CN105092678B - A kind of Capillary Electrophoresis and electrochromatography plug-in unit - Google Patents
A kind of Capillary Electrophoresis and electrochromatography plug-in unit Download PDFInfo
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- CN105092678B CN105092678B CN201510481523.7A CN201510481523A CN105092678B CN 105092678 B CN105092678 B CN 105092678B CN 201510481523 A CN201510481523 A CN 201510481523A CN 105092678 B CN105092678 B CN 105092678B
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Abstract
The present invention relates to the instrument and equipment technical field of analytical chemistry, more particularly to a kind of Capillary Electrophoresis and electrochromatography plug-in unit, including high voltage power supply, two high pressure liquid-accumulating troughs for being fixed with electrode and for the feed liquor unit to high pressure liquid-accumulating trough, capillary or electric chromatographic column feed flow；Feed liquor unit may connect to liquid chromatograph, one pole of high voltage power supply electrically connects with a wherein electrode, another pole of high voltage power supply electrically connects or is directly grounded with another electrode, and capillary or electric chromatographic column may connect between two high pressure liquid-accumulating troughs or wherein between a high pressure liquid-accumulating trough and mass spectrograph；The present invention is easy for installation, it can be directly used for various liquid chromatograph or liquid chromatograph and mass spectrograph combinations, when capillary electrophoresis separation is analyzed, directly Capillary Electrophoresis is completed using the injector, degasser and high-pressure pump of liquid chromatogram, without single HPCE, reduce analytical instrument cost.
Description
Technical field
The present invention relates to the instrument and equipment technical field of analytical chemistry, more particularly to a kind of liquid chromatograph that may connect to
Capillary Electrophoresis and electrochromatography plug-in unit.
Background technology
Capillary Electrophoresis is also known as HPCE, be one kind using capillary as split tunnel, with high-voltage dc
For the liquid phase separation techniques of driving force；And with the stationary phase of liquid chromatogram is introduced into Capillary Electrophoresis, electric color is developed again
Spectral technology, has electrophoresis and the separation mechanism of liquid chromatogram concurrently, further expands the application of Capillary Electrophoresis.Capillary electricity
The operator scheme of swimming is more, exploitation analysis method easily and separation analytical effect attracts people's attention, particularly to electrically charged, highly polar thing
Matter, Capillary Electrophoresis are usually described as compared with liquid-phase chromatographic analysis speed faster, and separative efficiency is higher, resolution ratio preferably separation point
Analysis technology.Perfect, high performance liquid chromatograph, ultra performance liquid chromatography are continuously improved although as the liquid chromatograph of commercialization
New instrument, the new technologies such as instrument, capillary liquid chromatography instrument are also arisen at the historic moment, but liquid chromatography technology is to electrically charged, highly polar
Material separating effect it is bad the problems such as, still could not enough be fully solved, therefore, capillary electrophoresis technique compared with liquid chromatogram separate skill
Art is usually more effective, is more beneficial for actually using.
But in practical application, liquid chromatograph is the indispensable basic instrument in laboratory from high end instrument variable body in the past,
It is widely used in the every field such as chemical, medicine food, environmental monitoring, commodity inspection.And commercial HPCE because
The limitation of itself, such as when being combined with mass spectrograph, often also need to separately connect a compression pump introducing sheath fluid again, use is not square
Just, and commercial HPCE is expensive, causes capillary electrophoresis separation analytical technology to can not show a candle to high performance liquid chromatography point
Popularized from analytical technology.
The content of the invention
For above-mentioned the deficiencies in the prior art, and liquid chromatogram can not substitute Capillary Electrophoresis, and two kinds of technologies respectively have excellent again
Gesture, object of the present invention is to provide a kind of Capillary Electrophoresis that may connect to liquid chromatograph and electrochromatography plug-in unit, by hair
Two kinds of technologies of cons electrophoresis and liquid chromatogram combine, and are complementary to one another it.
To achieve these goals, technical scheme is as follows：
A kind of Capillary Electrophoresis and electrochromatography plug-in unit, for capillary or electric chromatographic column to be connected into liquid chromatograph or liquid
The combination of chromatography-mass spectrograph, including feed liquor unit, high voltage power supply, the first high pressure liquid-accumulating trough for being fixed with first electrode and solid
Surely there is the second high pressure liquid-accumulating trough of second electrode；The feed liquor unit includes the one or four connectors and is connected respectively in institute
State main feed tube, the first feed tube, the second feed tube, the 3rd feed tube and on four ports of the one or four connectors
Two or four connectors, the main feed tube are used to be connected with the liquid chromatograph, and first feed tube is communicated in described the
One high pressure liquid-accumulating trough, the 3rd feed tube are communicated in the second high pressure liquid-accumulating trough；The pole electrical connection of the high voltage power supply
In the first electrode, another pole of the high voltage power supply is electrically connected to the second electrode, on the first high pressure liquid-accumulating trough
It is connected with the first connection sleeve pipe；The one of second feed tube, first connection sleeve pipe and the capillary or electric chromatographic column
End be connected respectively in the two or four connectors wherein on three ports, the capillary or electric chromatographic column it is another
End is connected with the second connection sleeve pipe, and second connection sleeve pipe and the 3rd feed tube are respectively communicated with to be stored in second high pressure
Liquid bath.
It is preferred that also include being connected to the first regulation pipe on the another port of the two or four connectors, described the
The first regulating valve is provided with one regulation pipe, the first flow divider is provided with first connection sleeve pipe.
It is preferred that being provided with first switch valve on first feed tube, being provided with second on second feed tube opens
Valve is closed, the 3rd switch valve is provided with the 3rd feed tube.
It is preferred that also including dispensing unit, the dispensing unit includes being connected to the first of the first high pressure liquid-accumulating trough
Drain pipe and the second drain pipe for being connected to the second high pressure liquid-accumulating trough, the first stop valve, institute are provided with the first drain pipe
State and the second stop valve is provided with the second drain pipe.
It is preferred that the dispensing unit also includes the first three-way connector and the connection being arranged on first feed tube
The second regulation is provided with second regulation pipe of first three-way connector wherein on Single port, second regulation pipe
Valve, for the fluid flow for entering the first high pressure liquid-accumulating trough to be adjusted.
It is preferred that it is additionally provided with on-line checking device in second connection sleeve pipe.
It is preferred that the first high pressure liquid-accumulating trough and the second high pressure liquid-accumulating trough are can closed groove.
A kind of combined system of liquid chromatogram-Capillary Electrophoresis or electrochromatography, it includes Capillary Electrophoresis as described above
And electrochromatography plug-in unit, liquid chromatograph and capillary or electric chromatographic column, the liquid chromatogram is connected to the main feed tube, described
Capillary or electric chromatographic column are connected between first connection sleeve pipe and second connection sleeve pipe.
A kind of Capillary Electrophoresis and electrochromatography plug-in unit, for capillary or electric chromatographic column to be connected into liquid chromatograph or liquid
Chromatography-mass spectrograph combination, including feed liquor unit, high voltage power supply and the first high pressure liquid-accumulating trough for being fixed with first electrode；Institute
Stating feed liquor unit includes the one or four connectors and is connected respectively on four ports of the one or four connectors
Main feed tube, the first feed tube, the second feed tube, the 3rd feed tube and the two or four connectors, the main feed tube are used for
It is connected with the liquid chromatograph, first feed tube is communicated in the first high pressure liquid-accumulating trough；The one of the high voltage power supply
Pole is electrically connected to the first electrode, and another pole of the high voltage power supply is directly grounded, and is connected on the first high pressure liquid-accumulating trough
There is the first connection sleeve pipe；Second feed tube, first connection sleeve pipe and one end of the capillary or electric chromatographic column point
Wherein on three ports of the two or four connectors are not correspondingly connected to；The other end of the capillary or electric chromatographic column connects
The second connection sleeve pipe is connected with, second connection sleeve pipe and the 3rd feed tube are respectively communicated with the mass spectrograph.
It is preferred that also include being connected to the first regulation pipe on the another port of the two or four connectors, described the
The first regulating valve is provided with one regulation pipe, the first flow divider is provided with first connection sleeve pipe.
It is preferred that being provided with first switch valve on first feed tube, being provided with second on second feed tube opens
Valve is closed, the 3rd switch valve is provided with the 3rd feed tube.
It is preferred that also including dispensing unit, the dispensing unit includes being connected to the first of the first high pressure liquid-accumulating trough
Drain pipe, the first stop valve is provided with the first drain pipe.
It is preferred that the dispensing unit also includes the first three-way connector being arranged on the first feed tube and is connected to institute
Second regulation pipe of first three-way connector wherein on Single port is stated, the second regulating valve is provided with second regulation pipe.
It is preferred that it is additionally provided with on-line checking device in second connection sleeve pipe.
It is preferred that the first high pressure liquid-accumulating trough is can closed groove.
A kind of combined system of liquid chromatograph-mass spectrograph-Capillary Electrophoresis or electrochromatography, it includes hair as described above
Cons electrophoresis and electrochromatography plug-in unit, the liquid chromatograph, the mass spectrograph and the capillary or electric chromatographic column, the liquid phase
Chromatograph is connected to the main feed tube, and the capillary or electric chromatographic column are connected to first connection sleeve pipe and described second
Between connection sleeve pipe, second connection sleeve pipe and the 3rd feed tube correspond to be communicated in the mass spectrometric electron spray respectively
Syringe needle.
Beneficial effects of the present invention：(1) it is easy for installation, it can be directly used for various liquid chromatographs, such as high performance liquid chromatography
The liquid chromatographs such as instrument, Ultra Performance Liquid Chromatography instrument, preparative liquid chromatograph, ion chromatograph；Also can directly and liquid chromatogram
Instrument-mass spectrograph combination；
(2) plug-in unit of the invention can switch between liquid chromatogram and Capillary Electrophoresis and electrochromatography, also can will not
It is combined with technology, adds the flexibility of separation method, and voltage and solvent can realize gradient, operator scheme is polynary
Change；
(3) automatic sampler of liquid chromatograph can be directly utilized, by shunting or not shunting to capillary or electric color
Compose post and carry out accurate sample introduction, improve dosing accuracy；Also can directly utilize liquid chromatograph degasser, reduce buffer solution or
Bubble in solvent, make Capillary Electrophoresis or electrochromatography more stable；Also can be directly using the high-pressure pump of liquid chromatograph to capillary
Or electric chromatographic column carry out it is positive, reversely, Bidirectional-pressure and forward and reverse flushing, it is ensured that bubble-free in capillary or electric chromatographic column, no
Cutout, make separation more efficiently, stably；Equally also directly capillary or electric chromatographic column are carried out using the high-pressure pump of liquid chromatogram
Thoroughly cleaning, capillary or electric chromatographic column pollution are reduced, improves reappearance；Even if during with mass spectrometry, it also can directly utilize liquid
The high-pressure pump of chromatography provides sheath fluid to Capillary Electrophoresis or capillary electric chromatogram, without separately introducing sheath fluid with compression pump again,
Lowering apparatus cost.
Brief description of the drawings
Fig. 1, the embodiment of the present invention 1 structural representation；
Fig. 2, the embodiment of the present invention 1 are used for structural representation associated with liquid chromatograph and capillary or capillary electric chromatographic column
Figure；
Fig. 3, the embodiment of the present invention 1 are used for the liquid chromatograph equipped with fraction collector and prepare knot associated with electric chromatographic column
Structure schematic diagram；
Fig. 4, the embodiment of the present invention 2 are used for associated with liquid chromatograph-mass spectrograph and capillary or capillary electric chromatographic column
Structural representation.
Embodiment
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1
As described in Figure 1, a kind of Capillary Electrophoresis and electrochromatography plug-in unit 100, for connecting liquid chromatograph 200, including enters
Liquid unit, high voltage power supply 1, the first high pressure liquid-accumulating trough 3a for being fixed with first electrode 2a, it is fixed with the second high of second electrode 2b
Press liquid-accumulating trough 3b and dispensing unit；A wherein pole for high voltage power supply 1 is electrically connected by wire 9a with first electrode 2a, high voltage power supply
1 another pole is electrically connected by wire 9b with second electrode 2b, and first electrode 2a is inserted and fixed in the first high pressure liquid-accumulating trough 3a
In, second electrode 2b is inserted and fixed in the second high pressure liquid-accumulating trough 3b, and first electrode 2a and second electrode 2b are platinum electricity
Pole, it is connected with the first connection sleeve pipe 4a, the second high pressure liquid-accumulating trough 3b on the first high pressure liquid-accumulating trough 3a and is connected with the second adapter sleeve
Interface is provided with pipe 4b, the first connection sleeve pipe 4a and the second connection sleeve pipe 4b, for being correspondingly connected to capillary or capillary
Pipe electric chromatographic column 30 or the both ends for preparing electric chromatographic column 40；In addition, the first high pressure liquid-accumulating trough 3a and the second high pressure liquid-accumulating trough 3b are equal
For can closed groove, it has good elasticity, can bear larger pressure；In addition, for ensure the first high pressure liquid-accumulating trough 3a and
Second high pressure liquid-accumulating trough 3b sealing, joint (11a, 11b, 11c, 11d) is provided with its inlet and liquid outlet, is passed through
Joint (11a, 11b, 11c, 11d) is connected with feed tube or drain pipe, is also convenient for the installation and removal of feed tube and drain pipe.
Feed liquor unit includes the one or four connectors 5a and is correspondingly connected on the one or four connectors 5a four ports
Main feed tube 8, the first feed tube 8a, the second feed tube 8b, the 3rd feed tube 8c, main feed tube 8 is used for and liquid chromatograph
200 connections, the first feed tube 8a are connected on interface 11a, are communicated in the first high pressure liquid-accumulating trough 3a, can be to the first high pressure liquid-accumulating trough
3a carries out fluid injection；Second feed tube 8b is used to connect capillary or capillary electric chromatographic column 30 or prepares electric chromatographic column 40, and the 3rd
Feed tube 8c is communicated in the second high pressure liquid-accumulating trough 3b；Specifically, the Capillary Electrophoresis and electrochromatography plug-in unit 100 also include the two or four
Connectors 5b, the second feed tube 8b, the first connection sleeve pipe 4a, capillary or capillary electric chromatographic column 30 prepare electric chromatographic column
40 are correspondingly connected to wherein on three ports of the two or four connectors 5b, and the first regulation pipe is connected with remaining Single port
7a, specifically, capillary or capillary electric chromatographic column 30 can be connected to the two or four connectors 5b by the 3rd connection sleeve pipe 4c
Port on, and then connected with the first connection sleeve pipe 4a；The first regulating valve 13a, the first regulation are provided with first regulation pipe 7a
Valve 13a can control capillary or capillary electric chromatographic column 30 or the sample size for preparing electric chromatographic column 40 by adjusting shunt volume,
In addition the first flow divider 14a, the first feed tube 8a is provided with the first connection sleeve pipe 4a and connects connecing for the first high pressure liquid-accumulating trough 3a
First switch valve 15a is provided with head 11a, first switch valve 15a can also be set directly on the first feed tube 8a, and second enters
Second switch valve 15b is provided with liquid pipe 8b, it is identical with first switch valve 15a, can also be set directly at the one or four and lead to
On the port for meeting device 5a or the two or four connectors 5b, the 3rd feed tube 8c is connected at the second high pressure liquid-accumulating trough 3b interface 11c
The 3rd switch valve 15c is provided with, certain 3rd switch valve 15c can also be set directly on the 3rd feed tube 8c.
The Capillary Electrophoresis and electrochromatography plug-in unit 100 also include dispensing unit, and specifically dispensing unit includes being connected to the
One high pressure liquid-accumulating trough 3a the first drain pipe 10a and the second drain pipe 10b for being connected to the second high pressure liquid-accumulating trough 3b, first goes out liquid
It is provided with pipe 10a on the first stop valve 12a, the second drain pipe 10b and is provided with the second stop valve 12b；The dispensing unit also wraps
The three-way connector 16 being arranged on the first feed tube 8a is included, it is specific that detailed in Example 2 and Fig. 4 are set；In addition, the second adapter sleeve
Pipe 4b is provided with detection window (not shown), and is furnished with on-line checking device 6, and the on-line checking device 6 can be ultraviolet-visible inspection
Survey device, PDAD, non-contact electric conductivity detector or other on-line checking devices.
As shown in Fig. 2 Capillary Electrophoresis and electrochromatography plug-in unit 100 are directly used on existing liquid chromatograph 200, you can
Capillary Electrophoresis and capillary electric chromatogram function are realized, main feed tube 8 is connected to the automatic sampler of liquid chromatograph 200
24, and wherein one end of capillary or capillary electric chromatographic column 30 is connected with the 3rd connection sleeve pipe 4c, the other end and second connects
The 4b connections of female connector pipe, that is, complete installation.Before use, ensureing that all valves are all disposed within closed mode, the first cut-off is first opened
Valve 12a and the second stop valve 12b, so that air or residual liquid in the first high pressure liquid-accumulating trough 3a and the second high pressure liquid-accumulating trough 3b
Discharge, is then turned off the first stop valve 12a and the second stop valve 12b, makes all valves all in closed mode.In use,
First switch valve 15a and the 3rd switch valve 15c are first turned on, is stored by the high-pressure pump 23 of liquid chromatograph 200 to the first high pressure
The buffer solution or solvent being pumped into liquid bath 3a and the second high pressure liquid-accumulating trough 3b in surge flask 25；It is being pumped into appropriate buffer solution or molten
After agent, the 3rd switch valve 15c is closed, opens the first flow divider 14a and the second stop valve 12b, you can pass through liquid chromatograph
200 high-pressure pump 23 carries out positive flushing to capillary or capillary electric chromatographic column 30；It is then turned off first switch valve 15a,
One flow divider 14a and the second stop valve 12b, second switch valve 15b is opened, passes through the automatic sampler 24 of liquid chromatograph 200
Sample introduction is carried out to capillary or capillary electric chromatographic column 30, while adjusts the first regulating valve 13a control sample shunt volumes, i.e., to hair
Tubule or capillary electric chromatographic column 30 carry out accurate sample introduction；Second switch valve 15b and the first regulating valve 13a is finally closed, and is opened
The first flow divider 14a is opened, high voltage power supply 1 is opened, to two liquid-accumulating troughs (3a, 3b) making alive, carries out the separation to sample；Separating
During, first switch valve 15a and the 3rd switch valve 15c can be opened as needed, pass through the high-pressure pump 23 of liquid chromatograph 200
Pressurizeed to both ends, improve the stability and reappearance of sample separation；High voltage power supply 1 can also be closed at any time, and is opened first and opened
Valve 15a and the second stop valve 12b is closed, buffering is pumped into the first high pressure liquid-accumulating trough 3a by the high-pressure pump 23 of liquid chromatograph 200
Liquid or solvent, realize the switching between Capillary Electrophoresis and electrochromatography and liquid chromatogram；Can also be in the making alive of high voltage power supply 1
While, first switch valve 15a and the second stop valve 12b is opened, buffer solution is pumped into by the high-pressure pump 23 of liquid chromatograph 200
Or solvent, so as to which liquid chromatogram and Capillary Electrophoresis and electrochromatographic technique are combined；If capillary or hair during use
Tubule electric chromatographic column 30 blocks, and can also close high voltage power supply 1, and opens the first stop valve 12a and the 3rd switch valve 15c, leads to
The high-pressure pump 23 for crossing liquid chromatograph 200 carries out back flush.In addition, liquid chromatograph can be directly used in separation process
200 original temperature-controlling systems, or according to being actually needed separately with cooling system come Joule heat caused by eliminating electrophoresis.
As shown in figure 3, Capillary Electrophoresis and electrochromatography plug-in unit 100 can also be directly used in the liquid equipped with fraction collector 21
On chromatography 200, realization prepares electrochromatography function.During installation, four connectors 5a wherein Single port is passed through into master first
Feed tube 8 is connected on the automatic sampler 24 of liquid chromatograph 200, then the wherein one end and second that will prepare electric chromatographic column 40
The remaining port connections of four connectors 5b, the other end is connected with the second connection sleeve pipe 4b, then by the second drain pipe 10b connections
Onto the second three-way connector 16b one of port, second another port of three-way connector 16b passes through the 4th feed liquor
Pipe 8d is connected to the fraction collector 21 of liquid chromatograph 200, and the second three-way connector 16b remaining a port passes through
Five drain pipe 10e are connected to other detectors (such as mass detector)；The 3rd stop valve 12c can be opened as needed to distribute
The efflux that sub-fraction prepares electrochromatography is sent into the detector, so as to realize the dual detector detection to isolate.Install
Cheng Hou, the operation in use is similar with the Capillary Electrophoresis of the foregoing description, except that, when on-line checking device 6 detects point
During from thing, the 3rd switch valve 15c, the second stop valve 12b need to be opened, then is pressurizeed by the high-pressure pump 23 of liquid chromatograph 200,
Corresponding isolate is sent into fraction collector 21；In addition, typically without shunting when preparing electrochromatography sample introduction, therefore, with above-mentioned hair
Cons electrophoresis or capillary electric chromatogram also differ in that, can close the first regulating valve 13a during sample introduction.
Embodiment 2
Embodiment 1 is roughly the same with embodiment 2, and it is differed only in, as shown in figure 4, Capillary Electrophoresis and electrochromatography are inserted
Part 100 ' only needs a first high pressure liquid-accumulating trough 3a for being fixed with first electrode 2a, here, one end of high voltage power supply 1 is by leading
Line 9a is electrically connected with electrode 2a, and the other end is directly grounded by wire 9b, and capillary or capillary electric chromatographic column 30 are wherein
One end connects with the electron spray syringe needle 51 on mass spectrograph, and the 3rd feed tube 8c is also directly connected in the interface of electron spray syringe needle 51
On, dispensing unit also includes the first three-way connector 16a being arranged on the first feed tube 8a and is connected to the first threeway in addition
Connector 16a is provided with the second regulating valve 13b on the second regulation pipe 7b, the second regulation pipe 7b wherein on Single port, can
Fluid flow through the 3rd feed tube 8c inflow electron sprays syringe needle 51 is adjusted by the second regulating valve 13b.
Specifically, the Capillary Electrophoresis and electrochromatography plug-in unit 100 ', for capillary or capillary electric chromatographic column 30 to be connected
It is connected to liquid chromatograph-mass spectrograph combination, including feed liquor unit, high voltage power supply 1 and the first high pressure for being fixed with first electrode 2a
Liquid-accumulating trough 3a；Feed liquor unit includes the one or four connectors 5a and is connected respectively in the one or four connectors 5a four ends
Main feed tube 8, the first feed tube 8a, the second feed tube 8b, the 3rd feed tube 8c and the two or four connectors 5b on mouth, its
Middle main feed tube 8 is used to be connected with liquid chromatograph 200, and the first feed tube 8a is communicated in the first high pressure liquid-accumulating trough 3a；High-tension electricity
One pole in source 1 is electrically connected to first electrode 2a, and another pole of high voltage power supply 1 is directly grounded, and is connected on the first high pressure liquid-accumulating trough 3a
There is the first connection sleeve pipe 4a；Second feed tube 8b, the first connection sleeve pipe 4a and the 3rd connection sleeve pipe 4c are connected respectively in institute
State wherein on three ports of the two or four connectors；One end of capillary or capillary electric chromatographic column 30 is connected to the 3rd connection
The other end of sleeve pipe 4c, capillary or capillary electric chromatographic column 30 connects two connection sleeve pipe 4b ', the second connection sleeve pipe 4b and the 3rd
Feed tube 8c is respectively communicated with capillary socket 51a and sheath fluid entrance 51b in mass spectrometric electron spray syringe needle 51；Dispensing unit bag
Include and be provided with the first stop valve 12a on the first the drain pipe 10a, the first drain pipe 10a for be connected to the first high pressure liquid-accumulating trough 3a；This
The first three-way connector 16a, the first three-way connector 16a two of which port point is additionally provided with external first feed tube 8a
Be not communicated in the first feed tube 8a, first switch valve 15a be arranged on the first three-way connector 16a and the first high pressure liquid-accumulating trough 3a it
Between, it is connected with the first three-way connector 16a another port on the second regulation pipe 7b, the second regulation pipe 7b and is provided with the second tune
Save valve 13b；It is also equipped with detecting window (not shown) on second connection sleeve pipe 4b ', and is furnished with on-line checking device 6, the online inspection
It can be ultraviolet-visible detector, PDAD, non-contact electric conductivity detector or other on-line checkings to survey device 6
Device；Further, since not needing the second high pressure liquid-accumulating trough 3b, this real embodiment also differ in that out liquid list with embodiment 1
Member does not include the second drain pipe 10b.
As shown in figure 4, the Capillary Electrophoresis in the present embodiment and electrochromatography plug-in unit 100 ' are directly used in existing liquid phase
In chromatograph-mass spectrometer combination, capillary electrophoresis-laser-induced fluorescence and capillary electric chromatogram-mass spectrometry function are realized.Using
When, the main feed tube 8 of the one or four connectors 5a upper ends need to be only connected on the automatic sampler 24 of liquid chromatograph 200,
Again by wherein one end of capillary or capillary electric chromatographic column 30 by more than the 3rd connection sleeve pipe 4c and the two or four connectors 5b
Under port connection, the other end connects capillary 30a by the second connection sleeve pipe 4b ', then capillary 30a is inserted into electron spray
Capillary the socket 51a, the 3rd feed tube 8c of syringe needle 51 are connected to the sheath fluid entrance 51b of electron spray syringe needle 51, that is, complete installation.
Other operations in use are similar with the Capillary Electrophoresis in embodiment 1 and capillary electric chromatogram：Before use, first open first section
Only valve 12a, the air or liquid that are remained in high pressure liquid-accumulating trough 3a are discharged, then all valves are all disposed within closed mode；
In use, it need to only open first switch valve 15a, you can buffer solution or solvent are injected to high pressure liquid-accumulating trough 3a by high-pressure pump 23；
Inject after buffer solution or solvent, only need to be then turned on the first flow divider 14a, you can by high-pressure pump 23 to capillary or capillary
Electric chromatographic column 30 is rinsed；First switch valve 15a and the first flow divider 14a are then turned off, opens second switch valve 15b, then
Adjust the first regulating valve 13a control sample shunt volumes, you can by the automatic sampler 24 of liquid chromatogram to capillary or capillary
Pipe electric chromatographic column 30 carries out accurate sample introduction；It is then turned off second switch valve 15b and the first regulating valve 13a and opens the 3rd switch valve
15c, sheath fluid is provided using the high-pressure pump 23 of liquid chromatograph 200, only need to open the second regulating valve 13b can divide sheath fluid
Stream, the sheath fluid distributed can collect reuse；Finally open the first flow divider 14a and pass through the making alive of high voltage power supply 1
Sample is separated.The second high pressure liquid-accumulating trough 3b need not be connected in the present embodiment, and directly the sample after separation is carried out
Mass spectroscopy, therefore, capillary or capillary electric chromatographic column 30 are connected directly or indirectly through capillary with mass spectrograph, are directly entered
Sample is measured, simple in construction, and easy to use.
It can be seen that by above-mentioned two embodiment：Capillary Electrophoresis and electrochromatography plug-in unit 100,100 ' can directly utilize liquid chromatogram
The automatic sampler 24 of instrument 200, by shunting or not shunting to capillary or capillary electric chromatographic column 30 or prepare electrochromatography
Post 40 carries out accurate sample introduction, improves dosing accuracy；Also the degasser 22 of liquid chromatograph 200 can be directly utilized, is reduced slow
Bubble in fliud flushing or solvent, make Capillary Electrophoresis or electrochromatography more stable；Capillary Electrophoresis and electrochromatography plug-in unit 100 ' simultaneously
Directly to capillary or capillary electric chromatographic column 30 or electric chromatographic column 40 can be prepared enter using the high-pressure pump 23 of liquid chromatograph 200
Row forward direction, reverse, Bidirectional-pressure and forward and reverse flushing, it is ensured that capillary or capillary electric chromatographic column 30 prepare electric chromatographic column
Bubble-free in 40, do not stop, make separation more efficiently, stably；Even if Capillary Electrophoresis and electrochromatography plug-in unit 100 ' join with mass spectrum
Used time, equally directly capillary or capillary electric chromatographic column 30 can be carried out thoroughly using the high-pressure pump 23 of liquid chromatograph 200
Cleaning, reduces capillary or capillary electric chromatographic column 30 pollutes, and improves reappearance, also can directly utilize liquid chromatograph 200
High-pressure pump 23 provides sheath fluid to Capillary Electrophoresis or capillary electric chromatogram, without separately introducing sheath fluid with compression pump again, reduces analysis
Instrument cost, improve the utilization rate of analytical instrument.It is all in above-mentioned two embodiment furthermore, it is contemplated that actual safety problem
Pipeline, joint and valve have insulating materials to be made.
Above-described embodiment, simply presently preferred embodiments of the present invention, is not used for limiting the scope of the present invention, therefore all with this
The equivalent change or modification that construction, feature and principle described in invention claim are done, all should be included in right of the present invention will
Within the scope of asking.
Claims (10)
1. a kind of Capillary Electrophoresis and electrochromatography plug-in unit, for capillary or electric chromatographic column to be connected into liquid chromatograph or liquid phase
In chromatograph-mass spectrometer combination, it is characterised in that：Including feed liquor unit, high voltage power supply, the first high pressure for being fixed with first electrode
Liquid-accumulating trough and the second high pressure liquid-accumulating trough for being fixed with second electrode；The feed liquor unit includes the one or four connectors and right respectively
The main feed tube that should be connected on four ports of the one or four connectors, the first feed tube, the second feed tube, the 3rd enter
Liquid pipe and the two or four connectors, the main feed tube are used to be connected with the liquid chromatograph, and first feed tube connects
Pass through the first high pressure liquid-accumulating trough；One pole of the high voltage power supply is electrically connected to the first electrode, the high voltage power supply
Another pole is electrically connected to the second electrode or is directly grounded, and the first connection sleeve pipe is connected with the first high pressure liquid-accumulating trough,
Second feed tube, first connection sleeve pipe and one end of the capillary or electric chromatographic column are connected respectively in described
Wherein on three ports of two or four connectors, the other end of the capillary or electric chromatographic column is communicated with the second adapter sleeve
Pipe；
When another pole of the high voltage power supply electrically connects with the second electrode, second connection sleeve pipe and the 3rd feed liquor
Pipe is respectively communicated with the second high pressure liquid-accumulating trough；When another pole of the high voltage power supply is directly grounded, second connection
Sleeve pipe and the 3rd feed tube are respectively communicated with the mass spectrograph.
2. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterised in that：Also include being connected to described the
The first regulation pipe on the another port of two or four connectors, is provided with the first regulating valve in first regulation pipe, and described
The first flow divider is provided with one connection sleeve pipe.
3. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterised in that：Set on first feed tube
First switch valve is equipped with, second switch valve is provided with second feed tube, being provided with the 3rd on the 3rd feed tube opens
Close valve.
4. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterised in that：Also include dispensing unit, institute
Stating dispensing unit includes being connected to the first drain pipe of the first high pressure liquid-accumulating trough and is connected to the second high pressure liquid-accumulating trough
The second drain pipe, be provided with the first stop valve on the first drain pipe, the second stop valve be provided with second drain pipe.
5. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterised in that：The dispensing unit also includes
The first three-way connector for being arranged on first feed tube and first three-way connector is connected to wherein on Single port
The second regulation pipe, be provided with the second regulating valve in second regulation pipe.
6. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterised in that：In second connection sleeve pipe
It is additionally provided with on-line checking device.
7. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterised in that：The first high pressure liquid-accumulating trough
Being with the second high pressure liquid-accumulating trough can closed groove.
A kind of 8. combined system of liquid chromatograph-Capillary Electrophoresis or electrochromatography, it is characterised in that：It includes such as claim
Capillary Electrophoresis and electrochromatography plug-in unit, the liquid chromatograph and the capillary or electric chromatographic column described in 1~7 any one,
The liquid chromatogram is connected to the main feed tube, and the capillary or electric chromatographic column are communicated in first connection sleeve pipe and institute
State between the second connection sleeve pipe.
A kind of 9. combined system of liquid chromatograph-mass spectrograph-Capillary Electrophoresis or electrochromatography, it is characterised in that：It is included such as
Capillary Electrophoresis and electrochromatography plug-in unit, the liquid chromatograph, the mass spectrograph and institute described in any one of claim 1~7
Capillary or electric chromatographic column are stated, the liquid chromatograph is connected to the main feed tube, capillary or the electric chromatographic column connection
Between first connection sleeve pipe and second connection sleeve pipe, second connection sleeve pipe and the 3rd feed tube difference
It is correspondingly connected to the mass spectrograph.
10. the combined system of liquid chromatograph-mass spectrograph-Capillary Electrophoresis according to claim 9 or electrochromatography, it is special
Sign is：The mass spectrograph is connected with second connection sleeve pipe and the 3rd feed tube respectively by electron spray syringe needle.
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| CN201510481523.7A CN105092678B (en) | 2015-08-03 | 2015-08-03 | A kind of Capillary Electrophoresis and electrochromatography plug-in unit |
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| CN201510481523.7A CN105092678B (en) | 2015-08-03 | 2015-08-03 | A kind of Capillary Electrophoresis and electrochromatography plug-in unit |
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| CN105092678B true CN105092678B (en) | 2018-03-09 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105548325B (en) * | 2016-01-30 | 2018-01-12 | 福州大学 | Capillary Electrophoresis rotary shaft drop sampling device and its sample injection method |
| CN117269287A (en) * | 2023-11-20 | 2023-12-22 | 中国计量科学研究院 | Ink-jet sample injection-capillary electrophoresis-mass spectrum combined device and working method |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62257055A (en) * | 1986-04-30 | 1987-11-09 | Shimadzu Corp | Equal velocity electrophoretic apparatus |
| CN1036265A (en) * | 1988-02-16 | 1989-10-11 | 应用生物系统公司 | Capillary electrophoresis |
| JPH0611484A (en) * | 1991-09-04 | 1994-01-21 | Hewlett Packard Co <Hp> | Capillary electrohporesis apparatus and apparatus and method for controlling electroendos- mose in flow in capillary electrophoresis |
| CN2476022Y (en) * | 2001-04-20 | 2002-02-06 | 阎超 | Multichannel pressure capillary tube electrochromatographic biological sample analyser |
| CN2476817Y (en) * | 2001-04-20 | 2002-02-13 | 天润通微(天津)分析技术有限公司 | Quantitative sample feeding gradient pressured capillary electrophoresis device |
| CN2552004Y (en) * | 2002-03-21 | 2003-05-21 | 复旦大学 | Interface for efficient liquid chromatograph and capillary tube electrophoresis 2-D separating system |
| CN201434855Y (en) * | 2009-06-16 | 2010-03-31 | 福州大学 | Linking interface device of capillary tube electrophoresis and jigger coupling plasma mass spectrograph |
| CN102016559A (en) * | 2008-03-07 | 2011-04-13 | 不列颠哥伦比亚大学 | Self-contained capillary electrophoresis system for interfacing with mass spectrometry |
| CN102890111A (en) * | 2012-06-15 | 2013-01-23 | 南京大学 | Device for detecting microchip electrophoresis by time and space resolution and application thereof |
| CN204989098U (en) * | 2015-08-03 | 2016-01-20 | 李绍平 | Capillary electrophoresis and electrochromatography plug -in components |
-
2015
- 2015-08-03 CN CN201510481523.7A patent/CN105092678B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62257055A (en) * | 1986-04-30 | 1987-11-09 | Shimadzu Corp | Equal velocity electrophoretic apparatus |
| CN1036265A (en) * | 1988-02-16 | 1989-10-11 | 应用生物系统公司 | Capillary electrophoresis |
| JPH0611484A (en) * | 1991-09-04 | 1994-01-21 | Hewlett Packard Co <Hp> | Capillary electrohporesis apparatus and apparatus and method for controlling electroendos- mose in flow in capillary electrophoresis |
| CN2476022Y (en) * | 2001-04-20 | 2002-02-06 | 阎超 | Multichannel pressure capillary tube electrochromatographic biological sample analyser |
| CN2476817Y (en) * | 2001-04-20 | 2002-02-13 | 天润通微(天津)分析技术有限公司 | Quantitative sample feeding gradient pressured capillary electrophoresis device |
| CN2552004Y (en) * | 2002-03-21 | 2003-05-21 | 复旦大学 | Interface for efficient liquid chromatograph and capillary tube electrophoresis 2-D separating system |
| CN102016559A (en) * | 2008-03-07 | 2011-04-13 | 不列颠哥伦比亚大学 | Self-contained capillary electrophoresis system for interfacing with mass spectrometry |
| CN201434855Y (en) * | 2009-06-16 | 2010-03-31 | 福州大学 | Linking interface device of capillary tube electrophoresis and jigger coupling plasma mass spectrograph |
| CN102890111A (en) * | 2012-06-15 | 2013-01-23 | 南京大学 | Device for detecting microchip electrophoresis by time and space resolution and application thereof |
| CN204989098U (en) * | 2015-08-03 | 2016-01-20 | 李绍平 | Capillary electrophoresis and electrochromatography plug -in components |
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| CN105092678A (en) | 2015-11-25 |
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