Supercritical fluid extraction method for extracting active ingredients of silybum marianum | |
| CN104027373A (en) | Method for extracting ligusticum wallichii effective substance by use of combined microwave and subcritical extraction | |
| CN107082791A (en) | A kind of method that phenylethanoid glycosides are extracted from saline cistanche | |
| CN106187978A (en) | A kind of method extracting pitaya peel procyanidins | |
| CN105395592A (en) | Method for preparing maea extract through ultrasonic wave countercurrent | |
| CN111205300A (en) | A kind of method for efficiently extracting sesamin in sesame meal | |
| CN106187976A (en) | A kind of method extracting Rhizoma Steudnerae Henryanae procyanidins | |
| CN104857108A (en) | Method for preparing hawthorn extractive through continuous countercurrent ultrasonic equipment | |
| CN105524036A (en) | High-efficiency low-consumption grape seed procyanidine extraction method | |
| CN104672195A (en) | Method of preparing theaflavins by virtue of centrifugal extraction and separation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20160817 |
|
| RJ01 | Rejection of invention patent application after publication |