CN108593810A - A kind of online purification devices and method for liquid chromatogram - Google Patents
A kind of online purification devices and method for liquid chromatogram Download PDFInfo
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- CN108593810A CN108593810A CN201810730982.8A CN201810730982A CN108593810A CN 108593810 A CN108593810 A CN 108593810A CN 201810730982 A CN201810730982 A CN 201810730982A CN 108593810 A CN108593810 A CN 108593810A
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- 239000007788 liquid Substances 0.000 title claims abstract description 59
- 238000000746 purification Methods 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000010926 purge Methods 0.000 claims abstract description 40
- 239000002699 waste material Substances 0.000 claims abstract description 28
- 238000005070 sampling Methods 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 27
- 238000003860 storage Methods 0.000 claims description 26
- 230000008676 import Effects 0.000 claims description 25
- 238000001179 sorption measurement Methods 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 17
- 230000006835 compression Effects 0.000 claims description 16
- 238000007906 compression Methods 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 238000004891 communication Methods 0.000 claims description 3
- 238000001228 spectrum Methods 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims 2
- 230000001413 cellular effect Effects 0.000 claims 1
- 239000007791 liquid phase Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 24
- 239000000523 sample Substances 0.000 description 91
- 239000000047 product Substances 0.000 description 32
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000003960 organic solvent Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 238000011160 research Methods 0.000 description 5
- 238000009835 boiling Methods 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 238000010828 elution Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000012856 packing Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 229910001873 dinitrogen Inorganic materials 0.000 description 3
- 239000012488 sample solution Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000012046 mixed solvent Substances 0.000 description 2
- 239000012264 purified product Substances 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000013375 chromatographic separation Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000003891 environmental analysis Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000004186 food analysis Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/027—Liquid chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/065—Preparation using different phases to separate parts of sample
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of online purification devices and method for liquid chromatogram, the online purification devices include switch unit, waste collection unit, sample collection unit, purge unit and control unit, the input end of the switch unit is connected with the outlet of the detector of liquid chromatogram, 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 invention, the online purification devices of the present invention can be combined with various common liquid chromatographs simultaneously, good compatibility, universality is strong, it is simple in structure, highly practical, high degree of automation, purification efficiency is high, has application value.
Description
Technical field
The present invention relates to a kind of online purification devices and method for liquid chromatogram, belong to chemical separation and purification technology neck
Domain.
Background technology
The post-processing of target compound is an important component of scientific research, and target compound isolates and purifies speed
Degree also contributes to the speed of scientific research, currently used to isolate and purify means mainly and have column chromatography, recrystallization etc., but for
For the mixture that the chemically or physically property of each component part is sufficiently close to, this conventional isolation technics is obviously difficult to realize
Compound efficiently separates.For such case, mainly isolated and purified at present using chromatographic separation technology.
Liquid chromatogram is to apply most chromatographic processes at present, 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.
The chromatographic system used in liquid chromatogram is by liquid storage device, pump, injector, chromatographic column, detector, recorder etc.
A few part compositions；Its working principle is that：Mobile phase in liquid storage device squeezes into system by high-pressure pump, and sample solution enters through injector
Mobile phase is loaded by mobile phase in chromatographic column (stationary phase), due to each component in sample solution have in two-phase it is different
Distribution coefficient, when being performed relative motion in two-phase, by the assigning process of repeated multiple times absorption-desorption, each component is in movement
Larger difference is generated in speed, single component is separated into and is flowed out out of column successively, 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 collection of illustrative plates.
But existing liquid chromatograph (includes the liquid chromatogram of tri- big main brand of Thermo, Agilent, Waters
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, separative efficiency is improved, but more root chromatogram columns in the device are connected, device complexity is isolated and purified, cost is higher, and
The device, which remains, artificially collects the then offline removal solvent of the sample component containing target compound, can not 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 larger 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, cannot still solve the online issues of purification of target compound；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.
Invention content
In view of the above-mentioned problems existing in the prior art, the object of the present invention is to provide a kind of for the online pure of liquid chromatogram
Change device and method.
To solve the above problems, the present invention adopts the following technical scheme that：
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 input end of the switch unit are connected with the outlet of the detector of liquid chromatogram, described useless
Liquid collector unit and sample collection unit are set to the outlet end of switch unit, outlet end and the sample collection list of the purge unit
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
Several outlets, the import of the multi-position switching valve are connected with the outlet of the detector of liquid chromatogram, 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 be nitrogen storage device (such as：Nitrogen cylinder, nitrogen gas tank etc.), institute
Nitrogen storage device is stated to be electrically connected with control unit.
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 compression pump all the way, another way is connected with the import of adsorption column,
The compression 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, compression pump are electrically connected with control unit respectively.
Preferably, the switching valve be 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 compression 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.
A method of it is purified online using the online purification devices realization of the present invention for liquid chromatogram, is to make
It is flowed into switch unit through liquid chromatogram detaches and detects sample component, control unit is according to the inspection of the detector of liquid chromatogram
It surveys output control switch unit to switch over the sample component of inflow, the sample component without containing target product is made to flow into waste liquid
In collector unit, the sample component containing target product is made to flow into sample collection unit, then purge unit is to flowing into sample
The sample component of collector unit is purged, and is removed the solvent in component, is obtained solvent-free target product.
Preferably, it is that the sample component for making to detach and detect through liquid chromatogram flows into switch unit, control is single
Member controls switch unit according to the testing result of the detector of liquid chromatogram and is switched over to the sample component of inflow, makes not containing
The sample component of target product flows into waste collection unit, makes the sample component containing target product by absorbing unit
Switching valve enters in adsorption column, is then turned on compression pump, so that the organic solvent stored in liquid storage device is passed through and enters suction in switching valve
Adsorption column is eluted in attached column, the solvent composition after elution flows into multiposition valve, passes through multiposition valve and sample collection unit
Realize that the packing to target compound is collected, the sample component that then purge unit collects sample collection unit purges,
The solvent in component is removed, solvent-free target product is obtained.
Compared to the prior art, the beneficial technical effect of the present invention lies in：
It may be implemented the online purifying of target compound using online purification devices provided by the invention, while the present invention
Online purification devices can be combined with various common liquid chromatographs, and good compatibility, universality is strong, simple in structure, practicability
By force, high degree of automation, purification efficiency is high, has application value.
Description of the drawings
Fig. 1 is the structural schematic diagram of online purification devices provided in an embodiment of the present invention；
Fig. 2 is the structural schematic diagram of the online purification devices provided in an embodiment of the present invention including absorbing unit；
Fig. 3 is the structure of the online purification devices provided in an embodiment of the present invention including absorbing unit and multidigit sampling unit
Schematic diagram；
Fig. 4 is the structural schematic diagram of the online purification devices provided in an embodiment of the present invention including multidigit sampling unit；
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, compression pump；75, liquid storage device；8, multidigit takes
Sample unit；81, multidigit sampling valve.
Specific implementation mode
Below with reference to drawings and examples to technical scheme of the present invention do further it is clear, describe in detail.
Embodiment
As shown in Figures 1 to 4：A kind of online purification devices for liquid chromatogram provided by the invention, including switching are single
Member 1, waste collection unit 2, sample collection unit 3, purge unit 4 and control unit (not shown), the switch unit 1 into
Mouth end is connected with the outlet of the detector 5 of liquid chromatogram, and the waste collection unit 2 and sample collection unit 3 are set to switching list
The outlet end of member 1, the outlet end of the purge unit 4 are connected to sample collection unit 3, and described control unit is single with switching respectively
Member 1, purge unit 4 and detector 5 are 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 import 11 of institute's rheme switching valve is connected with the outlet of the detector 5 of liquid chromatogram, 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 purging purifying to target product, control is single
Member control opening nitrogen storage device, nitrogen storage device (such as：Nitrogen cylinder, nitrogen gas tank etc.) in store purge gass (nitrogen)
It is sent at sample collection unit 3 (inlet for being specifically sent to target product receiving flask) by snorkel, sample is received
The component containing target product collected in collection unit 3 is purged, to obtain solvent-free target product.
Realize that the method that compound purifies online is as follows using above-mentioned apparatus：
Make to detach and detect through liquid chromatogram that (particularly sample solution enters the splitter of liquid chromatogram by injector
Several sample components are separated into 6, the sample component of separation flows out from splitter 6 and passes through detector 5, detector successively
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, so that the sample component without containing target product is flowed into waste collection unit 2, makes
Sample component containing target product flows into sample collection unit 3, and then purge unit 4 is to flowing into sample collection unit 3
Sample component is purged, and the solvent in component is removed, and obtains solvent-free target product, repeats aforesaid operations, you can online
The enriching and purifying of sample is completed, that accelerates sample isolates and purifies efficiency.
Preferably：
Liquid chromatogram detaches in sample, if the target compound polarity in sample is smaller, mobile phase can be selected
The smaller solvent of polarity is selected, if target compound polarity is larger, mobile phase is the solvent for needing to select polarity larger, such as：
The mixed solvent etc. of methanol, ethyl alcohol, acetonitrile and water, in the mixed solvent contain more water, can cause 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 of switch unit 1 12 for the switching valve 71, are connected with all the way
Compression pump 74, another way are connected with the import of adsorption column 73, and the compression 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, compression pump 74 are electrically connected with control unit respectively.
Specifically, the switching valve 71 be 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 compression 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.
Realize that the method that compound purifies online is as follows using the online purification devices with absorbing unit 7：
The sample component for detaching and detecting through liquid chromatogram is set to flow into switch unit 1, control unit is according to detector 5
Testing result control switch unit 1 switches over the sample component of inflow, and the sample component without containing target product is made to flow into
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 unimpeded outlet 12 is connected to switching valve 71), it is then turned on compression pump 74, is made
Stored in liquid storage device 75 organic solvent (such as：The low boiling point organic solvents such as dichloromethane) by switching valve 71 enter adsorption column
The target compound captured to adsorption column 73 in 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 relatively low 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 multi-position switching valve in switch unit 1 or the single multiposition valve 72 in absorbing unit 7, it is difficult to suitable
Profit 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 with the outlet 12 of switch unit 1 or the outlet 722 of multiposition valve 72 and (sees respectively shown in Fig. 4 and Fig. 3).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 detach and detect through liquid chromatogram
Sample component flow into switch unit 1 in, control unit according to the testing result of detector 5 control switch unit 1 to inflow
Sample component switches over, and so that the sample component without containing target product is flowed into 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, unimpeded
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, you can the online enrichment for completing sample 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 detach and detect through liquid chromatogram
Sample component flow into switch unit 1 in, control unit according to the testing result of detector 5 control switch unit 1 to inflow
Sample component switches over, and so that the sample component without containing target product is flowed into waste collection unit 2, makes containing target product
Sample component enter in adsorption column 73 (so that target compound is captured to absorption by the switching valve 71 in absorbing unit 7
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,
Unimpeded outlet 12 is connected to switching valve 71), it is then turned on compression pump 74, makes the organic solvent (low boiling stored in liquid storage device 75
Point organic solvent, such as：Dichloromethane) entered in adsorption column 73 to the target compound of the capture of adsorption column 73 by switching valve 71
It is eluted, the solvent composition after elution flows into multiposition valve 72, enters by multiposition valve 72 arbitrary 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 unimpeded 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, you can the online enriching and purifying for completing sample, it can from the above process
See, the multidigit sampling unit 8 and absorbing unit 7 that concurrently set can complete the complex sample that component is more and polarity is larger
Line purifies, and 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 implementation mode of the present invention, but the present invention
Protection domain be not limited thereto, any one skilled in the art in the technical scope disclosed by the present invention,
The change or replacement that can be readily occurred in, should be covered by the protection scope of the present invention.
Claims (10)
1. a kind of online purification devices for liquid chromatogram, it is characterised in that：Including switch unit, waste collection unit, sample
Product collector unit, purge unit and control unit, the outlet phase of the input end of the switch unit and the detector of liquid chromatogram
Even, the waste collection unit and sample collection unit are set to the outlet end of switch unit, the outlet end of the purge unit with
Sample collection unit is connected to, and described control unit is electrically connected with switch unit, purge unit and detector respectively.
2. the online purification devices according to claim 1 for liquid chromatogram, it is characterised in that：The switch unit packet
Include multi-position switching valve, the multi-position switching valve includes import and several outlets, the import of the multi-position switching valve and liquid chromatogram
The outlet of detector be connected, the waste collection unit and sample collection unit are respectively arranged on the different outlets of multi-position switching valve
Place, described control unit are electrically connected with multi-position switching valve.
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 inlet communication of the outlet end and target product receiving flask of purge unit.
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 outlet and the sample of the snorkel 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 compression pump all the way, another way is connected with the import of adsorption column, and the compression 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, compression 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 compression 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：It further include multidigit sampling
Unit, the multidigit sampling unit include several multidigit sampling valves being connected in parallel, the outlet of multidigit sampling valve and sample collection
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.
10. a kind of realizing the method purified online using the online purification devices for liquid chromatogram described in claim 1,
It is characterized in that：It is that the sample component for making to detach and detect through liquid chromatogram flows into switch unit, control unit is according to liquid phase color
The testing result control switch unit of the detector of spectrum switches over the sample component of inflow, makes the sample without containing target product
Product group is diverted into waste collection unit, so that the sample component containing target product is flowed into sample collection unit, is then purged
The sample component that cellular convection enters sample collection unit is purged, and the solvent in component is removed, and obtains solvent-free target production
Object.
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