CN208607187U - A kind of online purification devices for liquid chromatogram - Google Patents
A kind of online purification devices for liquid chromatogram Download PDFInfo
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- CN208607187U CN208607187U CN201821060634.6U CN201821060634U CN208607187U CN 208607187 U CN208607187 U CN 208607187U CN 201821060634 U CN201821060634 U CN 201821060634U CN 208607187 U CN208607187 U CN 208607187U
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Abstract
The utility model discloses a kind of online purification devices for liquid chromatogram, including switch unit, waste collection unit, sample collection unit, purge unit and control unit, the outlet of the detector of the input end and liquid chromatogram of the switch unit is connected, the waste collection unit and sample collection unit are set to the outlet end of switch unit, the outlet end of the purge unit is connected to sample collection unit, and described control unit is electrically connected with switch unit, purge unit and detector respectively.The online purifying of target compound may be implemented using online purification devices provided by the utility model, the online purification devices of the utility model can be combined with various common liquid chromatographs simultaneously, good compatibility, universality is strong, structure is simple, practical, high degree of automation, purification efficiency is high, has application value.
Description
Technical field
The utility model relates to a kind of online purification devices for liquid chromatogram, belong to chemical separation and purification technology neck
Domain.
Background technique
The post-processing of target compound is an important component of scientific research, and target compound isolates and purifies speed
Degree also affects the speed of scientific research, currently used to isolate and purify means mainly and have column chromatography, recrystallization etc., but for
For the very close mixture of the chemically or physically property of each component part, this conventional isolation technics is obviously difficult to realize
Compound efficiently separates.In response to this, it is mainly isolated and purified at present using chromatographic separation technology.
Liquid chromatogram be at present using most chromatographic processes, because of it with high-resolution, high sensitivity, speed is fast, color
Spectrum column can recycle, flow out the advantages that component easily collecting, and be widely applied to biochemistry, food analysis, medical research,
The various fields such as environmental analysis, inorganic analysis.
Chromatographic system is by liquid storage device, pump, sample injector, chromatographic column, detector, recorder etc. used in liquid chromatogram
A few part compositions；Its working principle is that: the mobile phase in liquid storage device squeezes into system by high-pressure pump, and sample solution enters through sample injector
Mobile phase, by mobile phase be loaded into chromatographic column (stationary phase) in, due to each component in sample solution in two-phase have it is different
Distribution coefficient, when performing relative motion in two-phase, by the assigning process of repeated multiple times absorption-desorption, each component is in movement
Biggish difference is generated in speed, single component is separated into and successively flows out out of column, and when passing through detector, sample concentration is turned
It changes electric signal into and is transmitted to recorder, data are printed in the form of map.
But the existing liquid chromatograph (liquid chromatogram including the big main brand of Thermo, Agilent, Waters tri-
Instrument) do not have enrichment function, if enrichment can only manually connect sample, i.e., it can only artificially collect the sample sets containing target compound
Point then offline removal solvent, isolates and purifies that the time is long, can not canbe used on line target compound purifying, affect scientific research speed
Degree.
Although current scientific research personnel is improved for the purifying function of chromatographic technique, such as Chinese patent
A kind of Two way chromatograms multichannel is disclosed in CN201110442118.6 and isolates and purifies device and method, although reduce separation
Between, it improves separative efficiency, but root chromatogram columns more in the device are connected, isolates and purifies device complexity, higher cost, and
The device, which remains, artificially collects the then offline removal solvent of the sample component containing target compound, not can solve targeted
Close the online issues of purification of object；Organic compound fast separating and purifying device is disclosed in Chinese patent CN201310366213.1
And isolation and purification method, the device are equipped with automatic transfer valve, to change the direction of the flow path in chromatography column, and then shorten color
The chromatographic column chromatographic elution time is composed, reduces and isolates and purifies the time, but to be directed to two kinds of polarity spectrums biggish for the device
Time-consuming during the sample of ingredient isolates and purifies, consuming mobile phase is more, mobile phase can not recycle use, components recoveries are low
The problems such as, it isolates and purifies principle and remains unchanged as traditional chromatographic technique, need first to artificially collect containing target compound
Sample component is then offline to remove solvent, not can solve the online issues of purification of target compound still；It can be seen that current
Chromatogram purification device all still belongs to offline purifying scope, can not canbe used on line target compound purifying.
Utility model content
Exist in view of the above problems existing in the prior art, the purpose of the utility model is to provide a kind of for liquid chromatogram
Line purification devices.
To solve the above problems, the utility model adopts the following technical solution:
A kind of online purification devices for liquid chromatogram, including switch unit, waste collection unit, sample collection list
Member, purge unit and control unit, the outlet of the detector of the input end and liquid chromatogram of the switch unit are connected, described useless
Liquid collector unit and sample collection unit are set to the outlet end of switch unit, the outlet end of the purge unit and sample collection list
Member connection, described control unit are electrically connected with switch unit, purge unit and detector respectively.
As a kind of embodiment, the switch unit includes multi-position switching valve, the multi-position switching valve include import and
The outlet of several outlets, the detector of the import and liquid chromatogram of the multi-position switching valve is connected, the waste collection unit and
Sample collection unit is respectively arranged on the different exits of multi-position switching valve, and described control unit is electrically connected with multi-position switching valve.
Preferably, the multi-position switching valve is pneumatic type multi-position switching valve.
As a kind of scheme, the outlet at least two of the multi-position switching valve.
As a kind of embodiment, the waste collection unit includes waste collection bottle, and the sample collection unit includes
Target product receiving flask, the waste collection bottle and target product receiving flask are set to the outlet end of switch unit, purge unit
The inlet communication of outlet end and target product receiving flask.
As a kind of embodiment, the purge unit includes gas storage device, the outlet of the gas storage device
Mouth is connected with snorkel, and the outlet of the snorkel is connected to sample collection unit.
Preferably, the gas storage device is nitrogen storage device (such as: nitrogen cylinder, nitrogen gas tank etc.), institute
Nitrogen storage device is stated to be electrically connected with control unit.
It preferably, further include absorbing unit, the absorbing unit includes switching valve, multiposition valve and adsorption column, institute
Being connected all the way with the outlet of switch unit for switching valve to be stated, is connected with pressure pump all the way, another way is connected with the import of adsorption column,
The pressure pump is connected with liquid storage device, and the outlet of the adsorption column is connected with the import of multiposition valve, the outlet of the multiposition valve with
Sample collection unit is connected, and the switching valve, multiposition valve, pressure pump are electrically connected with control unit respectively.
Preferably, the switching valve is automatic transfer valve (such as: pneumatic type switching valve), including import and several
Outlet, the import of the switching valve is connected with the outlet of pressure pump, switching valve export respectively with the outlet of switch unit and suction
The import of attached column is connected.
As further preferred scheme, the switching valve includes evacuation port.
As further preferred scheme, the outlet of the switching valve at least two.
Preferably, the multiposition valve is pneumatic type multiposition valve, the outlet of the multiposition valve at least two.
Preferably, further include multidigit sampling unit, the multidigit sampling unit include it is several be connected in parallel it is more
Position sampling valve, the outlet of multidigit sampling valve are connected with sample collection unit, and multidigit sampling valve is electrically connected with control unit.
Preferably, the outlet end of purge unit is connected with the common end of multidigit sampling valve.
Preferably, the multidigit sampling unit is connected with the outlet of switch unit or the outlet of multiposition valve.
Realize that the method purified online is as follows using the online purification devices of the present invention for liquid chromatogram:
It is to flow into the sample component for separating and detecting through liquid chromatogram in switch unit, control unit is according to liquid chromatogram
The testing result control switch unit of detector the sample component of inflow is switched over, make the sample without containing target product
Group is diverted into waste collection unit, flows into the sample component containing target product in sample collection unit, and then purging is single
Member purges the sample component for flowing into sample collection unit, removes the solvent in component, obtains solvent-free target product.
Compared to the prior art, the advantageous effects of the utility model are:
The online purifying of target compound, while this reality may be implemented using online purification devices provided by the utility model
It can be combined with various common liquid chromatographs with novel online purification devices, good compatibility, universality is strong, structure letter
Single, practical, high degree of automation, purification efficiency is high, has application value.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of online purification devices provided by the embodiment of the utility model；
Fig. 2 is the structural schematic diagram of the online purification devices provided by the embodiment of the utility model including absorbing unit；
Fig. 3 is the online purification devices provided by the embodiment of the utility model including absorbing unit and multidigit sampling unit
Structural schematic diagram；
Fig. 4 is the structural representation of the online purification devices provided by the embodiment of the utility model including multidigit sampling unit
Figure；
Figure label is schematically as follows: 1, switch unit；11, the import of switch unit；12, the outlet of switch unit；2, it gives up
Liquid collector unit；3, sample collection unit；4, purge unit；5, the detector of liquid chromatogram；6, the splitter of liquid chromatogram；7,
Absorbing unit；71, switching valve；711, the import of switching valve；712, the outlet of switching valve；713, the evacuation port of switching valve；72, more
Position valve；721, the import of multiposition valve；722, the outlet of multiposition valve；73, adsorption column；74, pressure pump；75, liquid storage device；8, multidigit takes
Sample unit；81, multidigit sampling valve.
Specific embodiment
Below with reference to drawings and examples to the technical solution of the utility model do further it is clear, describe in detail.
Embodiment
It is as shown in Figures 1 to 4: a kind of online purification devices for liquid chromatogram provided by the utility model, including cut
Change unit 1, waste collection unit 2, sample collection unit 3, purge unit 4 and control unit (not shown), the switch unit 1
Input end be connected with the outlet of the detector 5 of liquid chromatogram, the waste collection unit 2 and sample collection unit 3 are set to and cut
Change the outlet end of unit 1, the outlet end of the purge unit 4 is connected to sample collection unit 3, described control unit respectively with cut
Unit 1, purge unit 4 and detector 5 is changed to be electrically connected.
Specifically, the switch unit 1 includes multi-position switching valve, the multi-position switching valve includes import 11 and several outlets
12, the outlet of the detector 5 of the import 11 and liquid chromatogram of institute's rheme switching valve is connected, the waste collection unit 2 and sample
Collector unit 3 is respectively arranged at the different outlets 12 of multi-position switching valve, and described control unit is electrically connected with multi-position switching valve.It is described
The outlet at least two of multi-position switching valve, as shown in Figure 1, setting there are three different outlets 12 in the present embodiment, one of them
Outlet is connect with waste collection unit 2, and residue outlet 12 is connect with sample collection unit 3, meanwhile, the multi-position switching valve is gas
Dynamic formula multi-position switching valve, multi-position switching valve described in the present embodiment are Pneumatic four-way valve.
The waste collection unit 2 includes waste collection bottle, and the sample collection unit 3 includes target product receiving flask,
The waste collection bottle and target product receiving flask are set to the outlet end of switch unit 1 (particularly by waste liquid in the present embodiment
Receiving flask and target product receiving flask are respectively arranged at the different outlets 12 of multi-position switching valve), the outlet end of purge unit 4 and mesh
The inlet communication of collection of products bottle is marked, the component that the purge gass of purge unit 4 collect target product receiving flask is purged, removed
The solvent in component is removed, to obtain solvent-free purified product.
The purge unit 4 includes gas storage device, and the gas outlet of the gas storage device is connected with snorkel (figure
In do not show), the outlet of the snorkel is connected to sample collection unit, due to gas purging class device already belong to more at
Ripe technology, just no longer repeats one by one herein.The gas storage device be nitrogen storage device (such as: nitrogen cylinder, nitrogen gas tank
Deng), the nitrogen storage device is electrically connected with control unit.When needing to carry out target product purging purifying, control is single
Nitrogen storage device, the purge gass (nitrogen) stored in nitrogen storage device (such as: nitrogen cylinder, nitrogen gas tank etc.) are opened in member control
It is sent at sample collection unit 3 by snorkel and (is specifically sent to the inlet of target product receiving flask), sample is received
The component containing target product collected in collection unit 3 is purged, to obtain solvent-free target product.
The method for realizing that compound purifies online using above-mentioned apparatus is as follows:
Make to separate and detect through liquid chromatogram that (particularly sample solution enters the splitter of liquid chromatogram by sample injector
It is separated into several sample components in 6, isolated sample component successively outflow and device 5 after testing, detector from splitter 6
The component flowed through is detected, whether contains target product in judgement sample component) sample component flow into switch unit 1 in
(specific to flow into multi-position switching valve), control unit control (the multidigit switching of switch unit 1 according to the testing result of detector 5
Valve) sample component of inflow is switched over, it flows into the sample component without containing target product in waste collection unit 2, makes
Sample component containing target product flows into sample collection unit 3, then flows into sample collection unit 3 for 4 pairs of purge unit
Sample component is purged, and the solvent in component is removed, and obtains solvent-free target product, repeats aforesaid operations, can be online
The enriching and purifying of sample is completed, that accelerates sample isolates and purifies efficiency.
As a preferred solution:
Liquid chromatogram separates in sample, if the target compound polarity in sample is smaller, mobile phase can be selected
The lesser solvent of polarity is selected, if target compound polarity is larger, mobile phase needs to select the biggish solvent of polarity, such as:
Methanol, ethyl alcohol, acetonitrile and mixed solvent of water etc., in the mixed solvent contains more water, will lead to purge unit 4 be not easy by
Solvent in the sample component collected in sample collection unit 3 removes, and cannot be quickly obtained solvent-free purified product, influences
Purification efficiency, therefore, as shown in Fig. 2, the online purification devices further include absorbing unit 7, the absorbing unit 7 includes switching
Valve 71, multiposition valve 72 and adsorption column 73, being connected all the way with the outlet 12 of switch unit 1 for the switching valve 71, are connected with all the way
Pressure pump 74, another way are connected with the import of adsorption column 73, and the pressure pump 74 is connected with liquid storage device 75, the adsorption column 73
Outlet is connected with the import 721 of multiposition valve 72, and the outlet 722 of the multiposition valve 72 is connected with sample collection unit 3, the switching
Valve 71, multiposition valve 72, pressure pump 74 are electrically connected with control unit respectively.
Specifically, the switching valve 71 is automatic transfer valve (such as: pneumatic type switching valve), including import 711 and several
Outlet 712, the import 711 of the switching valve is connected with the outlet of pressure pump 74, the outlet 712 of switching valve respectively with switch unit
1 outlet is connected with the import of adsorption column 73.In addition, the switching valve 71 includes evacuation port 713, evacuation port is identical as air,
Play the role of balancing 71 internal and external pressure balance of switching valve.
At least there are two (switching valve 71 includes 1 import 711 in the present embodiment, and two go out for the outlet 712 of the switching valve
Mouth 712 and an evacuation port 713, therefore the switching valve 71 is set as Pneumatic four-way valve).
The multiposition valve 72 is pneumatic type multiposition valve, and there are two the outlets 722 at least of the multiposition valve 72, in the present embodiment
Multiposition valve 72 be equipped with 5 outlet 722, therefore the multiposition valve 72 be pneumatic six-way valve.
The method for realizing that compound purifies online using the online purification devices with absorbing unit 7 is as follows:
Flow into the sample component for separating and detecting through liquid chromatogram in switch unit 1, control unit is according to detector 5
The sample component that testing result controls 1 pair of switch unit inflow switches over, and flows into the sample component without containing target product
In waste collection unit 2, the sample component containing target product is made to enter adsorption column 73 by the switching valve 71 in absorbing unit 7
In (so that target compound is captured on adsorption column 73, during this, the multi-position switching valve in switch unit 1 only retains one
A outlet 12 is unimpeded, remaining outlet 12 is closed, and smooth outlet 12 is connected to switching valve 71), it is then turned on pressure pump 74, is made
The organic solvent (such as: the low boiling point organic solvents such as methylene chloride) stored in liquid storage device 75 enters adsorption column by switching valve 71
The target compound captured in 73 to adsorption column 73 elutes, and the solvent composition after elution flows into multiposition valve 72, by more
Position valve 72 and sample collection unit 3 realize that the packing to target compound is collected, and then purge unit 4 is to sample collection unit 3
The sample component of collection is purged, and the solvent in component is removed, and obtains solvent-free target product, repeats aforesaid operations, i.e.,
The enriching and purifying of sample can be completed online, and that accelerates sample isolates and purifies efficiency, from the above process as it can be seen that the absorbing unit of setting
7 can the polarity that flowed out in liquid chromatogram is larger, water content is more, boiling point is higher, be not easy the mobile phase solvent purged replacement
Organic solvent that is lower at boiling point, being easy purging, further improves online purification efficiency.
In addition, in liquid chromatogram separation sample, if sample component is more complicated, the component of required target product compared with
It is more, then, only by the single multiposition valve 72 in the single multi-position switching valve or absorbing unit 7 in switch unit 1, it is difficult suitable
Benefit complete target compound collection and encapsulation, inevitably influence online purification efficiency, therefore, as shown in Figure 3 and Figure 4, it is described
Line purification devices further include multidigit sampling unit 8, and the multidigit sampling unit 8 includes several multidigit sampling valves 81 being connected in parallel
(two multidigit sampling valves 81 being set in the present embodiment, the two can be used alternatingly, to ensure online purification efficiency), multidigit sampling
The outlet of valve 81 is connected with sample collection unit 3, and multidigit sampling valve 81 is electrically connected with control unit.The multidigit sampling unit 8
It is connected (respectively as shown in Fig. 4 and Fig. 3) with the outlet 12 of switch unit 1 or the outlet 722 of multiposition valve 72.At this point, purging is single
The outlet end of member 4 is connected with the common end of multidigit sampling valve 81 or is connected with sample collection unit 3 (purge unit in the present embodiment
4 outlet end is connected with the common end of multidigit sampling valve 81, purges air through multidigit sampling valve 81 and enters in sample collection unit 3
The component collected to sample collection unit 3 purges).
When the multidigit sampling unit 8 is connected with the outlet 12 of switch unit 1, make to separate and detect through liquid chromatogram
Sample component flow into switch unit 1 in, control unit according to the testing result of detector 5 control 1 pair of switch unit inflow
Sample component switches over, and flows into the sample component without containing target product in waste collection unit 2, makes containing target product
Sample component enter any one multidigit sampling valve 81 in multidigit sampling unit 8 (multidigit sampling valve 81 set in the present embodiment
Surely have 16 sample taps) in, realize that the packing to target compound is collected by multidigit sampling valve 81 and sample collection unit 3
(during this, it is unimpeded that the multi-position switching valve in switch unit 1 only retains one outlet 12, remaining outlet 12 is closed, smooth
Outlet 12 is connected to multidigit sampling valve 81), the sample component that then purge unit 4 collects sample collection unit 3 purges,
The solvent in component is removed, solvent-free target product is obtained, repeats aforesaid operations, the enrichment that can complete sample online is pure
Change, from the above process as it can be seen that the multidigit sampling unit 8 of setting can complete the online purifying of the more complex sample of component, into
One step improves online purification efficiency and the scope of application；
When the multidigit sampling unit 8 is connected with the outlet 722 of multiposition valve 72, make to separate and detect through liquid chromatogram
Sample component flow into switch unit 1 in, control unit according to the testing result of detector 5 control 1 pair of switch unit inflow
Sample component switches over, and flows into the sample component without containing target product in waste collection unit 2, makes containing target product
Sample component enter in adsorption column 73 by the switching valve 71 in absorbing unit 7 (so that target compound is captured to absorption
On column 73, during this, the multi-position switching valve in switch unit 1 only retains that one outlet 12 is unimpeded, remaining outlet 12 is closed,
Smooth outlet 12 is connected to switching valve 71), it is then turned on pressure pump 74, makes the organic solvent (low boiling stored in liquid storage device 75
Point organic solvent, such as: methylene chloride) entered in adsorption column 73 by switching valve 71 to the target compound of the capture of adsorption column 73
It is eluted, the solvent composition after elution flows into multiposition valve 72, enters by multiposition valve 72 any in multidigit sampling unit 8
In one multidigit sampling valve 81, realize that the packing to target compound is collected by multidigit sampling valve 81 and sample collection unit 3
(during this, the reservation of multiposition valve 72 one outlet 722 is unimpeded, remaining outlet 722 is closed, and smooth outlet 722 takes with multidigit
Sample valve 81 is connected to), the sample component that then purge unit 4 collects sample collection unit 3 purges, and removes molten in component
Agent obtains solvent-free target product, repeats aforesaid operations, can complete the enriching and purifying of sample online, can from the above process
See, the multidigit sampling unit 8 and absorbing unit 7 concurrently set can complete that component is more and the biggish complex sample of polarity
Line purifying, further improves online purification efficiency and the scope of application.
It is last it is necessarily pointed out that: the foregoing is merely the preferable specific embodiments of the utility model, but this
The protection scope of utility model is not limited thereto, and anyone skilled in the art discloses in the utility model
In technical scope, any changes or substitutions that can be easily thought of, should be covered within the scope of the utility model.
Claims (9)
1. a kind of online purification devices for liquid chromatogram, including waste collection unit and sample collection unit, feature exist
In: it further include switch unit, purge unit and control unit, the switch unit includes multi-position switching valve, the multidigit switching
Valve includes import and several outlets, and the outlet of the detector of the import and liquid chromatogram of the multi-position switching valve is connected, described useless
Liquid collector unit and sample collection unit are respectively arranged on the different exits of multi-position switching valve, the outlet end of the purge unit with
Sample collection unit connection, described control unit are electrically connected with multi-position switching valve, purge unit and detector respectively.
2. the online purification devices according to claim 1 for liquid chromatogram, it is characterised in that: the multi-position switching valve
Outlet at least two.
3. the online purification devices according to claim 1 for liquid chromatogram, it is characterised in that: the waste collection list
Member includes waste collection bottle, and the sample collection unit includes target product receiving flask, the waste collection bottle and target product
Receiving flask is set to the outlet end of switch unit, the outlet end of purge unit and the inlet communication of target product receiving flask.
4. the online purification devices according to claim 1 for liquid chromatogram, it is characterised in that: the purge unit packet
Gas storage device is included, the gas outlet of the gas storage device is connected with snorkel, and the outlet of the snorkel and sample are received
Collect unit connection.
5. the online purification devices according to claim 4 for liquid chromatogram, it is characterised in that: the gas storage dress
It is set to nitrogen storage device, the nitrogen storage device is electrically connected with control unit.
6. the online purification devices according to claim 1 for liquid chromatogram, it is characterised in that: further include that absorption is single
Member, the absorbing unit include switching valve, multiposition valve and adsorption column, the switching valve all the way with the outlet phase of switch unit
Even, it is connected with pressure pump all the way, another way is connected with the import of adsorption column, and the pressure pump is connected with liquid storage device, the absorption
The outlet of column is connected with the import of multiposition valve, and the outlet of the multiposition valve is connected with sample collection unit, the switching valve, multidigit
Valve, pressure pump are electrically connected with control unit respectively.
7. the online purification devices according to claim 6 for liquid chromatogram, it is characterised in that: the switching valve is certainly
Dynamic switching valve, including import and several outlets, the import of the switching valve are connected with the outlet of pressure pump, the outlet point of switching valve
It is not connected with the outlet of switch unit and the import of adsorption column.
8. the online purification devices according to claim 6 for liquid chromatogram, it is characterised in that: further include multidigit sampling
Unit, the multidigit sampling unit include several multidigit sampling valves being connected in parallel, the outlet and sample collection of multidigit sampling valve
Unit is connected, and multidigit sampling valve is electrically connected with control unit.
9. the online purification devices according to claim 8 for liquid chromatogram, it is characterised in that: the multidigit sampling is single
Member is connected with the outlet of switch unit or the outlet of multiposition valve.
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| CN108593810A (en) * | 2018-07-05 | 2018-09-28 | 中国科学院上海有机化学研究所 | A kind of online purification devices and method for liquid chromatogram |
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| CN108593810A (en) * | 2018-07-05 | 2018-09-28 | 中国科学院上海有机化学研究所 | A kind of online purification devices and method for liquid chromatogram |
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