CN205549683U - Novel chromatography column suitable for separation and purification of immunosuppressant ascomycin - Google Patents
Novel chromatography column suitable for separation and purification of immunosuppressant ascomycin Download PDFInfo
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- CN205549683U CN205549683U CN201620208089.5U CN201620208089U CN205549683U CN 205549683 U CN205549683 U CN 205549683U CN 201620208089 U CN201620208089 U CN 201620208089U CN 205549683 U CN205549683 U CN 205549683U
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- bucket
- outflow
- interior
- filter plate
- porous filter
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Abstract
The utility model relates to a novel chromatography column suitable for separation and purification of immunosuppressant ascomycin, the chromatography column is including outflow bucket, internal flow bucket, resin separation filler, interior bucket porous filtering plate, outer bucket porous filtering plate, water conservancy diversion weir, crude import and liquid outlet, the coaxial interval of outflow bucket suit is outside the internal flow bucket, the top of internal flow bucket sets up a blind flange, sets up the crude import on this blind flange, bucket porous filtering plate in the top suit of this internal flow bucket, the outer barrel porous filtering plate of coaxial arrangement in the outflow bucket of the top below of the bucket that should outflow, coaxial arrangement water conservancy diversion weir and liquid outlet in the outflow bucket, the bottom of internal flow bucket is opening status, the airtight setting in bottom of outflow bucket and setting up with the bottom looks interval of internal flow bucket, it packs all to load the resin separation in the outflow bucket of the inside and outside bucket porous filtering plate below of internal flow bucket of interior bucket porous filtering plate below. This chromatography column design science, simple structure, separation are effectual, the cost is reduced, improved work efficiency.
Description
Technical field
This utility model belongs to the separation equipment technical field of biochemical industry, especially one and is applicable to immunosuppressant jizi for making dumplings
The Novel chromatographic column that capsule mycin is isolated and purified.
Background technology
At present, the compositions of multiple compounds, natural product and Chinese medicine isolated and purified, mainly use column chromatography, make
With chromatographic column, realized by column chromatography procedure.
Ascosin (ascomycin, FK-520) is by streptomyces hygroscopicus ascus subspecies (Streptomyces
Hygroscopicus var.ascomyceticus) fermentation produce a kind of Macrolide being made up of two thirteen rings resist
Raw element, is jointly synthesized by polyketide synthase/non-ribosomal synzyme, has the sky of the strongest antifungal and immunosuppressive activity
So compound, has obtained using the most widely at present, but, owing in ascosin crude product, homologue is many, impurity composition
Many, separating difficulty is big, in industry uses high through repeatedly chromatographing than the chromatographic column for 10:1 more, removes removal of impurity complex process, cost
Height, brings inconvenience to use.
By retrieval, not yet find the patent publication us relevant to present patent application.
Summary of the invention
In place of the purpose of this utility model is to overcome the deficiencies in the prior art, it is provided that a kind of design science, simple in construction,
Good separating effect, reduce cost, improve work efficiency be applicable to isolated and purified novel of immunosuppressant ascosin
Chromatographic column.
This utility model solves it and technical problem is that and take techniques below scheme to realize:
A kind of being applicable to the Novel chromatographic column that immunosuppressant ascosin is isolated and purified, described chromatographic column includes outflow
Bucket, interior stream bucket, resin separating filler, interior bucket porous filter plate, outer barrel porous filter plate, weir, crude product import and liquid outlet, described
Outflow bucket coaxial spaced is set in outside interior stream bucket, and the tight of described interior stream bucket removably connects and arranges a blind flange, this method
Orchid covers and arranges crude product import with being connected inside interior stream bucket, in the top of the interior stream bucket below this crude product import in coaxial package
Bucket porous filter plate, the top of described outflow bucket is arranged at the lower section of interior bucket porous filter plate with the interior airtight setting of stream bucket and its top,
Outer barrel porous filter plate it is co-axially mounted, this outer barrel porous filter plate and the top of outflow bucket in outflow bucket below the top of this outflow bucket
Between outflow bucket in be co-axially mounted weir, the outflow bucket above this weir is connected is provided with out liquid with in outflow bucket
Mouthful；
The opening-like state in bottom of described interior stream bucket, the airtight setting in bottom of described outflow bucket and the bottom phase with interior stream bucket
Interval is arranged, and all loads resin in the outflow bucket below interior stream bucket inside and outside bucket porous filter plate below described interior bucket porous filter plate
Separating filler.
And, the bottom of described outflow bucket closely removably connects and arranges mounting flange bottom.
And, the diameter d2 of described outflow bucket is the √ 2 times of the diameter d1 of interior stream bucket, and a height of h of described interior stream bucket is described
A height of H of outflow bucket, described d2, d1, h and H meet following relation: h/d1=10, H/d2=8.This utility model obtains
Advantage and good effect be:
1, this chromatographic column design science, simple in construction, stream bucket and outflow bucket one step chromatography in using, the most removable ascus is mould
Related impurities in element, good separating effect, reduce cost, improve work efficiency.
2, the bottom of the outflow bucket of this chromatographic column closely removably connects and arranges mounting flange bottom, by bottom this
Mounting flange removably connects with the bottom of outflow bucket so that outflow bucket and the connection of bottom mounting flange and dismounting
The most more convenient, when needing to change the resin separating filler in outflow bucket and interior stream bucket so that change more convenient, the most also
It is beneficial to clean inside outflow bucket and interior stream bucket, brings conveniently to use.
3, √ 2 times, a height of h of described interior stream bucket of the diameter d1 that diameter d2 is interior stream bucket of the outflow bucket of this chromatographic column,
A height of H of described outflow bucket, described d2, d1, h and H meet following relation: h/d1=10, H/d2=8, this kind of this chromatographic column
The setting of structure so that the separating effect of this chromatographic column is preferable.
Accompanying drawing explanation
Fig. 1 is structure connection diagram of the present utility model.
Detailed description of the invention
Below by specific embodiment, the utility model is described in further detail, and following example are illustrative, no
It is determinate, it is impossible to limit protection domain of the present utility model with this.
Structure, annexation and the method not described in detail in this utility model, all can be understood as the public affairs in this area
Know general knowledge.
A kind of it is applicable to the Novel chromatographic column that immunosuppressant ascosin is isolated and purified, as it is shown in figure 1, described chromatographic column
Including outflow bucket 1, interior stream bucket 2, resin separating filler (not shown), interior bucket porous filter plate 5, outer barrel porous filter plate 6, water conservancy diversion
Weir 7, crude product import 4 and liquid outlet 8, described outflow bucket coaxial spaced is set in outside interior stream bucket, the tight of described interior stream bucket
Removably connect and a blind flange 3 is set, this blind flange arranges crude product import, under this crude product import with being connected inside interior stream bucket
Bucket porous filter plate in coaxial package in the top of the interior stream bucket of side, the top of described outflow bucket and the interior airtight setting of stream bucket and its top
Portion is arranged at the lower section of interior bucket porous filter plate, is co-axially mounted outer barrel porous filter plate in the outflow bucket below the top of this outflow bucket,
It is co-axially mounted weir, the outflow bucket above this weir in outflow bucket between the top of this outer barrel porous filter plate and outflow bucket
Above it is provided with liquid outlet with being connected in outflow bucket；
The opening-like state in bottom of described interior stream bucket, the airtight setting in bottom of described outflow bucket and the bottom phase with interior stream bucket
Interval is arranged, and all loads resin in the outflow bucket below interior stream bucket inside and outside bucket porous filter plate below described interior bucket porous filter plate
Separating filler.
This chromatographic column design science, simple in construction, stream bucket and outflow bucket one step chromatography, the most removable ascosin in using
In related impurities, good separating effect, reduce cost, improve work efficiency.
In the present embodiment, the bottom of described outflow bucket closely removably connects and arranges mounting flange 9 bottom, passes through
Bottom this, mounting flange removably connects with the bottom of outflow bucket so that outflow bucket and the connection of bottom mounting flange
And dismounting is the most more convenient, when needing to change the resin separating filler in outflow bucket and interior stream bucket so that change more convenient,
The most also it is beneficial to clean inside outflow bucket and interior stream bucket, brings conveniently to use.
Optimally, the diameter d2 of described outflow bucket is the √ 2 times of the diameter d1 of interior stream bucket, a height of h of described interior stream bucket, institute
Stating a height of H of outflow bucket, described d2, d1, h and H meet following relation: h/d1=10, H/d2=8, this kind of this chromatographic column is tied
The setting of structure so that the separating effect of this chromatographic column is preferable, owing to ascosin impurity content is high, homologue is many, is belonging to difficulty
One class antibiotic medicine of purification, a small amount of sample separates available preparative hplc preparative separation or more normal than the room temperature reaching 20 times with post footpath
Compression leg separates, and hectogram to be separated above ascosin crude product is necessary for using industrial large-sized preparative hplc, and cost is high, wants
Normal temperature and pressure chromatographic column separation hectogram above ascosin crude product bore to be used is used to reach the chromatographic column of 150mm, if to reach
Needing post footpath ratio to reach more than 20 to higher detached dowel effect, chromatographic column height to reach 3 meters high and just can efficiently separate, and commercial production is conventional
Chromatographic column is high through ratio usually 10 times, and ascosin crude product is only capable of isolating 2 impurity in this type of post, with ascosin product
Structure and similar demethyl ascosin thereof because of between differ only by a methyl group and be little to efficiently separate, need to be by once
Crude product after post separates processes loading chromatography again, and product is through repeatedly chromatographing, and condensing crystallizing loss is many, and energy consumption is big, unfavorable environmental protection,
In order to improve disadvantages mentioned above, this device designs stream bucket in increasing by a group in Conventional chromatography post, by the diameter d2 of outflow bucket is
The √ of the diameter d1 of interior stream bucket 2 times, a height of h of interior stream bucket, a height of H of outflow bucket, d2, d1, h and H meet following relation: h/
D1=10, H/d2=8, this device, on the premise of not increasing column length, improves chromatographic column post effect, and ascosin crude product is at interior bucket
Start chromatography after the once uniform loading of porous filter plate 5 upper end, by liquid outlet 8 fraction collection, qualified ascomycin solution is received
Collection, obtains ascosin sterling after subsequent treatment, technique is simple, ascosin good separating effect.
Utilize and be originally applicable to the isolated and purified Novel chromatographic column of immunosuppressant ascosin to carry out isolated and purified ascus mould
The result of element crude product is as shown in table 1, from table 1 it follows that relevant ascosin impurity Ex-all before 9.6min, substantially detects
Existing less than material, 9.660min impurity remaining is 0.32%, and 11.009min is demethyl ascosin impurity, and its impurity is residual
Depositing area is 0.11%, and 15.451min is demethyl ascosin isomers impurity, and its impurity remaining area is
0.33%, 22.981min and 25.381min impurity remaining are respectively 0.15 and 0.07%, also comply with product quality requirement,
19.158min is ascosin monomer, and its purity has reached 99.02%, and separating effect is obvious.
Table 1 utilizes a kind of result figure SAMPLE INFORMATION after this utility model purification ascosin crude product
Auto-Scaled Chromatogram
Peak Results
。
Claims (3)
1. one kind is applicable to the Novel chromatographic column that immunosuppressant ascosin is isolated and purified, it is characterised in that: described chromatographic column
Including outflow bucket, interior stream bucket, resin separating filler, interior bucket porous filter plate, outer barrel porous filter plate, weir, crude product import and go out
Liquid mouth, described outflow bucket coaxial spaced is set in outside interior stream bucket, and the tight of described interior stream bucket removably connects and arranges a method
Blue lid, this blind flange arranges crude product import with being connected inside interior stream bucket, in the top of the interior stream bucket below this crude product import
Bucket porous filter plate in coaxial package, the top of described outflow bucket and the interior airtight setting of stream bucket and its top are arranged at the filter of interior bucket porous
The lower section of plate, is co-axially mounted outer barrel porous filter plate in the outflow bucket below the top of this outflow bucket, this outer barrel porous filter plate is with outer
It is co-axially mounted weir in outflow bucket between the top of stream bucket, the outflow bucket above this weir is connected with in outflow bucket
It is provided with liquid outlet；
The opening-like state in bottom of described interior stream bucket, the airtight setting in bottom of described outflow bucket and with the bottom of interior stream bucket separately
Arrange, all load resin in the outflow bucket below interior stream bucket inside and outside bucket porous filter plate below described interior bucket porous filter plate and separate
Filler.
The most according to claim 1 it is applicable to the Novel chromatographic column that immunosuppressant ascosin is isolated and purified, its feature
It is: the bottom of described outflow bucket closely removably connects and arranges mounting flange bottom.
The most according to claim 1 and 2 being applicable to the Novel chromatographic column that immunosuppressant ascosin is isolated and purified, it is special
Levy and be: the diameter d2 of described outflow bucket is the √ 2 times of the diameter d1 of interior stream bucket, a height of h of described interior stream bucket, described outflow bucket
A height of H, described d2, d1, h and H meet following relation: h/d1=10, H/d2=8.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620208089.5U CN205549683U (en) | 2016-03-18 | 2016-03-18 | Novel chromatography column suitable for separation and purification of immunosuppressant ascomycin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201620208089.5U CN205549683U (en) | 2016-03-18 | 2016-03-18 | Novel chromatography column suitable for separation and purification of immunosuppressant ascomycin |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN205549683U true CN205549683U (en) | 2016-09-07 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201620208089.5U Expired - Fee Related CN205549683U (en) | 2016-03-18 | 2016-03-18 | Novel chromatography column suitable for separation and purification of immunosuppressant ascomycin |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN205549683U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749329A (en) * | 2016-11-28 | 2017-05-31 | 无锡福祈制药有限公司 | A kind of method that ascosin is isolated and purified in the liquid from streptomycete fermentation |
-
2016
- 2016-03-18 CN CN201620208089.5U patent/CN205549683U/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749329A (en) * | 2016-11-28 | 2017-05-31 | 无锡福祈制药有限公司 | A kind of method that ascosin is isolated and purified in the liquid from streptomycete fermentation |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20160907 Termination date: 20190318 |