CN106267891A - The rapid separation and purification method of compound - Google Patents
The rapid separation and purification method of compound Download PDFInfo
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- CN106267891A CN106267891A CN201510298605.8A CN201510298605A CN106267891A CN 106267891 A CN106267891 A CN 106267891A CN 201510298605 A CN201510298605 A CN 201510298605A CN 106267891 A CN106267891 A CN 106267891A
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Abstract
The present invention proposes the rapid separation and purification method of a kind of compound, utilizes fast separating and purifying device to carry out the fast separating and purifying of described compound, and the method includes: dress sample: by sample uniform adsorption to be separated on described sample-adding slot packing；Dress post: fill filler to described second housing；Balance: send solvent by solvent unit to chromatography unit and be balanced；Sample-adding: the described loading slot being adsorbed with sample to be separated is loaded in chromatography unit；Eluting: utilize described solvent unit that described sample to be separated is carried out eluting, in order to isolated purpose compound；Detection: take described isolated purpose compound, is analyzed detection.Thus, it is possible to realize quickly efficiently separating of sample to be separated.
Description
Technical field
The invention belongs to pharmacy or chemical industry synthesis field, concrete, relate to the rapid separation and purification method of a kind of compound.
Background technology
Column chromatography belongs to the common isolated and purified means in pharmacy or chemical industry synthesis field, the most commonly utilizes dissimilar
Fine filler compound is separated.But when sample to be separated is more, filler is meticulous was easily caused post relatively slowly,
Cross long stop and both easily caused loss, affect again efficiency.
Therefore, isolation and purification method is still further improved.
Summary of the invention
It is contemplated that solve present in prior art one of technical problem the most to a certain extent or provide at one and have
Business select.To this end, it is an object of the present invention to provide the rapid separation and purification method of a kind of compound, utilize
The method, it is possible to achieve quickly efficiently separating of sample to be separated.
To this end, in the one side of invention, it is proposed that the rapid separation and purification method of a kind of compound.A reality according to invention
Execute example, utilize fast separating and purifying device to carry out the fast separating and purifying of described compound, wherein, described fast separating and purifying
Device includes: solvent unit, and described solvent unit includes: the first housing, and described first housing limits solvent and accommodates space；
Liquid outlet, described liquid outlet is positioned at the lower end of described first housing, chromatography unit, described chromatography unit and described solvent unit
Being connected, described chromatography unit includes: the second housing, and described second housing limits filler and accommodates space；Import: described in enter
Mouth is connected with described liquid outlet, is positioned at the upper end of described second housing；Outlet, described outlet is positioned under described second housing
End, loading slot, described loading slot is positioned at described filler and accommodates top of space；And reception unit, described reception unit and institute
Stating chromatography unit to be connected, the method for the fast separating and purifying of described compound includes: (1) dress sample: by uniform for sample to be separated
It is adsorbed on described sample-adding slot packing；(2) dress post: fill filler to described second housing；(3) balance: pass through solvent
Unit is sent solvent to described chromatography unit and is balanced；(4) sample-adding: the described loading slot being adsorbed with sample to be separated is filled
Enter in chromatography unit；(4) eluting: utilize described solvent unit that described sample to be separated is carried out eluting, in order to isolated
Purpose compound；(5) detection: take described isolated purpose compound, is analyzed detection.
Thus, utilize loading slot, in advance by sample uniform adsorption to be separated in filler, meanwhile, utilize the present invention's
Method, can synchronize to carry out filler dress post and equilibrium process, thus, it is to avoid conventional need first to load material and balance after,
Can carry out filling the operation of sample, the most time-consuming, improve efficiency.
According to embodiments of the invention, in step (1) sample to be separated sample-loading amount is packing volume in described loading slot 2～
3 times.Thus, it is to avoid when sample-loading amount is very few, the filled absorption of sample is too much, causes damage；Also sample-loading amount can be avoided too much
Time, sample transships, and fails the sample of filled absorption and can flow directly out with eluent, affects separating effect, and cause damage.
According to embodiments of the invention, described loading slot is removable loading slot.Thus, it is simple to by single for loading slot removal chromatography
Unit, makes dress sample step and dress post step synchronize to carry out, and, loading slot can also be according to how many adjustment positions of filler.
According to embodiments of the invention, the upper and lower surface of described loading slot is respectively provided with well.Thus, can will treat point
After filler, loading slot is loaded in the second housing of chromatography unit, the upper surface of loading slot from sample adsorption in loading slot
It is easy to the eluent eluting to sample with the well of lower surface, eluent local can be avoided simultaneously to have rushed filler, affect eluting
Effect.
According to embodiments of the invention, the aperture of described well is the 1/3～2/3 of described packing material size.Thus, filler exists
It is difficult in loading slot overflow, and does not block well, it is simple to eluent flows out.
According to embodiments of the invention, fast separating and purifying device farther includes: vacuum unit, wherein, described in take out true
Dummy cell includes: evacuation drainage hopper, and described evacuation drainage hopper is connected with described outlet and described reception unit, bag
Include: bleeding point；And evacuation part, described evacuation part is connected with described bleeding point.Thus, available vacuum unit,
Realize the fast separating and purifying of compound.
According to embodiments of the invention, described evacuation drainage hopper is detachable evacuation drainage hopper.Thus, it is simple to wash
Pour out filler after having taken off, or change filler.
According to embodiments of the invention, described chromatography unit farther includes: sieve plate, and described sieve plate is positioned at described filler and accommodates
In space, and it is positioned at below described filler, is used for intercepting filler and flows out from described outlet, including: at least one through hole.
Thus, it is simple to dress post.
According to a particular embodiment of the invention, the upper surface of described sieve plate has filter membrane.Thus, it is to avoid the eluent of outflow will
The imperceptible filler of particle diameter is real to be taken out of, causes filler loss and affects sample detection.
According to embodiments of the invention, the aperture in the hole on described sieve plate is the 1/3～2/3 of chromatographic apparatus packing material size.Thus,
Aperture is the least is unfavorable for that a large amount of effluent passes through, and aperture is too big, the easy plugging hole of filler.
According to embodiments of the invention, described solvent unit farther includes flow speed controller, for controlling the stream of described solvent
Go out speed.
According to a particular embodiment of the invention, described flow speed controller is valve, and described flow speed controller has flow and shows
Show device.Thus, adjust, control the flow velocity of the eluant held in solvent unit, and carry out eluant flow velocity as required
Regulation, it is simple in separation purifying technique, flow velocity is carried out parameter preferably, accumulation data, to realize optimal separation purification.
According to embodiments of the invention, the outer wall of described hollow cylinder has longitudinal dial chart layer.Thus, it is simple to observe and fill out
Material height and eluting agent change, it is achieved the quantitative parameter screening of separation purifying technique.
According to embodiments of the invention, described second housing is cylinder.
According to embodiments of the invention, described second housing uses quartz glass or high boron glass to make.
According to embodiments of the invention, described import is ground.Thus, going out by sealing-plug with holes and described solvent unit
Liquid mouth matches.
According to embodiments of the invention, described first housing is spheroid.
According to embodiments of the invention, the volume of described solvent unit can be adjusted according to experiment needs.Further,
Can be selected for the 500～2000ml of routine during pilot plant test, meet the demand of different amounts of sample to be separated.
According to embodiments of the invention, described first flow speed controller uses politef material to be formed.
The isolated and purified device of the present invention is applicable to dry column-packing or wet method dress post.
The isolated and purified device of the present invention can be used for isolated and purified medicine, chemical products and intermediate thereof, in described chromatography unit
The filler filled can be aluminium oxide, silica gel, polyamide, gel, magnesium oxide, activated carbon, macroporous resin, ion exchange
At least one in resin, cellulose, quartz sand.Experimenter can select to close according to the properties of samples of purification to be separated
Suitable filler.
The additional aspect of the present invention and advantage will part be given in the following description, and part will become bright from the following description
Aobvious, or recognized by the practice of the present invention.
Accompanying drawing explanation
Fig. 1 is the structural representation of fast separating and purifying device according to an embodiment of the invention.
Detailed description of the invention
Embodiments of the invention are described below in detail, and the example of described embodiment is shown in the drawings, the most identical
Or similar label represents same or similar element or has the element of same or like function.Retouch below with reference to accompanying drawing
The embodiment stated is exemplary, it is intended to is used for explaining the present invention, and is not considered as limiting the invention.
According to an aspect of the present invention, the present invention proposes a kind of rapid separation and purification method, utilizes fast separating and purifying to fill
Put the fast separating and purifying carrying out this compound.Below with reference to Fig. 1, the method for the fast separating and purifying of the present invention is carried out
Describe in detail:
According to some embodiments of the present invention, this fast separating and purifying device includes: solvent unit 100, chromatography unit 200,
Loading slot 300 and reception unit 400.Wherein, solvent unit 100 also includes: the first housing 120 and liquid outlet 110, its
In, the first housing limits solvent and accommodates space；Liquid outlet 110 is positioned at the lower end of the first housing 120, chromatography unit 200
Being connected with solvent unit 100, chromatography unit 200 also includes: the second housing 210, import 220 and outlet 230, wherein,
Second housing 210 limits filler and accommodates space；Import 220 is connected with liquid outlet 110, is positioned at the upper of the second housing 210
End；Outlet 230 is positioned at the lower end of the second housing 210.Loading slot 300 is positioned at described filler and accommodates top of space.Described connect
Receiving unit 400 to be connected with described chromatography unit 300, the method for the fast separating and purifying of described compound includes: (1) dress sample:
By sample uniform adsorption to be separated in described loading slot 300 on filler；(2) dress post: fill to described second housing 210
Filler；(3) balance: send solvent by solvent unit 100 to chromatography unit 200 and be balanced；(4) sample-adding: will inhale
Load in chromatography unit 200 with the described loading slot 300 of sample to be separated；(4) eluting: utilize described solvent unit 100
Described sample to be separated is carried out eluting, in order to isolated purpose compound；(5) detection: take described isolated purpose
Compound, is analyzed detection.
Thus, utilize loading slot 300, in advance by sample uniform adsorption to be separated in filler, meanwhile, can synchronize to carry out
Filler dress post and balance, thus, it is to avoid conventional need first to load material and balance after, just can carry out filling the operation of sample, significantly
Time-consuming, improve efficiency.
Loading slot 300 is removable loading slot according to a particular embodiment of the invention, i.e. loading slot 300 can be removed chromatography
Unit 200, loading slot 300 can also vertically move in the second housing 210.Thus, it is simple to dress sample step and dress post step
Rapid synchronization is carried out.Meanwhile, loading slot 300 can carry out accommodation according to the height of filler filling in chromatography unit 200,
It is particularly well-suited to the chromatography unit that the second housing 210 bore is bigger.
According to embodiments of the invention, the upper and lower surface of described loading slot 300 is respectively provided with well 310.Thus,
The of chromatography unit 200 can be loaded by overall for loading slot 300 by sample adsorption to be separated in loading slot 300 after filler
In two housings 210.The well 310 of the upper and lower surface of loading slot 300 can be easy to the eluent eluting to sample,
Eluent local can be avoided simultaneously to have rushed filler, affect eluting effect.
According to embodiments of the invention, the aperture of well 310 is the 1/3～2/3 of packing material size.Thus, when well 310
Aperture more than packing material size 2/3 time, filler easily under eluant pressure overflow loading slot；Aperture when well 310
Less than packing material size 1/3 time, well is easily blocked by filler, is unfavorable for that eluent flows out.Aperture is described packing material size
1/3～2/3 time filler be difficult to overflow in loading slot 300, and do not block well, it is simple to eluent flows out.
According to embodiments of the invention, fast separating and purifying device farther includes: vacuum unit 500, this evacuation list
Unit 500 includes: evacuation drainage hopper 510 and evacuation part 520, and wherein, evacuation drainage hopper 510 is single with chromatography
The outlet of unit 200 is connected with receiving unit 400, including: bleeding point 511；Evacuation part 520 is connected with bleeding point 511.
Thus, available vacuum unit 500, it is achieved the fast separating and purifying of compound.
According to embodiments of the invention, evacuation drainage hopper 510 is detachable evacuation drainage hopper.Thus, it is simple to wash
Pour out filler after having taken off, or change filler.
According to some embodiments of the present invention, chromatography unit 200 farther includes: sieve plate 240, and this sieve plate 240 is positioned to be filled out
Material accommodates in space, and is positioned at below filler, is used for intercepting filler and flows out from outlet, including: at least one through hole.By
This, it is simple to dress post, and be easy to the sample effluent from chromatography unit 200 eluting is complete and flow out through sieve plate 240.
According to a particular embodiment of the invention, sieve plate 240 upper surface has filter membrane.Thus, it is to avoid the eluent of outflow is by grain
The imperceptible filler in footpath is real to be taken out of, causes filler loss and affects sample detection.
According to embodiments of the invention, on sieve plate 240, the aperture of through hole is not particularly limited, can be according to different fillers
Matter selects different pore size, as long as can guarantee that separating effect.
According to embodiments of the invention, on sieve plate 240, the aperture of through hole is chromatography unit 200 the 1/3～2/3 of packing material size.
When the aperture of through hole is more than the 2/3 of packing material size, filler easily overflows sieve plate 240 under eluant pressure；Aperture when through hole
Less than packing material size 1/3 time, sieve plate is easily blocked by filler, is unfavorable for that effluent flows out.Aperture is described packing material size
When 1/3～2/3, filler is difficult to overflow on sieve plate 240, and non clogging screen plate, it is simple to effluent flows out.
According to embodiments of the invention, described solvent unit 100 farther includes: for controlling the stream of the rate of outflow of solvent
Speed controller 130.Thus, it is simple to control the speed that solvent flows out.
According to a particular embodiment of the invention, flow speed controller 130 is valve, and has flow indicator 131.Thus,
Adjust, control the flow velocity of the eluant held in solvent unit 100, and carry out eluant flow rate regulation as required, just
In carrying out flow velocity in separation purifying technique, parameter is preferred, accumulate data, to realize optimal separation purification.
According to embodiments of the invention, the outer wall of the second housing 210 has longitudinal dial chart layer.Thus, it is simple to observe and fill out
Material height and eluting agent change, it is achieved the quantitative parameter screening of separation purifying technique.
According to embodiments of the invention, the second housing 210 is cylinder.
According to some embodiments of the present invention, the second housing 210 can use quartz glass or high boron glass to make.
According to a particular embodiment of the invention, described import is ground, by sealing-plug with holes and described solvent unit 100
Liquid outlet matches.
According to embodiments of the invention, the first housing 120 is spherical.
According to embodiments of the invention, the volume of the first housing 120 can be adjusted according to experiment needs.Further,
Can be selected for the 500～2000ml of routine during pilot plant test, meet the demand of different amounts of sample to be separated.
According to embodiments of the invention, flow speed controller 130 can use politef material to make.
In describing the invention, it is to be understood that term " first ", " second " are only used for describing purpose, and are not understood that
For indicating or imply relative importance or the implicit quantity indicating indicated technical characteristic.Thus, define " first ", "
Two " feature can express or implicitly include one or more this feature.In describing the invention, " multiple "
It is meant that two or more, unless otherwise expressly limited specifically.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " concrete example ",
Or specific features, structure, material or the feature bag that the description of " some examples " etc. means to combine this embodiment or example describes
It is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term necessarily
It is directed to identical embodiment or example.And, the specific features of description, structure, material or feature can be arbitrary
Individual or multiple embodiment or example combine in an appropriate manner.Additionally, in the case of the most conflicting, the skill of this area
The feature of the different embodiments described in this specification or example and different embodiment or example can be combined by art personnel
And combination.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is exemplary,
Being not considered as limiting the invention, those of ordinary skill in the art within the scope of the invention can be to above-described embodiment
It is changed, revises, replaces and modification.
Claims (10)
1. the rapid separation and purification method of a compound, it is characterised in that the rapid separation and purification method of described compound is
Fast separating and purifying device is utilized to carry out, wherein,
Described fast separating and purifying device includes:
Solvent unit, described solvent unit includes:
First housing, described first housing limits solvent and accommodates space；
Liquid outlet, described liquid outlet is positioned at the lower end of described first housing,
Chromatography unit, described chromatography unit is connected with described solvent unit, and described chromatography unit includes:
Second housing, described second housing limits filler and accommodates space；
Import, described import is connected with described liquid outlet, is positioned at the upper end of described second housing；
Outlet, described outlet is positioned at the lower end of described second housing,
Loading slot, described loading slot is positioned at described filler and accommodates top of space；And
Receiving unit, described reception unit is connected with described chromatography unit,
The method of the fast separating and purifying of described compound includes:
(1) dress sample: by sample uniform adsorption to be separated on described sample-adding slot packing；
(2) dress post: fill filler to described second housing；
(3) balance: send solvent by described solvent unit to described chromatography unit and be balanced；
(4) sample-adding: the described loading slot after dress sample is loaded in described chromatography unit；
(5) eluting: utilize described solvent unit that described sample to be separated is carried out eluting, in order to isolated purpose compound；
(6) detection: take described purpose compound, is analyzed detection.
Method the most according to claim 1, it is characterised in that in step (1), the sample-loading amount of sample to be separated is
2～3 times of packing volume described in described loading slot.
Method the most according to claim 1, it is characterised in that described loading slot is removable loading slot.
Method the most according to claim 1, it is characterised in that the upper and lower surface of described loading slot is respectively provided with and adds
Sample hole.
Method the most according to claim 5, it is characterised in that the aperture of described well is described packing material size
1/3～2/3.
Method the most according to claim 1, it is characterised in that in step (2), farther include: utilize and take out
Vacuum unit carries out evacuation process to described filler,
Wherein, described vacuum unit includes:
Evacuation drainage hopper, described evacuation drainage hopper is connected with described outlet and described reception unit, described evacuation
Drainage hopper includes bleeding point；And
Evacuation part, described evacuation part is connected with described bleeding point.
Method the most according to claim 1, it is characterised in that described evacuation drainage hopper is detachable evacuation row
Liquid funnel.
Method the most according to claim 1, it is characterised in that in step (2), farther include: utilize sieve
Plate intercepts described filler and flows out from described outlet, and wherein, described sieve plate is positioned at described filler and accommodates space, and is positioned at institute
Stating below filler, described sieve plate includes at least one through hole.
Method the most according to claim 9, it is characterised in that the aperture of described through hole be described packing material size 1/3～
2/3。
Method the most according to claim 9, it is characterised in that the upper surface of described sieve plate has filter membrane.
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| CN201510298605.8A CN106267891B (en) | 2015-06-03 | 2015-06-03 | Method for rapid separation and purification of compound |
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| CN201510298605.8A CN106267891B (en) | 2015-06-03 | 2015-06-03 | Method for rapid separation and purification of compound |
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| CN106267891A true CN106267891A (en) | 2017-01-04 |
| CN106267891B CN106267891B (en) | 2023-06-06 |
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| CN106267891B (en) | 2023-06-06 |
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