CN211426396U - Automatic sample introduction and analysis device for multiple samples - Google Patents
Automatic sample introduction and analysis device for multiple samples Download PDFInfo
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- CN211426396U CN211426396U CN201922053302.6U CN201922053302U CN211426396U CN 211426396 U CN211426396 U CN 211426396U CN 201922053302 U CN201922053302 U CN 201922053302U CN 211426396 U CN211426396 U CN 211426396U
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- 238000001514 detection method Methods 0.000 claims description 33
- 239000002699 waste material Substances 0.000 claims description 9
- 238000001802 infusion Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 abstract description 10
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- 238000000520 microinjection Methods 0.000 description 2
- 238000011002 quantification Methods 0.000 description 2
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- 238000000926 separation method Methods 0.000 description 2
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Abstract
The utility model relates to a many samples carry out autoinjection analytical equipment relates to cell analysis technical field for solve the technical problem of sample loss. The utility model discloses a many samples carry out autoinjection analytical equipment, including sampling device and liquid chromatography device, sampling device include with the multichannel microfluid diverter valve that the liquid chromatography device links to each other switches on through the passageway selectivity that links to each other with the liquid chromatography device in the multichannel microfluid diverter valve, can switch the passageway that switches on after the completion is advanced to last sample to carry out next sample and advance the appearance process, consequently can carry out autoinjection analysis to many samples on line in real time, wherein the sample loading obstacle that the evaporation caused has been avoided to the sample liquid of continuous flow, thereby the technical problem of sample loss has been solved.
Description
Technical Field
The utility model relates to a cell analysis technical field especially relates to a many samples carry out autoinjection analytical equipment.
Background
In recent years, aiming at the hot research directions of cell analysis, drug research and the like in the academia at present, the microfluid technology can be used for simulating different organ models in vitro with the characteristics of obvious low cost and high flux; mass spectrometry, as a powerful analytical technique, is particularly useful for identifying biomacromolecule structures, such as cell-secreted factors or drug molecular structures. Therefore, the microfluidic technology and the mass spectrometry technology are combined, the high-sensitivity mass spectrometry technology is integrated at the tail end of a multi-channel microfluidic chip, and different biological samples can be subjected to highly parallel online analysis, so that a large amount of drug toxicity screening work in a new drug research and development stage is greatly improved and promoted. In addition, the combination of the two technologies has important development and application in the fields of separation processing and detection of complex multi-component samples, such as environmental monitoring, food detection and the like.
Conventional methods often use a length of fused silica capillary as an interface to connect the outlet of the microfluidic channel to the inlet of the mass spectrometer. This method lacks a high degree of integration and results in some sample loss. Moreover, the multi-channel detection depends on manual switching, and the method is time-consuming and labor-consuming and cannot realize automatic and high-flux detection. Thus. How to establish a microfluid-mass spectrometry interface for realizing on-line, fast and efficient switching of multiple microfluids becomes a great challenge at present.
SUMMERY OF THE UTILITY MODEL
The utility model provides a many samples carry out autoinjection analytical equipment for solve the technical problem of sample loss.
According to a first aspect of the present invention, the present invention provides an automatic sample introduction and analysis device for multiple samples, comprising a sampling device and a liquid chromatography device, wherein the sampling device comprises a multi-channel micro-fluid switching valve connected to the liquid chromatography device via a tapping line,
wherein, the multichannel microfluid switching valve has two at least passageways, and the passageway selectively leads to with connect out the pipeline.
In one embodiment, the multi-channel microfluidic switching valve comprises a first switching valve, the passageway comprises a first inlet/outlet port disposed on the first switching valve;
the first switching valve is further provided with an external interface, one end of the external interface is selectively communicated with one of the first inlet/outlet, and the other end of the external interface is connected with the liquid chromatography device through the outlet pipeline.
In one embodiment, the sampling device further comprises:
a chip for carrying a sample; and
a second switching valve arranged above the first switching valve, at least two second inlet/outlet ports arranged on the second switching valve, the second inlet/outlet ports and the first inlet/outlet ports being arranged in one-to-one correspondence,
the second inlet/outlet is used for receiving the sample input by the chip and inputting the sample into the first inlet/outlet.
In one embodiment, the first inlet/outlet ports are provided on the first switching valve at equal intervals in a circumferential direction of the first switching valve, and the second inlet/outlet ports are provided on the second switching valve at equal intervals in a circumferential direction of the second switching valve.
In one embodiment, the first switching valve is rotatably disposed below the second switching valve, and an angle of each rotation of the first switching valve is an included angle between two adjacent first inlet/outlet ports.
In one embodiment, at least one sample channel is disposed in the chip, and the sample channel is communicated with the second inlet/outlet corresponding to the sample channel.
In one embodiment, the liquid chromatography apparatus comprises:
a mobile phase storage bottle for storing a mobile phase;
the detection device is used for detecting the sample; and
the device comprises a through valve at least provided with two interfaces, a quantitative ring is arranged between the two interfaces, one interface is communicated with the external interface or the mobile phase storage bottle, and the other interface is communicated with the detection device or the waste liquid bottle.
In one embodiment, the sampling device further comprises a micro-syringe pump for delivering a sample into the chip.
In one embodiment, the mobile phase storage bottle is connected to the through valve by an infusion pump.
In one embodiment, the detection device comprises a chromatographic column and a detector connected in series.
Compared with the prior art, the utility model has the advantages of, selectively switch on through the passageway that links to each other with the liquid chromatography device in the multichannel microfluid diverter valve, can advance the passageway that switches on after kind accomplishes at last sample to carry out next sample and advance the appearance process, consequently can carry out the autoinjection analysis to many samples on line in real time, wherein the sample loading obstacle that the evaporation caused has been avoided to the sample liquid of continuous flow, thereby solved the technical problem of sample loss.
Drawings
The present invention will be described in more detail hereinafter based on embodiments and with reference to the accompanying drawings.
Fig. 1 is a schematic structural view of an automatic sample feeding and analyzing device for multiple samples according to an embodiment of the present invention;
fig. 2 is a schematic structural diagram of a multi-channel microfluidic switching valve according to an embodiment of the present invention;
fig. 3 is a schematic flow path diagram of a first switching valve according to an embodiment of the present invention;
fig. 4 is a schematic diagram of the distribution of the port of the through valve in the embodiment of the present invention;
fig. 5a is a schematic diagram of a sample loading process in an embodiment of the present invention;
FIG. 5b is a schematic diagram of a sample injection process according to an embodiment of the present invention;
fig. 6a-6f are schematic diagrams of the sample switching process of the present invention.
Reference numerals:
100-a sampling device; 110-multi-channel microfluidic switching valves;
200-a liquid chromatography device; 210-a detection device;
1-micro injection pump; 2-chip; 3-a second switching valve; 4-a first switching valve; 5-way valve; 6-waste liquid bottle; 7-mobile phase storage bottle; 8-an infusion pump; 9-a chromatographic column; 10-a detector; 11-connect out line.
Detailed Description
The present invention will be further explained with reference to the accompanying drawings.
As shown in fig. 1, the utility model provides a many samples carry out autoinjection analytical equipment, including sampling device 100 and liquid chromatography device 200, sampling device 100 includes through connecing out multichannel microfluid diverter valve 110 that pipeline 11 and liquid chromatography device 200 are connected, and wherein, multichannel microfluid diverter valve 110 has two routes at least, and the route is selectively switched on with connecing out pipeline 11 to can select to carry the sample to liquid chromatography device 200 through connecing out pipeline 11 through a certain route.
Specifically, the multi-channel microfluidic switching valve 110 includes a first switching valve 4, the channel includes a first inlet/outlet port provided on the first switching valve 4, an external port g is further provided on the first switching valve 4, one end of the external port g is selectively connected to and communicated with one of the inlet/outlet ports, and the other end of the external port g is connected to the liquid chromatography apparatus 200 through a connecting-out line 11.
The first switching valve 4 is provided with 12 first inlet/outlet ports as an example.
Of the 12 first inlet/outlet ports, 6 are first inlet ports, and the other 6 are first outlet ports. As shown in fig. 3, the 6 first inlets are 1 ', 3', 5 ', 7', 9 'and 11', respectively; the 6 first outlets are 2 ', 4', 6 ', 8', 10 'and 12', respectively. One end of the external interface g can be selectively communicated with any one of the 6 first inlets.
The 6 first outlets can be used as temporary receiving ports for non-detection samples during sampling, namely, a passage communicated with the first inlets 1 'and 2' can be used as a temporary receiving passage for the non-detection samples during sampling, and a passage communicated with the first inlets 3 'and 4' can be used as a temporary receiving passage for the non-detection samples during sampling; the passage of the first inlets 5 'and 6' can be used as a temporary receiving passage of non-detection samples during sampling; the passage of the first inlets 7 'and 8' can be used as a temporary receiving passage of non-detection samples during sampling; the communicating passage of the first inlets 9 'and 10' can be used as a temporary receiving passage for the non-detection sample during sampling, and the communicating passage of the first inlets 11 'and 12' can be used as a temporary receiving passage for the non-detection sample during sampling.
Further, the sampling device 100 further includes a chip 2 for carrying a sample and a second switching valve 3 disposed above the first switching valve 4. The second switching valve 3 is provided with at least two second inlet/outlet ports, the second inlet/outlet ports are arranged in one-to-one correspondence with the first inlet/outlet ports, and the second inlet/outlet ports are used for receiving the sample input by the chip 2 and inputting the sample into the first inlet/outlet ports.
It will be appreciated that the number of second inlet/outlet ports on the second switching valve 3 may be 6 or more, for example 12. Further, the first inlet/outlet ports are provided on the first switching valve 4 at equal intervals in the circumferential direction of the first switching valve 4, and the second inlet/outlet ports are provided on the second switching valve 3 at equal intervals in the circumferential direction of the second switching valve 3. As shown in fig. 2 and 3, the first switching valve 4 is divided into 12 equal parts, wherein each of the first inlet/outlet ports is provided on one of the equal dividing lines. It is understood that, in order to have a one-to-one correspondence of the first switching valves 4 to the second switching valves 3, the second switching valves 3 may also be equally divided by 12, with each of the second inlet/outlet ports being provided on one of the equally divided lines.
The first switching valve 4 is rotatably arranged below the second switching valve 3, and the angle of each rotation of the first switching valve 4 is the included angle between two adjacent first inlet/outlet ports. Since the first inlet/outlet ports are equally spaced, after each rotation of the first switching valve 4, each first inlet/outlet port on the first switching valve can find the corresponding second inlet/outlet port on the second switching valve 3 again.
For example, if the first switching valve 4 has 12 first inlet/outlet ports, the angle of each rotation of the first switching valve 4 is 60 °.
At least one sample channel is arranged in the chip 2, and the sample channel is communicated with a second inlet/outlet corresponding to the sample channel. For example, chip 2 has 6 sample channels, six microchannels, I, ii, iii, iv, v and vi. Six sample channels are arranged on the chip 2, and the same cell line can be cultured in the sample channels, so that the consistency of biological environments is ensured.
As shown in FIG. 2, 6 second inlet/outlet ports a, b, c, d, e and f of the second switching valve 3 are connected to the six microchannels I, II, III, IV, V and VI, respectively. These 6 second inlet/outlet ports are communicated with the 6 first inlet/outlet ports in one-to-one correspondence, respectively, so that the sample in the chip 2 is inputted into the first outlet port.
As shown in fig. 6, the first switching valve 4 is rotated integrally as follows.
As shown in fig. 6a, when the second inlet/outlet a of the second switching valve 3 is loaded with a sample, a path is formed as I-a-1 '-g-11, i.e. the sample enters the second inlet/outlet a after entering the I path, and then enters the first inlet 1' and enters the outlet pipeline 11 through the external port g.
As shown in fig. 6b, the first switching valve 4 is rotated by 60 ° with reference to the second inlet/outlet a on the second switching valve 3 for sample loading, and the formed path is II-b-3 '-g-11, i.e. the sample enters the second inlet/outlet b after entering the path II, enters the first inlet 3' and enters the outlet pipeline 11 through the external port g.
As shown in fig. 6c, when the second inlet/outlet a of the second switching valve 3 is used for sample loading, the first switching valve 4 is rotated by 120 ° (i.e. twice by 60 °), so that a channel III-c-5 '-g-11 is formed, i.e. the sample enters the channel III, enters the second inlet/outlet c, enters the first inlet 5', and enters the outlet pipeline 11 through the external port g.
As shown in fig. 6d, when the second inlet/outlet a of the second switching valve 3 is used for sample loading, the first switching valve 4 is rotated 180 ° (i.e. three times 60 °), and a path is formed as IV-d-7 '-g-11, i.e. the sample enters the second inlet/outlet d after entering the IV path, and then enters the first inlet 7' and then enters the outlet pipeline 11 through the external port g.
As shown in fig. 6e, when the second inlet/outlet a of the second switching valve 3 is used for sample loading, the first switching valve 4 is rotated 240 ° (i.e. rotated four times by 60 °), and a path is formed as V-e-9 '-g-11, i.e. the sample enters the V path, enters the second inlet/outlet e, enters the first inlet 9', and enters the outlet pipeline 11 through the external port g.
As shown in fig. 6f, when the first switching valve 4 is rotated 300 ° (i.e., five times 60 °) based on the second inlet/outlet a on the second switching valve 3 for sample loading, a path VI-f-11 '-g-11 is formed, i.e., the sample enters the second inlet/outlet f after entering the VI path, enters the first inlet 11' and then enters the outlet pipe 11 through the external port g.
Furthermore, the sampling device 100 comprises a micro-syringe pump 1 for delivering the sample into the chip 2. Wherein the micro syringe pump 1 may be a haver syringe pump. The inlets of the sample channels of the chip 2 are respectively connected with the micro-injection pump 1, and the outlets are respectively connected with 6 second inlets. The harvard syringe pump continuously delivers the drug solution with gradient concentration to the 6 micro-channels of the chip 2 at a constant speed to form a uniform pumping condition, so that high parallelism is ensured, and the sample loading barrier caused by evaporation can be avoided by the continuously flowing sample solution.
The operation of the sampling device 100 is described in detail below.
As shown in fig. 2, the second inlet/outlet ports a, b, c, d, e and f of the second switching valve 3 are connected to the outlets of six microchannels I, ii, iii, iv, v and vi, respectively; six first inlets, namely, the first inlets 1 ', 3', 5 ', 7', 9 'and 11' on the first switching valve 4 correspond to six interfaces, namely, ports a, b, c, d, e and f, on the second switching valve 3 in a one-to-one correspondence and are in a communication state, and the sample liquid enters the first inlets 1 ', 3', 5 ', 7', 9 'and 11' of the first switching valve 4 through the second inlets/outlets a, b, c, d, e and f on the second switching valve 3 respectively so as to temporarily receive the non-detection sample liquid during sampling.
The external port g may selectively communicate with the first inlets 1 ', 3', 5 ', 7', 9 ', and 11' of the first switching valve 4 through the internal flow path. For example, the external port g communicates with the first inlet 1 ' of the first switching valve 4 via the internal flow paths 1 ' -g, and the sample liquid in the first inlet 1 ' is outputted to the liquid chromatography apparatus 200 via the external port g.
The analysis of the sample in the I channel connected to the second inlet/outlet a of the second switching valve 3 will be described as an example. As shown in fig. 5, the micro syringe pump 1 provides the power required by the whole flow path, and the sample solution flows into the channel between the chip 2 and the second switching valve 3 from the inlet of the chip 2 and flows through the whole channel by the pumping of the micro syringe pump 1, flows out from the channel outlet, enters the second inlet/outlet a of the second switching valve 3, enters the first inlet 1 'of the first switching valve 4, passes through the internal flow path 1' -g, and is delivered to the liquid chromatography apparatus 200 through the external port g and the outlet line 11.
The liquid chromatography apparatus 200 will be described in detail below. The liquid chromatography apparatus 200 includes a mobile phase storage bottle 7, a detection apparatus 210, and a through valve 5 having at least two ports. Wherein, the mobile phase storage bottle 7 is used for storing the mobile phase; the detection device 210 is used for detecting the sample; a quantitative ring is arranged between two interfaces of the through valve 5, one interface is communicated with an external interface g or a mobile phase storage bottle 7, and the other interface is communicated with a detection device 210 or a waste liquid bottle 6.
As shown in fig. 4, a through valve 5 having 6 ports will be described as an example. The 6 ports of the through valve 5 are A, B, C, D, E and F, respectively. Wherein, be equipped with quantitative ring between interface C and the interface F, can realize quantitative determination.
The on-off between the 6 connections of the through valve 5 can be selectively switched. For example, when sample loading is performed, port B, C, F is in communication with A and ports D and E are in communication. So that the sample is input into the quantitative ring through the external interface g and the output pipeline 11; when sample injection is performed, ports D, C, F and E are in communication, and ports A and B are in communication, so that the mobile phase passes through the quantification ring to bring the sample in the quantification ring into the detection device 210.
Specifically, when sample loading is performed, the port B, C, F is communicated with the port a, the port B is connected to the outlet line 11, and the port a is connected to the waste liquid bottle 6. The sample is conveyed to the interface B through the external interface g and the output pipeline 11, flows through the quantitative ring between the interface C and the interface F, and then flows into the waste liquid bottle 6.
And when the sample loading is finished, sample injection is carried out. And (3) switching the communicated interfaces in the through valve 5 to communicate the interfaces D, C, F and E, so that the mobile phase in the mobile phase storage bottle 7 enters the interface D and is conveyed to the quantitative ring between the interface C and the interface F, and the sample in the quantitative ring is driven to enter the detection device 210 through the interface E for detection.
After the sample introduction is finished, the communicated interface in the through valve 5 is switched again to communicate the interface B, C, F with the interface A, namely, the channel state in the sample loading process is recovered.
In addition, a mobile phase storage bottle 7 is connected to the through valve 5 via an infusion pump 8. The flow path is powered by an infusion pump 8.
The detection device 210 comprises a chromatographic column 9 and a detector 10 connected in sequence. The detector can be replaced, so that the detector can be suitable for detection items such as separation of multi-component samples.
The working process of the multi-sample automatic sample feeding and analyzing device of the utility model is explained in detail below.
In the first step, sample loading is performed.
As shown in fig. 5a, the micro syringe pump 1 provides the power required by the whole flow path, and the sample solution flows into the channel between the chip 2 and the second switching valve 3 from the inlet of the chip 2 and flows through the whole channel by the pumping of the micro syringe pump 1, flows out from the channel outlet, enters the second inlet/outlet a of the second switching valve 3, enters the first inlet 1 'of the first switching valve 4, passes through the internal flow path 1' -g, and is delivered to the liquid chromatography apparatus 200 through the external port g and the outlet line 11.
The port B, C, F of the through valve 5 is communicated with the port A, the port B is connected with the outlet pipeline 11, and the port A is connected with the waste liquid bottle 6. The sample is conveyed to the interface B through the external interface g and the output pipeline 11, flows through the quantitative ring between the interface C and the interface F, and then flows into the waste liquid bottle 6.
And secondly, sample injection is carried out.
As shown in fig. 5b, the connected ports in the through valve 5 are switched to connect the ports D, C, F and E, so that the mobile phase in the mobile phase storage bottle 7 enters the port D and is transported to the quantitative ring between the port C and the port F, and the sample in the quantitative ring is driven to enter the chromatographic column 9 and the detector 10 through the port E for detection.
In the third step, the connected interface in the through valve 5 is switched again to connect the interface B, C, F and a, that is, the access state in the sample loading process is restored.
In the fourth step, the multi-microfluidic switching valve 110 automatically switches to the next sample for detection.
Specifically, the first switching valve 4 is rotated clockwise by 60 °, at this time, the 1 ' -g path is switched to the 3 ' -g path, and the sample liquid in the channel ii flows through the second inlet/outlet port in sequence, passes through the B and 3 ' -g paths, enters the outlet pipeline 11, and is then pumped to the interface B of the through valve 5.
And repeating the loading in the second step and the sample introduction in the third step until the sample detection in the channel II on the chip 2 is finished.
Subsequently, the first switching valve 4 is rotated clockwise by 120 °, 180 °, 240 °, and 300 ° as a whole (based on the state of the first switching valve 4 when detecting the sample in the I channel as a rotation), and accordingly the 1 ' -g path can be flexibly switched to the 5 ' -g, 7 ' -g, 9 ' -g, and 11 ' -g paths to detect the samples in the iii, iv, v, and vi channels on the channel chip 2, respectively. Therefore, the waste of human resources is greatly reduced, and the detection efficiency is greatly improved.
To sum up, the utility model discloses can replace the manual model that trades when multichannel chip and LC-MS used of coupling among the prior art, but advance the appearance through the real-time sample of mechanical control microfluid diverter valve 110 and logical valve 5, can reduce manpower resources's use, reduce the detection cost to also obtain a large amount of real-time data when unmanned on duty, thereby improved efficiency greatly, realize high flux detection.
It should be noted that, in the drawings of the present invention, two components connected by a solid line are communicated with each other.
While the invention has been described with reference to a preferred embodiment, various modifications may be made and equivalents may be substituted for elements thereof without departing from the scope of the invention. In particular, the technical features mentioned in the embodiments can be combined in any way as long as there is no structural conflict. The present invention is not limited to the particular embodiments disclosed herein, but encompasses all technical solutions falling within the scope of the claims.
Claims (8)
1. An automatic sample introduction and analysis device for multiple samples is characterized by comprising a sampling device and a liquid chromatography device, wherein the sampling device comprises a chip for bearing samples and a multi-channel microfluid switching valve connected with the liquid chromatography device through a connecting-out pipeline,
the multi-channel microfluid switching valve is provided with at least two passages, and the passages selectively conduct the chip and the outgoing pipeline;
the multi-channel microfluidic switching valve comprises a first switching valve and a second switching valve disposed above the first switching valve, the passageway comprising a first inlet/outlet port disposed on the first switching valve;
the first switching valve is also provided with an external interface, one end of the external interface is selectively communicated with one first inlet/outlet, and the other end of the external interface is connected with the liquid chromatography device through the outlet pipeline;
the second switching valve is provided with at least two second inlet/outlet ports which are arranged in one-to-one correspondence with the first inlet/outlet ports,
the second inlet/outlet is used for receiving the samples input by the chip and inputting the samples into the first inlet/outlet corresponding to the second inlet/outlet one by one.
2. The apparatus of claim 1, wherein the first inlet/outlet ports are disposed on the first switching valve at equal intervals in a circumferential direction of the first switching valve, and the second inlet/outlet ports are disposed on the second switching valve at equal intervals in a circumferential direction of the second switching valve.
3. The apparatus of claim 2, wherein the first switch valve is rotatably disposed below the second switch valve, and the angle of each rotation of the first switch valve is an included angle between two adjacent first inlet/outlet ports.
4. The device for performing automatic sample injection and analysis on multiple samples according to any one of claims 1 to 3, wherein at least one sample channel is arranged in the chip, and the sample channel is communicated with the second inlet/outlet corresponding to the sample channel.
5. A device for multiple sample autoinjection analysis according to any one of claims 1 to 3, wherein the liquid chromatography device comprises:
a mobile phase storage bottle for storing a mobile phase;
the detection device is used for detecting the sample; and
the device comprises a through valve at least provided with two interfaces, a quantitative ring is arranged between the two interfaces, one interface is communicated with the external interface or the mobile phase storage bottle, and the other interface is communicated with the detection device or the waste liquid bottle.
6. A device for multiple sample autoinjection analysis according to any one of claims 1 to 3, wherein the sampling device further comprises a micro syringe pump for delivering samples into the chip.
7. The device for multiple-sample analysis for automated sample feeding according to claim 5, wherein the mobile phase storage bottle is connected to the valve via an infusion pump.
8. The device for multiple-sample analysis for automated sample introduction according to claim 5, wherein the detection device comprises a chromatographic column and a detector connected in series.
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| CN201922053302.6U CN211426396U (en) | 2019-11-25 | 2019-11-25 | Automatic sample introduction and analysis device for multiple samples |
| PCT/CN2020/108645 WO2021103658A1 (en) | 2019-11-25 | 2020-08-12 | Automatic sample injection and analysis device for multiple samples |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110988228A (en) * | 2019-11-25 | 2020-04-10 | 清华大学 | Automatic sample introduction and analysis device for multiple samples |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110988228A (en) * | 2019-11-25 | 2020-04-10 | 清华大学 | Automatic sample introduction and analysis device for multiple samples |
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