CN105092678A - Capillary electrophoresis and eletro-chromatography insert part - Google Patents
Capillary electrophoresis and eletro-chromatography insert part Download PDFInfo
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- CN105092678A CN105092678A CN201510481523.7A CN201510481523A CN105092678A CN 105092678 A CN105092678 A CN 105092678A CN 201510481523 A CN201510481523 A CN 201510481523A CN 105092678 A CN105092678 A CN 105092678A
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Abstract
The invention relates to the technical field of instruments and equipment for analytical chemistry, in particular to a capillary electrophoresis and eletro-chromatography insert part. The capillary electrophoresis and eletro-chromatography insert part comprises a high-voltage power supply, two high-voltage liquid storage tanks fixed with electrodes and a liquid inlet unit for supplying liquid for the high-voltage liquid storage tanks, a capillary tube or an electro-chromatographic column. The liquid inlet unit can be connected to a liquid chromatograph, one pole of the high-voltage power supply is electrically connected with the one electrode, the other pole of the high-voltage power supply is electrically connected with the other electrode or is directly grounded, and the capillary tube or the electro-chromatographic column can be connected between the two high-voltage liquid storage tanks or between one high-voltage liquid storage tank and a mass spectrometer. The capillary electrophoresis and eletro-chromatography insert part is convenient to install and can be directly connected with various liquid chromatographs or the liquid chromatograph and the mass spectrometer for usage. When capillary electrophoretic separation analysis is performed, a sample injector of the liquid chromatograph, a degasser and a high-pressure pump are directly utilized to complete capillary electrophoresis without a single capillary electrophoresis apparatus, and the cost of an analytical instrument is reduced.
Description
Technical field
The present invention relates to the instrument and equipment technical field of analytical chemistry, particularly relate to a kind of Capillary Electrophoresis and the electrochromatography plug-in unit that are connected to liquid chromatograph.
Background technology
Capillary Electrophoresis, also known as high performance capillary electrophoresis, be a kind of is split tunnel with kapillary, take high-voltage dc as the liquid phase separation techniques of driving force; And along with the Stationary liquid of liquid chromatography is introduced in Capillary Electrophoresis, develop again electrochromatographic technique, have the separation mechanism of electrophoresis and liquid chromatography concurrently, expand the range of application of Capillary Electrophoresis further.The operator scheme of Capillary Electrophoresis is many, exploitation analytical approach is easy and compartment analysis effect attracts people's attention, particularly to electrically charged, high polar material, it is faster that Capillary Electrophoresis is usually described as comparatively liquid-phase chromatographic analysis speed, and separation efficiency is higher, the better separate analytical technique of resolution.Although along with commercial liquid chromatograph constantly improves perfect, new instrument, the new technologies such as high performance liquid chromatograph, Ultra Performance Liquid Chromatography instrument, capillary liquid chromatography instrument are also arisen at the historic moment, but liquid chromatography technology is to problems such as the separating substances poor effect of electrically charged, high polarity, still could not reach and solve completely, therefore, capillary electrophoresis technique comparatively liquid chromatography isolation technics is usually more effective, is more conducive to actual use.
But in practical application, liquid chromatograph has been the indispensable basic instrument in laboratory from high end instrument variable body in the past, is widely used in the every field such as chemical, medicine food, environmental monitoring, commodity inspection.And commercial capillary electrophoresis apparatus is because of the limitation of itself, as when with mass spectrometer coupling, need separately to connect a forcing pump again toward contact and introduce sheath fluid, use inconvenience, and commercial capillary electrophoresis apparatus is expensive, causes capillary electrophoresis separation analytical technology to can not show a candle to high performance liquid chromatography separate analytical technique and popularize.
Summary of the invention
For above-mentioned the deficiencies in the prior art, and liquid chromatography can not replace Capillary Electrophoresis, two kinds of technology each tool advantage again, the object of the present invention is to provide a kind of Capillary Electrophoresis and electrochromatography plug-in unit being connected to liquid chromatograph, by Capillary Electrophoresis and liquid chromatography two kinds of combine with technique, it is made mutually to supplement.
To achieve these goals, technical scheme of the present invention is as follows:
A kind of Capillary Electrophoresis and electrochromatography plug-in unit, for kapillary or electric chromatographic column being connected to liquid chromatograph or liquid chromatograph-mass spectrometer coupling, comprising feed liquor unit, high-voltage power supply, be fixed with the first high pressure liquid-accumulating trough of the first electrode and be fixed with the second high pressure liquid-accumulating trough of the second electrode; Described feed liquor unit comprises the one or four connectors and is connected respectively main feed tube, the first feed tube, the second feed tube, the 3rd feed tube and the two or four connectors on four ports of described one or four connectors, described main feed tube is used for being connected with described liquid chromatograph, described first feed tube is communicated in described first high pressure liquid-accumulating trough, and described 3rd feed tube is communicated in described second high pressure liquid-accumulating trough; One pole of described high-voltage power supply is electrically connected on described first electrode, and another pole of described high-voltage power supply is electrically connected on described second electrode, and described first high pressure liquid-accumulating trough is connected with the first joint sleeve; One end of described second feed tube, described first joint sleeve and described kapillary or electric chromatographic column is connected respectively on wherein three ports of described two or four connectors, the other end of described kapillary or electric chromatographic column is connected with the second joint sleeve, and described second joint sleeve and described 3rd feed tube are communicated in described second high pressure liquid-accumulating trough respectively.
Preferably, also comprise the first adjustable pipe on the another port being connected to described two or four connectors, described first adjustable pipe is provided with the first variable valve, described first joint sleeve is provided with the first diverting valve.
Preferably, described first feed tube is provided with the first switch valve, described second feed tube is provided with second switch valve, described 3rd feed tube is provided with the 3rd switch valve.
Preferably, also comprise dispensing unit, described dispensing unit comprises the first drain pipe being connected to described first high pressure liquid-accumulating trough and the second drain pipe being connected to described second high pressure liquid-accumulating trough, the first drain pipe is provided with the first stop valve, described second drain pipe is provided with the second stop valve.
Preferably, described dispensing unit also comprises and is arranged at the first three-way connector on described first feed tube and is connected to second adjustable pipe of described first three-way connector wherein on Single port, described second adjustable pipe is provided with the second variable valve, for regulating the fluid flow entering described first high pressure liquid-accumulating trough.
Preferably, described second joint sleeve is also provided with on-line checkingi device.
Preferably, be can closed groove for described first high pressure liquid-accumulating trough and described second high pressure liquid-accumulating trough.
The combined system of a kind of liquid chromatography-Capillary Electrophoresis or electrochromatography, it comprises Capillary Electrophoresis as above and electrochromatography plug-in unit, liquid chromatograph and kapillary or electric chromatographic column, described liquid chromatography is connected to described main feed tube, and described kapillary or electric chromatographic column are connected between described first joint sleeve and described second joint sleeve.
A kind of Capillary Electrophoresis and electrochromatography plug-in unit, for kapillary or electric chromatographic column being connected to liquid chromatograph or liquid chromatograph-mass spectrometer coupling, comprising feed liquor unit, high-voltage power supply and being fixed with the first high pressure liquid-accumulating trough of the first electrode; Described feed liquor unit comprises the one or four connectors and is connected respectively main feed tube, the first feed tube, the second feed tube, the 3rd feed tube and the two or four connectors on four ports of described one or four connectors, described main feed tube is used for being connected with described liquid chromatograph, and described first feed tube is communicated in described first high pressure liquid-accumulating trough; One pole of described high-voltage power supply is electrically connected on described first electrode, and another extremely direct ground connection of described high-voltage power supply, described first high pressure liquid-accumulating trough is connected with the first joint sleeve; One end of described second feed tube, described first joint sleeve and described kapillary or electric chromatographic column is connected respectively on wherein three ports of described two or four connectors; The other end of described kapillary or electric chromatographic column is communicated with the second joint sleeve, and described second joint sleeve and described 3rd feed tube are communicated in described mass spectrometer respectively.
Preferably, also comprise the first adjustable pipe on the another port being connected to described two or four connectors, described first adjustable pipe is provided with the first variable valve, described first joint sleeve is provided with the first diverting valve.
Preferably, described first feed tube is provided with the first switch valve, described second feed tube is provided with second switch valve, described 3rd feed tube is provided with the 3rd switch valve.
Preferably, also comprise dispensing unit, described dispensing unit comprises the first drain pipe being connected to described first high pressure liquid-accumulating trough, the first drain pipe is provided with the first stop valve.
Preferably, described dispensing unit also comprises and is arranged at the first three-way connector on the first feed tube and is connected to second adjustable pipe of described first three-way connector wherein on Single port, and described second adjustable pipe is provided with the second variable valve.
Preferably, described second joint sleeve is also provided with on-line checkingi device.
Preferably, described first high pressure liquid-accumulating trough is can closed groove.
The combined system of a kind of liquid chromatograph-mass spectrometer-Capillary Electrophoresis or electrochromatography, it comprises Capillary Electrophoresis as above and electrochromatography plug-in unit, described liquid chromatograph, described mass spectrometer and described kapillary or electric chromatographic column, described liquid chromatograph is connected to described main feed tube, described kapillary or electric chromatographic column are connected between described first joint sleeve and described second joint sleeve, and described second joint sleeve and described 3rd feed tube respectively correspondence are communicated in described mass spectrometric electron spray syringe needle.
Beneficial effect of the present invention: (1) is easy for installation, can be directly used in various liquid chromatograph, as liquid chromatographs such as high performance liquid chromatograph, Ultra Performance Liquid Chromatography instrument, preparative liquid chromatograph, ion chromatographs; Also can directly and liquid chromatograph-mass spectrometer coupling;
(2) plug-in unit of the present invention can switch between liquid chromatography and Capillary Electrophoresis and electrochromatography, also different technologies can be combined, and adds the dirigibility of separation method, and voltage and solvent can realize gradient, operator scheme diversification;
(3) directly can utilize the automatic sampler of liquid chromatograph, by shunting or not shunting, accurate sample introduction be carried out to kapillary or electric chromatographic column, improve dosing accuracy; Also directly can utilize the degasser of liquid chromatograph, reduce bubble in damping fluid or solvent, make Capillary Electrophoresis or electrochromatography more stable; Also can directly utilize the high-pressure pump of liquid chromatograph to kapillary or electric chromatographic column carry out forward, oppositely, Bidirectional-pressure and forward and reverse flushing, guarantee bubble-free in kapillary or electric chromatographic column, continue to flow, make separation more efficient, stable; Equally also directly utilize the high-pressure pump of liquid chromatography thoroughly to clean kapillary or electric chromatographic column, reduce kapillary or electric chromatographic column pollution, improve reappearance; Even if during with mass spectrometry, the high-pressure pump of liquid chromatograph also directly can being utilized to provide sheath fluid to Capillary Electrophoresis or capillary electric chromatogram, introducing sheath fluid, lowering apparatus cost without the need to separately joining forcing pump again.
Accompanying drawing explanation
The structural representation of Fig. 1, the embodiment of the present invention 1;
Fig. 2, the embodiment of the present invention 1 are for the structural representation of liquid chromatograph and kapillary or capillary electric chromatographic column coupling;
Fig. 3, the embodiment of the present invention 1 are for being furnished with the liquid chromatograph of fraction collector and preparing the structural representation of electric chromatographic column coupling;
Fig. 4, the embodiment of the present invention 2 are for the structural representation of liquid chromatograph-mass spectrometer and kapillary or capillary electric chromatographic column coupling.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Embodiment 1
As described in Figure 1, a kind of Capillary Electrophoresis and electrochromatography plug-in unit 100, for connecting fluid chromatography 200, comprise feed liquor unit, high-voltage power supply 1, be fixed with the first high pressure liquid-accumulating trough 3a of the first electrode 2a, be fixed with second high pressure liquid-accumulating trough 3b and the dispensing unit of the second electrode 2b, a wherein pole of high-voltage power supply 1 is electrically connected with the first electrode 2a by wire 9a, another pole of high-voltage power supply 1 is electrically connected with the second electrode 2b by wire 9b, first electrode 2a inserts and is fixed in the first high pressure liquid-accumulating trough 3a, second electrode 2b inserts and is fixed in the second high pressure liquid-accumulating trough 3b, and the first electrode 2a and the second electrode 2b is platinum electrode, first high pressure liquid-accumulating trough 3a is connected with the first joint sleeve 4a, second high pressure liquid-accumulating trough 3b is connected with the second joint sleeve 4b, first joint sleeve 4a and the second joint sleeve 4b is provided with interface, be connected to kapillary or capillary electric chromatographic column 30 for correspondence or prepare the two ends of electric chromatographic column 40, in addition, the first high pressure liquid-accumulating trough 3a and the second high pressure liquid-accumulating trough 3b is can closed groove, and it has good elasticity, can bear larger pressure, in addition, for ensureing the sealing of the first high pressure liquid-accumulating trough 3a and the second high pressure liquid-accumulating trough 3b, its inlet and liquid outlet are provided with joint (11a, 11b, 11c, 11d), by joint (11a, 11b, 11c, 11d) be connected with feed tube or drain pipe, also facilitate the installation and removal of feed tube and drain pipe.
Feed liquor unit comprises the one or four connectors 5a and corresponding main feed tube 8, first feed tube 8a, the second feed tube 8b, the 3rd feed tube 8c be connected on four ports of the one or four connectors 5a, main feed tube 8 is for being connected with liquid chromatograph 200, first feed tube 8a is connected on interface 11a, be communicated in the first high pressure liquid-accumulating trough 3a, fluid injection can be carried out to the first high pressure liquid-accumulating trough 3a, second feed tube 8b is for being communicated with kapillary or capillary electric chromatographic column 30 or preparing electric chromatographic column 40, and the 3rd feed tube 8c is communicated in the second high pressure liquid-accumulating trough 3b, particularly, this Capillary Electrophoresis and electrochromatography plug-in unit 100 also comprise the two or four connectors 5b, second feed tube 8b, the first joint sleeve 4a, kapillary or capillary electric chromatographic column 30 or prepare electric chromatographic column 40 correspondence and be connected on wherein three ports of the two or four connectors 5b, remaining Single port is connected with the first adjustable pipe 7a, particularly, kapillary or capillary electric chromatographic column 30 are connected on the port of the two or four connectors 5b by the 3rd joint sleeve 4c, and then are communicated with the first joint sleeve 4a, first adjustable pipe 7a is provided with the first variable valve 13a, first variable valve 13a is by regulating shunt volume to control kapillary or capillary electric chromatographic column 30 or preparing the sample size of electric chromatographic column 40, in addition the first joint sleeve 4a is provided with the first diverting valve 14a, the joint 11a place that first feed tube 8a is communicated with the first high pressure liquid-accumulating trough 3a is provided with the first switch valve 15a, first switch valve 15a also can be set directly on the first feed tube 8a, second feed tube 8b is provided with second switch valve 15b, it is identical with the first switch valve 15a, also can be set directly on the port of the one or four connectors 5a or the two or four connectors 5b, the interface 11c place that 3rd feed tube 8c is communicated with the second high pressure liquid-accumulating trough 3b is provided with the 3rd switch valve 15c, certain 3rd switch valve 15c also can be set directly on the 3rd feed tube 8c.
This Capillary Electrophoresis and electrochromatography plug-in unit 100 also comprise dispensing unit, dispensing unit comprises the first drain pipe 10a being connected to the first high pressure liquid-accumulating trough 3a and the second drain pipe 10b being connected to the second high pressure liquid-accumulating trough 3b particularly, first drain pipe 10a is provided with the first stop valve 12a, the second drain pipe 10b is provided with the second stop valve 12b; This dispensing unit also comprises the three-way connector 16 be arranged on the first feed tube 8a, specifically arranges detailed in Example 2 and Fig. 4; In addition, second joint sleeve 4b is provided with detection window (not shown), and be furnished with on-line checkingi device 6, this on-line checkingi device 6 can be ultraviolet-visible detector, diode array detector, non-contact electric conductivity detector or other on-line checkingi device.
As shown in Figure 2, Capillary Electrophoresis and electrochromatography plug-in unit 100 are directly used on existing liquid chromatograph 200, Capillary Electrophoresis and capillary electric chromatogram function can be realized, main feed tube 8 is connected to the automatic sampler 24 of liquid chromatograph 200, and wherein one end of kapillary or capillary electric chromatographic column 30 is connected with the 3rd joint sleeve 4c, the other end is connected with the second joint sleeve 4b, namely completes installation.Before using, ensure that all valves are all arranged on closed condition, first open the first stop valve 12a and the second stop valve 12b, discharge to make the air in the first high pressure liquid-accumulating trough 3a and the second high pressure liquid-accumulating trough 3b or residual liquid, close the first stop valve 12a and the second stop valve 12b subsequently, make all valves all be in closed condition.During use, first open the first switch valve 15a and the 3rd switch valve 15c, in the first high pressure liquid-accumulating trough 3a and the second high pressure liquid-accumulating trough 3b, pump into damping fluid in surge flask 25 or solvent by the high-pressure pump 23 of liquid chromatograph 200; After pumping into appropriate damping fluid or solvent, close the 3rd switch valve 15c, open the first diverting valve 14a and the second stop valve 12b, namely carry out forward flushing by high-pressure pump 23 pairs of kapillaries of liquid chromatograph 200 or capillary electric chromatographic column 30; Close the first switch valve 15a, the first diverting valve 14a and the second stop valve 12b subsequently, open second switch valve 15b, sample introduction is carried out by automatic sampler 24 pairs of kapillaries of liquid chromatograph 200 or capillary electric chromatographic column 30, regulate the first variable valve 13a Quality control shunt volume simultaneously, namely accurate sample introduction is carried out to kapillary or capillary electric chromatographic column 30; Finally close second switch valve 15b and the first variable valve 13a, and open the first diverting valve 14a, open high-voltage power supply 1, to two liquid-accumulating trough (3a, 3b) making alives, carry out the separation to sample; In detachment process, the first switch valve 15a and the 3rd switch valve 15c can be opened as required, be pressurizeed to two ends by the high-pressure pump 23 of liquid chromatograph 200, improve stability and the reappearance of sample separation; Also high-voltage power supply 1 can be closed at any time, and open the first switch valve 15a and the second stop valve 12b, pump into damping fluid or solvent by the high-pressure pump 23 of liquid chromatograph 200 to the first high pressure liquid-accumulating trough 3a, realize in Capillary Electrophoresis and the switching between electrochromatography and liquid chromatography; High-voltage power supply 1 is alive while, the first switch valve 15a and the second stop valve 12b can also be opened, pump into damping fluid or solvent by the high-pressure pump 23 of liquid chromatograph 200, thus liquid chromatography and Capillary Electrophoresis and electrochromatographic technique are combined; If kapillary or capillary electric chromatographic column 30 block in use procedure, high-voltage power supply 1 can also be closed, and open the first stop valve 12a and the 3rd switch valve 15c, carry out counterflush by the high-pressure pump 23 of liquid chromatograph 200.In addition, in detachment process, directly can use the original temperature-controlling system of liquid chromatograph 200, or separately join the Joule heat that cooling system produces to eliminate electrophoresis according to actual needs.
As shown in Figure 3, Capillary Electrophoresis and electrochromatography plug-in unit 100 can also be directly used in be furnished with on the liquid chromatograph 200 of fraction collector 21, realizes preparing electrochromatography function.During installation, first the wherein Single port of four connectors 5a is connected on the automatic sampler 24 of liquid chromatograph 200 by main feed tube 8, again the wherein one end of preparing electric chromatographic column 40 is connected with the port of the two or four connectors 5b remainder, the other end is connected with the second joint sleeve 4b, then the second drain pipe 10b is connected on one of them port of the second three-way connector 16b, second three-way connector 16b another one port is connected to the fraction collector 21 of liquid chromatograph 200 by the 4th feed tube 8d, a port of the remainder of the second three-way connector 16b is connected to other detecting device (as mass detector) by the 5th drain pipe 10e, can can open the 3rd stop valve 12c as required to distribute the efflux that sub-fraction prepares electrochromatography and send into this detecting device, thus realize detecting the dual-detector of separator.After installation, operation in using and Capillary Electrophoresis described before similar, difference is, when on-line checkingi device 6 detects separator, the 3rd switch valve 15c, the second stop valve 12b need be opened, pressurizeed by the high-pressure pump 23 of liquid chromatograph 200 again, corresponding separator is sent into fraction collector 21; In addition, usually without the need to shunting when preparing electrochromatography sample introduction, therefore, be also with above-mentioned Capillary Electrophoresis or capillary electric chromatogram difference, the first variable valve 13a can be closed during sample introduction.
Embodiment 2
Embodiment 1 is roughly the same with embodiment 2, its difference is only, as shown in Figure 4, Capillary Electrophoresis and electrochromatography plug-in unit 100 ' only need a first high pressure liquid-accumulating trough 3a being fixed with the first electrode 2a, at this, one end of high-voltage power supply 1 is electrically connected with electrode 2a by wire 9a, the other end is by the direct ground connection of wire 9b, be communicated with the electron spray syringe needle 51 on mass spectrometer with kapillary or wherein one end of capillary electric chromatographic column 30, 3rd feed tube 8c is also directly connected on the interface of electron spray syringe needle 51, dispensing unit also comprises and is arranged at the first three-way connector 16a on the first feed tube 8a and is connected to the second adjustable pipe 7b of the first three-way connector 16a wherein on Single port in addition, described second adjustable pipe 7b is provided with the second variable valve 13b, the fluid flow flowing into electron spray syringe needle 51 through the 3rd feed tube 8c is regulated by the second variable valve 13b.
Particularly, this Capillary Electrophoresis and electrochromatography plug-in unit 100 ', for kapillary or capillary electric chromatographic column 30 are connected to liquid chromatograph-mass spectrometer coupling, comprise feed liquor unit, high-voltage power supply 1 and be fixed with the first high pressure liquid-accumulating trough 3a of the first electrode 2a; Feed liquor unit comprises the one or four connectors 5a and main feed tube 8, the first feed tube 8a be connected respectively on four ports of the one or four connectors 5a, the second feed tube 8b, the 3rd feed tube 8c and the two or four connectors 5b, wherein main feed tube 8 is for being connected with liquid chromatograph 200, and the first feed tube 8a is communicated in the first high pressure liquid-accumulating trough 3a; One pole of high-voltage power supply 1 is electrically connected on the first electrode 2a, and another extremely direct ground connection of high-voltage power supply 1, the first high pressure liquid-accumulating trough 3a is connected with the first joint sleeve 4a; Second feed tube 8b, the first joint sleeve 4a and the 3rd joint sleeve 4c are connected respectively on wherein three ports of described two or four connectors; One end of kapillary or capillary electric chromatographic column 30 is connected to the 3rd joint sleeve 4c, the other end of kapillary or capillary electric chromatographic column 30 connects two joint sleeve 4b ', and the second joint sleeve 4b and the 3rd feed tube 8c is communicated in kapillary socket 51a and the sheath fluid entrance 51b of mass spectrometric electron spray syringe needle 51 respectively; Dispensing unit comprises the first drain pipe 10a being connected to the first high pressure liquid-accumulating trough 3a, the first drain pipe 10a is provided with the first stop valve 12a; This external first feed tube 8a is also provided with the first three-way connector 16a, wherein two ports of the first three-way connector 16a are communicated in the first feed tube 8a respectively, first switch valve 15a is arranged between the first three-way connector 16a and the first high pressure liquid-accumulating trough 3a, the another port of the first three-way connector 16a is connected with the second adjustable pipe 7b, the second adjustable pipe 7b is provided with the second variable valve 13b; Second joint sleeve 4b ' is also provided with detection window (not shown), and be furnished with on-line checkingi device 6, this on-line checkingi device 6 can be ultraviolet-visible detector, diode array detector, non-contact electric conductivity detector or other on-line checkingi device; In addition, owing to not needing the second high pressure liquid-accumulating trough 3b, the difference of this real embodiment and embodiment 1 is also that dispensing unit does not comprise 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 chromatograph-mass spectrometer coupling, realize capillary electrophoresis-laser-induced fluorescence and capillary electric chromatogram-mass spectrometry function.In use, only need the main feed tube 8 of the one or four connectors 5a upper end be connected on the automatic sampler 24 of liquid chromatograph 200, again wherein one end of kapillary or capillary electric chromatographic column 30 is connected with the port of the two or four connectors 5b remainder by the 3rd joint sleeve 4c, the other end connects kapillary 30a by the second joint sleeve 4b ', again kapillary 30a is inserted the kapillary socket 51a of electron spray syringe needle 51,3rd feed tube 8c is connected to the sheath fluid entrance 51b of electron spray syringe needle 51, namely completes installation.Capillary Electrophoresis in other operation used and embodiment 1 and capillary electric chromatogram similar: before use, first open the first stop valve 12a, by air residual in high pressure liquid-accumulating trough 3a or liquid discharge, more all valves be all arranged on closed condition; During use, only the first switch valve 15a be need open, namely damping fluid or solvent injected by high-pressure pump 23 to high pressure liquid-accumulating trough 3a; After injecting damping fluid or solvent, only need open the first diverting valve 14a again, namely rinse by high-pressure pump 23 pairs of kapillaries or capillary electric chromatographic column 30; Close the first switch valve 15a and the first diverting valve 14a subsequently, open second switch valve 15b, then regulate the first variable valve 13a Quality control shunt volume, namely carry out accurate sample introduction by automatic sampler 24 pairs of kapillaries of liquid chromatography or capillary electric chromatographic column 30; Close second switch valve 15b and the first variable valve 13a subsequently and open the 3rd switch valve 15c, the high-pressure pump 23 of liquid chromatograph 200 is utilized to provide sheath fluid, only need open the second variable valve 13b can shunt sheath fluid, the sheath fluid distributed can be collected and reuse; Finally open the first diverting valve 14a to be separated sample by high-voltage power supply 1 making alive.Do not need connection second high pressure liquid-accumulating trough 3b in the present embodiment, directly mass spectroscopy is carried out to the sample after separation, therefore, kapillary or capillary electric chromatographic column 30 are connected with mass spectrometer directly or indirectly through kapillary, direct injected measures, and structure is simple, and easy to use.
Can be found out by above-mentioned two embodiments: Capillary Electrophoresis and electrochromatography plug-in unit 100,100 ' the automatic sampler 24 that directly can utilize liquid chromatograph 200, by shunting or do not shunt kapillary or capillary electric chromatographic column 30 or prepare electric chromatographic column 40 and carry out accurate sample introduction, improve dosing accuracy; Also directly can utilize the degasser 22 of liquid chromatograph 200, reduce bubble in damping fluid or solvent, make Capillary Electrophoresis or electrochromatography more stable; Simultaneously Capillary Electrophoresis and electrochromatography plug-in unit 100 ' also directly can utilize high-pressure pump 23 pairs of kapillaries of liquid chromatograph 200 or capillary electric chromatographic column 30 or prepare electric chromatographic column 40 carry out forward, oppositely, Bidirectional-pressure and forward and reverse flushing, guarantee kapillary or capillary electric chromatographic column 30 or prepare bubble-free in electric chromatographic column 40, continue to flow, making separation more efficient, stable; Even if when Capillary Electrophoresis and electrochromatography plug-in unit 100 ' are with mass spectrometry, high-pressure pump 23 pairs of kapillaries of liquid chromatograph 200 or capillary electric chromatographic column 30 can be directly utilized thoroughly to clean equally, minimizing kapillary or capillary electric chromatographic column 30 pollute, improve reappearance, also high-pressure pump 23 pairs of Capillary Electrophoresis of liquid chromatograph 200 or capillary electric chromatogram can be directly utilized to provide sheath fluid, introducing sheath fluid without the need to separately joining forcing pump again, reducing analytical instrument cost, improving the utilization factor of analytical instrument.In addition, consider actual safety problem, pipeline, joint and valve all in above-mentioned two embodiments have insulating material to make.
Above-described embodiment, just preferred embodiment of the present invention, is not used for limiting the scope of the present invention, therefore all equivalences done with the structure described in the claims in the present invention, feature and principle change or modify, and all should be included within the claims in the present invention scope.
Claims (10)
1. a Capillary Electrophoresis and electrochromatography plug-in unit, for kapillary or electric chromatographic column being connected in liquid chromatograph or liquid chromatograph-mass spectrometer coupling, it is characterized in that: comprise feed liquor unit, high-voltage power supply, be fixed with the first high pressure liquid-accumulating trough of the first electrode and be fixed with the second high pressure liquid-accumulating trough of the second electrode; Described feed liquor unit comprises the one or four connectors and is connected respectively main feed tube, the first feed tube, the second feed tube, the 3rd feed tube and the two or four connectors on four ports of described one or four connectors, described main feed tube is used for being connected with described liquid chromatograph, and described first feed tube is communicated in described first high pressure liquid-accumulating trough; One pole of described high-voltage power supply is electrically connected on described first electrode, another pole of described high-voltage power supply is electrically connected on described second electrode or direct ground connection, described first high pressure liquid-accumulating trough is connected with the first joint sleeve, one end of described second feed tube, described first joint sleeve and described kapillary or electric chromatographic column is connected respectively on wherein three ports of described two or four connectors, and the other end of described kapillary or electric chromatographic column is communicated with the second joint sleeve;
When another pole of described high-voltage power supply is electrically connected with described second electrode, described second joint sleeve and described 3rd feed tube are communicated in described second high pressure liquid-accumulating trough respectively; When described high-voltage power supply another extremely directly ground connection time, described second joint sleeve and described 3rd feed tube are communicated in described mass spectrometer respectively.
2. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterized in that: also comprise the first adjustable pipe on the another port being connected to described two or four connectors, described first adjustable pipe is provided with the first variable valve, described first joint sleeve is provided with the first diverting valve.
3. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, is characterized in that: described first feed tube is provided with the first switch valve, and described second feed tube is provided with second switch valve, and described 3rd feed tube is provided with the 3rd switch valve.
4. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterized in that: also comprise dispensing unit, described dispensing unit comprises the first drain pipe being connected to described first high pressure liquid-accumulating trough and the second drain pipe being connected to described second high pressure liquid-accumulating trough, first drain pipe is provided with the first stop valve, described second drain pipe is provided with the second stop valve.
5. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, it is characterized in that: described dispensing unit also comprises and is arranged at the first three-way connector on described first feed tube and is connected to second adjustable pipe of described first three-way connector wherein on Single port, and described second adjustable pipe is provided with the second variable valve.
6. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, is characterized in that: described second joint sleeve is also provided with on-line checkingi device.
7. Capillary Electrophoresis according to claim 1 and electrochromatography plug-in unit, is characterized in that: described first high pressure liquid-accumulating trough and described second high pressure liquid-accumulating trough are can closed groove.
8. the combined system of liquid chromatograph-Capillary Electrophoresis or electrochromatography, it is characterized in that: it comprise Capillary Electrophoresis as described in any one of claim 1 ~ 7 and electrochromatography plug-in unit, as described in liquid chromatograph and as described in kapillary or electric chromatographic column, described liquid chromatography is connected to described main feed tube, and described kapillary or electric chromatographic column are communicated between described first joint sleeve and described second joint sleeve.
9. the combined system of liquid chromatograph-mass spectrometer-Capillary Electrophoresis or electrochromatography, it is characterized in that: it comprise Capillary Electrophoresis as described in any one of claim 1 ~ 7 and electrochromatography plug-in unit, as described in liquid chromatograph, as described in mass spectrometer and as described in kapillary or electric chromatographic column, described liquid chromatograph is connected to described main feed tube, described kapillary or electric chromatographic column are connected between described first joint sleeve and described second joint sleeve, and described second joint sleeve and described 3rd feed tube are connected respectively in described mass spectrometer.
10. the combined system of liquid chromatograph-mass spectrometer-Capillary Electrophoresis according to claim 9 or electrochromatography, is characterized in that: described mass spectrometer is connected with described second joint sleeve and described 3rd feed tube respectively by electron spray syringe needle.
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