CN110038322A - A kind of tripterygium glycosides chromatographic silica gel dress column method - Google Patents
A kind of tripterygium glycosides chromatographic silica gel dress column method Download PDFInfo
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- CN110038322A CN110038322A CN201910331603.2A CN201910331603A CN110038322A CN 110038322 A CN110038322 A CN 110038322A CN 201910331603 A CN201910331603 A CN 201910331603A CN 110038322 A CN110038322 A CN 110038322A
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- silica gel
- column
- chromatographic
- tripterygium
- column chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/14—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the introduction of the feed to the apparatus
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
- B01D15/20—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the sorbent material
- B01D15/206—Packing or coating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/42—Selective adsorption, e.g. chromatography characterised by the development mode, e.g. by displacement or by elution
- B01D15/424—Elution mode
Abstract
The invention discloses a kind of tripterygium glycosides chromatographic silica gels to fill column method, including S1: suitable column chromatography silica gel being filled in chromatographic column, silica gel face stabilization is evacuated to vacuum pump and does not sink；S2: chlorination is imitative to impregnate elution, is washed till mobile phase outflow uniformly, chromatographic column empty calory sheds；S3: being taken the extraction medicinal extract of column chromatography silica gel Yu appropriate tripterygium wilfordii, be stirred using trough type mixing machine, volatilize material, then crosses 80 meshes as loading spice silica gel；S4: spice silica gel obtained above being added in the silicagel column that chloroform is washed in step S2, and cylinder keeps smooth；The present invention will extract medicinal extract material and stir evenly with part silicone gel, volatilize filling on silica gel, it reuses eluting solvent and carries out elution separation, collect tripterygium glycosides effective component, reduce the material loss of mobile phase loading, the smooth stabilization of separation process central column face, reducing influences the risk of chromatography since chloroform silica gel Contact heat release blocks chromatographic column, improves product yield.
Description
Technical field
The present invention relates to pharmaceutical field, specially a kind of tripterygium glycosides chromatographic silica gel fills column method.
Background technique
Tripterygium glycosides (tripterygium glycosides) are formed from Celastraceae plant tripterygium root Hydrolysis kinetics
A kind of fat-soluble mixture, be China's research and utilization first anti inflammatory immunity adjust Chinese herbal medicine, have the title of " Chinese herbal medicine hormone ".
Its physiological activity is cooperateed with by Multiple components (diterpenoid-lactone, alkaloid, triterpene etc.) and is generated, and has both remained the immune of tripterygium wilfordii crude drug
The effects of inhibition, eliminates many toxic components again.Pharmacological research proves that tripterygium wilfordii has anti-inflammatory, immunosupress or immune tune
The effects of saving, is antitumor is the immunomodulator of domestic and international hot research at present.It can be used for treating rheumatoid arthritis, original
It is hair property glomerulus nephrosis, nephrotic syndrome, purple scar and lupus nephritis, lupus erythematosus, subacute and chronic hepatitis gravis, slow
Sexuality hepatitis；Also can be used for allergic skin vasculitis, dermatitis and eczema and psoriasis arthropathica, lepra reaction,
White Sai Shi disease, recurrent aphthous ulcer, ankylosing spondylitis etc..In recent years, go deep into clinical research, application range constantly expands
Greatly, such as treatment Purpura ephritis, chronic urticaria, Sjogren syndrome, Graves eye disease, renal albuminuria,
All achieve certain curative effect.
At present during tripterygium glycosides production of raw medicine, chromatography process will extract medicinal extract using silicagel column and carry out layer
Analysis separation, the filling mode of silicagel column generally use wet method dress post and dry column-packing two ways, and either way is all
Material is adsorbed on silica gel by mobile phase after dress column, the lossy of which mobile phase loading is big, and chloroform silica gel connects
Touching moment heat release easily blocks chromatographic column, influences chromatography efficiency.
Summary of the invention
The purpose of the present invention is to provide a kind of tripterygium glycosides chromatographic silica gels to fill column method, to solve above-mentioned background technique
The problem of middle proposition.
To achieve the above object, the invention provides the following technical scheme: a kind of tripterygium glycosides chromatographic silica gel fills column method,
It comprises the following specific steps that:
S1: suitable column chromatography silica gel is filled in chromatographic column, is evacuated to silica gel face stabilization with vacuum pump and is not sunk；
S2: chlorination is imitative to impregnate elution, is washed till mobile phase outflow uniformly, and chromatographic column empty calory sheds, and keeps liquid in silicagel column
Body stops that eluent is added；
S3: the column chromatography silica gel of 2/3 amount of the column chromatography silica gel loaded in step S1 and the extraction of appropriate tripterygium wilfordii are taken
Medicinal extract is taken, is stirred using trough type mixing machine, material is volatilized, then crosses 80 meshes as loading spice silica gel；
S4: spice silica gel obtained above being added in the silicagel column that chloroform is washed in step S2, and cylinder keeps smooth, thunder
The public more glycosides column chromatography silica gel dress columns of rattan are completed.
Preferably, the granularity of the column chromatography silica gel is 100-200 mesh.
Preferably, the model D400H2000 of the chromatographic column.
Preferably, the flow velocity that chloroform is added dropwise in step S2 is 80L/h.
Preferably, the model CH200 of trough type mixing machine.
Compared with prior art, the beneficial effects of the present invention are: the present invention will extract medicinal extract material and part silicone gel stirs
Uniformly, it volatilizes filling on silica gel, reuses eluting solvent and carry out elution separation, collect tripterygium glycosides effective component, reduce
The material loss of mobile phase loading, the smooth stabilization of separation process central column face reduce due to chloroform silica gel Contact heat release
Blocking chromatographic column and influence the risk of chromatography, improve product yield.
Detailed description of the invention
Fig. 1 is whole dress column flow diagram of the invention.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
In the description of the present invention, it should be noted that the orientation of the instructions such as term "vertical", "upper", "lower", "horizontal"
Or positional relationship is to be based on the orientation or positional relationship shown in the drawings, and is merely for convenience of description of the present invention and simplification of the description, and
It is not that the device of indication or suggestion meaning or element must have a particular orientation, be constructed and operated in a specific orientation, therefore
It is not considered as limiting the invention.
In the description of the present invention, it is also necessary to which explanation is unless specifically defined or limited otherwise, term " setting ",
" installation ", " connected ", " connection " shall be understood in a broad sense, for example, it may be fixedly connected, may be a detachable connection or one
Connect to body；It can be mechanical connection, be also possible to be electrically connected；It can be directly connected, it can also be indirect by intermediary
It is connected, can be the connection inside two elements.For the ordinary skill in the art, it can manage as the case may be
Solve the concrete meaning of above-mentioned term in the present invention.
Embodiment 1: referring to Fig. 1, the present invention provides a kind of technical solution: a kind of tripterygium glycosides chromatographic silica gel dress column side
Method comprises the following specific steps that:
S1: suitable column chromatography silica gel is filled in chromatographic column, is evacuated to silica gel face stabilization with vacuum pump and is not sunk；
S2: chlorination is imitative to impregnate elution, is washed till mobile phase outflow uniformly, and chromatographic column empty calory sheds, and keeps liquid in silicagel column
Body stops that eluent is added；
S3: the column chromatography silica gel of 2/3 amount of the column chromatography silica gel loaded in step S1 and the extraction of appropriate tripterygium wilfordii are taken
Medicinal extract is taken, is stirred using trough type mixing machine, material is volatilized, then crosses 80 meshes as loading spice silica gel；
S4: spice silica gel obtained above being added in the silicagel column that chloroform is washed in step S2, and cylinder keeps smooth, thunder
The public more glycosides column chromatography silica gel dress columns of rattan are completed.
Further, the granularity of the column chromatography silica gel is 100-200 mesh.
Further, the model D400H2000 of the chromatographic column.
Further, the flow velocity that chloroform is added dropwise in step S2 is 80L/h.
Further, the model CH200 of trough type mixing machine.
Embodiment 2: tripterygium glycosides chromatographic silica gel fills column step are as follows:
S1: the column chromatography silica gel of 65kg is filled in chromatographic column, is evacuated to silica gel face stabilization with vacuum pump and is not sunk；
S2: chlorination is imitative to impregnate elution, is washed till mobile phase outflow uniformly, and chromatographic column empty calory sheds, and keeps liquid in silicagel column
Body stops that eluent is added；
S3: the extraction medicinal extract 50kg of 40kg column chromatography silica gel Yu 1200kg tripterygium wilfordii is taken, is stirred using trough type mixing machine
Mixing is mixed, material is volatilized, then crosses 80 meshes as loading spice silica gel；
S4: spice silica gel obtained above being added in the silicagel column that chloroform is washed in step S2, and cylinder keeps smooth, thunder
The public more glycosides column chromatography silica gel dress columns of rattan are completed.
The present invention will extract medicinal extract material and stir evenly with part silicone gel, volatilize filling on silica gel, and it is molten to reuse elution
Agent carries out elution separation, collects tripterygium glycosides effective component, reduces the material loss of mobile phase loading, separation process center pillar
The smooth stabilization in face, reducing influences the risk of chromatography since chloroform silica gel Contact heat release blocks chromatographic column, improves
Product yield.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (5)
1. a kind of tripterygium glycosides chromatographic silica gel fills column method, which is characterized in that comprise the following specific steps that:
S1: suitable column chromatography silica gel is filled in chromatographic column, is evacuated to silica gel face stabilization with vacuum pump and is not sunk；
S2: chlorination is imitative to impregnate elution, is washed till mobile phase outflow uniformly, and chromatographic column empty calory sheds, and keeps liquid in silicagel column, stops
Eluent is only added；
S3: the extraction of the column chromatography silica gel and appropriate tripterygium wilfordii of 2/3 amount of the column chromatography silica gel loaded in step S1 is taken to soak
Cream is stirred using trough type mixing machine, volatilizes material, then crosses 80 meshes as loading spice silica gel；
S4: spice silica gel obtained above being added in the silicagel column that chloroform is washed in step S2, and cylinder keeps smooth, tripterygium wilfordii
More glycosides column chromatography silica gel dress columns are completed.
2. a kind of tripterygium glycosides chromatographic silica gel according to claim 1 fills column method, it is characterised in that: the column chromatography
The granularity of silica gel is 100-200 mesh.
3. a kind of tripterygium glycosides chromatographic silica gel according to claim 1 fills column method, it is characterised in that: the chromatographic column
Model D400H2000.
4. a kind of tripterygium glycosides chromatographic silica gel according to claim 1 fills column method, it is characterised in that: chlorine in step S2
The imitative flow velocity being added dropwise is 80L/h.
5. a kind of tripterygium glycosides chromatographic silica gel according to claim 1 fills column method, it is characterised in that: trough type mixing machine
Model CH200.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910331603.2A CN110038322A (en) | 2019-04-24 | 2019-04-24 | A kind of tripterygium glycosides chromatographic silica gel dress column method |
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| CN201910331603.2A CN110038322A (en) | 2019-04-24 | 2019-04-24 | A kind of tripterygium glycosides chromatographic silica gel dress column method |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482115A (en) * | 2002-09-13 | 2004-03-17 | 中国科学院武汉植物研究所 | Process for preparing oridonin |
| CN200951333Y (en) * | 2006-09-22 | 2007-09-26 | 上海复旦复华药业有限公司 | Chromatographic separation equipment |
| CN101747406A (en) * | 2010-01-06 | 2010-06-23 | 福建省汉堂生物制药股份有限公司 | Technology for producing triptodiolide with leaf of tripterygium |
| US20120004434A1 (en) * | 2010-06-03 | 2012-01-05 | University Of South Florida | Germania-silica-based sol-gel monolith and uses thereof |
| CN103242335A (en) * | 2013-04-28 | 2013-08-14 | 四川省裕通生物技术有限公司 | Method for extracting and purifying artemisinin |
| CN107793430A (en) * | 2017-12-25 | 2018-03-13 | 禹州市天源生物科技有限公司 | A kind of method of purification of qinghaosu |
-
2019
- 2019-04-24 CN CN201910331603.2A patent/CN110038322A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1482115A (en) * | 2002-09-13 | 2004-03-17 | 中国科学院武汉植物研究所 | Process for preparing oridonin |
| CN200951333Y (en) * | 2006-09-22 | 2007-09-26 | 上海复旦复华药业有限公司 | Chromatographic separation equipment |
| CN101747406A (en) * | 2010-01-06 | 2010-06-23 | 福建省汉堂生物制药股份有限公司 | Technology for producing triptodiolide with leaf of tripterygium |
| US20120004434A1 (en) * | 2010-06-03 | 2012-01-05 | University Of South Florida | Germania-silica-based sol-gel monolith and uses thereof |
| CN103242335A (en) * | 2013-04-28 | 2013-08-14 | 四川省裕通生物技术有限公司 | Method for extracting and purifying artemisinin |
| CN107793430A (en) * | 2017-12-25 | 2018-03-13 | 禹州市天源生物科技有限公司 | A kind of method of purification of qinghaosu |
Non-Patent Citations (1)
| Title |
|---|
| 熊万明等: "《有机化学实验》", 31 January 2017, 北京理工大学出版社 * |
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Application publication date: 20190723 |