CN111122741A - Multi-liquid-phase chromatography mobile phase switching system and switching method - Google Patents
Multi-liquid-phase chromatography mobile phase switching system and switching method Download PDFInfo
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- CN111122741A CN111122741A CN201911425291.8A CN201911425291A CN111122741A CN 111122741 A CN111122741 A CN 111122741A CN 201911425291 A CN201911425291 A CN 201911425291A CN 111122741 A CN111122741 A CN 111122741A
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- 238000000034 method Methods 0.000 title claims abstract description 12
- 239000012071 phase Substances 0.000 title description 93
- 238000004587 chromatography analysis Methods 0.000 title description 2
- 239000007791 liquid phase Substances 0.000 title description 2
- 238000004811 liquid chromatography Methods 0.000 claims abstract description 21
- 238000002347 injection Methods 0.000 claims abstract description 14
- 239000007924 injection Substances 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000007872 degassing Methods 0.000 claims description 3
- 238000001802 infusion Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000903 blocking effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
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- General Health & Medical Sciences (AREA)
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Abstract
The invention discloses a multi-element liquid chromatography mobile phase switching system and a switching method, wherein the switching system comprises an upper computer, a sample introduction system and a plurality of mobile phase systems, and the sample introduction system comprises a quantifying device and a liquid suction pump; the mobile phase system comprises a sample bottle and a sample introduction pipeline, wherein the sample bottle is filled with a mobile phase, and the mobile phase is sucked into the quantitative device through the sample introduction pipeline; the sample introduction pipeline comprises a first pipeline, a second pipeline and a third pipeline, the third pipeline is connected with the sample bottle, and the first pipeline and the third pipeline are connected with the second pipeline through a flowing phase switching valve; in the multiple mobile phase systems, the second pipeline of the first mobile phase system is connected to the sample injection system, and the second pipelines of the other mobile phase systems are respectively connected to the first pipeline of the previous mobile phase system. The switching system and the switching method can seamlessly switch different mobile phases for transfusion through the switching combination of the mobile phase switching valves, and can adapt to more liquid chromatogram application conditions.
Description
Technical Field
The invention relates to the technical field of liquid chromatography sample introduction, in particular to a multi-element liquid chromatography mobile phase switching system and a multi-element liquid chromatography mobile phase switching method.
Background
Gradient mixing is a common infusion requirement in liquid chromatography (liquid chromatography) infusion processes, which require liquid chromatography pump systems capable of mixing mobile phases (usually up to 4) in variable proportions on-line, and to this end, a widely accepted solution is to have the proportional valve 1 open in proportion before the pump for a period of time corresponding to the concentration ratio of each solvent in the mobile phase. The traditional proportional valve structure is characterized in that a plurality of diaphragm valves respectively control each path of mobile phase switching, when the two paths are switched, two actions of closing an original diaphragm valve and opening a new diaphragm valve are required, mismatching can be caused, and the situations of inaccurate mobile phase switching, unstable infusion and the like are caused. Meanwhile, the traditional quaternary low-pressure chromatographic pump can only support at most four mobile phases, and the structural arrangement of the quaternary low-pressure chromatographic pump limits the development of more mobile phase proportional valves and needs to be improved.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide an expandable multi-liquid chromatography mobile phase switching system and a switching method, and the switching system and the switching method can seamlessly switch different mobile phases for transfusion through the switching combination of a mobile phase switching valve and can adapt to more liquid chromatography application conditions.
The technical scheme adopted by the invention for solving the technical problems is as follows: a multi-element liquid chromatogram flowing phase switching system comprises an upper computer, a sample introduction system and a plurality of flowing phase systems, wherein the sample introduction system comprises a quantifying device and a liquid suction pump, and the liquid suction pump sucks the flowing phases in the flowing phase systems into the quantifying device;
the mobile phase system comprises a sample bottle and a sample introduction pipeline, wherein the sample bottle is filled with a mobile phase, and the mobile phase is sucked into the quantitative device through the sample introduction pipeline;
the sample introduction pipeline comprises a first pipeline, a second pipeline and a third pipeline, the third pipeline is connected with the sample bottle, and the first pipeline and the third pipeline are connected with the second pipeline through a flowing phase switching valve;
in the plurality of mobile phase systems, the second pipeline of the first mobile phase system is connected to the sample introduction system, and the second pipelines of the rest mobile phase systems are respectively connected to the first pipeline of the previous mobile phase system.
Optionally, in the sample introduction pipeline of the mobile phase system, a mobile phase degassing assembly is installed in the third pipeline.
Optionally, in a plurality of the mobile phase systems, the mobile phase switching valves are respectively connected with an upper computer, so that the mobile phase switching valves are respectively controlled by the upper computer.
Optionally, in the plurality of mobile phase systems, the first pipeline of the mobile phase system at the last position is in a normally closed state.
Optionally, a plurality of the mobile phase systems are arranged and distributed in a unilateral binary tree form.
The invention also provides a multi-component liquid chromatography mobile phase switching method, and the mobile phase is switched by the multi-component liquid chromatography mobile phase switching system during sample injection.
Alternatively, when switching the mobile phase, the switching is performed in two steps, wherein,
switching a flowing phase switching valve in a flowing phase system with switching to a third pipeline;
and secondly, switching a flowing phase switching valve in a flowing phase system currently carrying out sample injection to a first pipeline.
By adopting the technical scheme, different mobile phases can be seamlessly switched to carry out infusion through the switching combination of the mobile phase switching valves, each switching only comprises one key action, the stability of the infusion and the precision of gradient switching are ensured, and meanwhile, a single-path mobile phase system can be arbitrarily added and matched, so that the method can adapt to the application condition of complex liquid chromatography.
Drawings
FIG. 1 is a system block diagram of the present invention;
FIG. 2 is a schematic view of a sample injection line of the mobile phase system of the present invention;
FIG. 3 is a schematic arrangement of the mobile phase system of the present invention.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
As shown in fig. 1, the present invention discloses a multi-element liquid chromatography flow phase switching system, which comprises an upper computer, a sample introduction system 1 and a plurality of mobile phase systems 2, wherein the sample introduction system comprises a quantitative device and a liquid absorption pump, when a liquid chromatograph introduces a sample, the liquid absorption pump absorbs the mobile phases in the plurality of mobile phase systems 2 into the quantitative device, and the liquid absorption pump is usually a peristaltic pump.
In the present invention, the mobile phase system 2 includes a sample bottle 201 and a sample injection pipeline, the sample bottle 201 contains mobile phase, and the mobile phase is sucked into the quantitative device through the sample injection pipeline. As shown in fig. 2, the sample injection pipeline includes a first pipeline 202, a second pipeline 203, and a third pipeline 204, the third pipeline 204 is connected to the sample bottle 201, the first pipeline 202 and the third pipeline 204 are connected to the second pipeline 203 through a flow phase switching valve 205, and the flow phase switching valves 205 are respectively connected to an upper computer, so that the flow phase switching valves 205 are respectively controlled by the upper computer. A mobile phase degassing assembly 206 is installed in the third pipeline 204 to ensure that no gas is separated out during low-pressure mixing, thereby improving the precision of the mobile phase.
In the multiple mobile phase systems 2, the second pipeline 203 of the first mobile phase system 2 is connected to the sample injection system 1, the second pipelines 203 of the remaining mobile phase systems 2 are respectively connected to the first pipeline 202 of the previous mobile phase system 2, and the first pipeline 202 of the mobile phase system 2 located at the last position is in a normally closed state.
In the present invention, a plurality of mobile phase systems 2 are arranged and distributed in a one-sided binary tree form, as shown in fig. 3.
When the mobile phase switching system of the multi-component liquid chromatography is used for switching the mobile phase, the switching is carried out in two steps, wherein in the first step, a mobile phase switching valve in the mobile phase system with the switching is switched to a third pipeline; and secondly, switching a flowing phase switching valve in a flowing phase system currently carrying out sample injection to a first pipeline.
The present invention will be described in detail below by taking a quaternary gradient as an example.
As shown in fig. 3, the mobile phases and the switching units of the quaternary gradient mobile phase system are arranged in a one-sided binary tree.
In the present embodiment, the default phase switching valve 205 is switched to the left to use the current mobile phase output, that is, in the mobile phase system, the phase switching valve 205 communicates with the second pipeline 203 and the third pipeline 204, which are represented by binary 0, the phase switching valve 205 is switched to the right to use the first pipeline 202 to output, that is, the phase switching valve 205 communicates with the first pipeline 202 and the second pipeline 203, which are represented by binary 1, any state of the phase switching valve 205 is represented by x, and states of the four phase switching valves 205 are represented by four-digit binary.
Before the sample injection system 1 starts to work, all the flow phase switching valves 205 are switched to the first pipeline 202 input state, namely 1111 state, and the flow path is in a blocking state.
Before the sample injection system 1 starts to work, the corresponding flow phase switching valve 205 is opened, and the input switching valves corresponding to the flow phase A, B, C, D are respectively 0xxx, 10xx, 110x and 1110.
When the gradient switching is performed, the upper computer changes the state of the flow phase switching valve 205 in accordance with time according to the ratio of each flow phase.
When the sample injection state is switched from the mobile phase positioned at the rear row to the mobile phase positioned at the front row, the sample injection state can be directly switched by the switching valve corresponding to the flow at the front row to change. For example, in the case of the D → C, D → B, D → A switch, the state change of the phase-switching valve 205 is: 1110 → 1100, 1110 → 1010, 1110 → 0110.
In the above description, → indicates switching, and in the following description, → indicates switching similarly.
In order to reduce the number of actions of the phase switching valve 205 at the key switching point, the auxiliary switching may be performed before the key switching point, so as to ensure that only one phase switching valve 205 is operated when the key switching point is switched, thereby improving the gradient switching accuracy. For example, when the mobile phase output is a and the switching valve state is 0110, the mobile phase switching valve 205 needs to output B, C by advancing the assist switch, with the corresponding switching steps being 0110 → 0010 → 1010, 0110 → 0000 → 1000. The auxiliary switching step of the first step does not change the output of the original mobile phase, and the key switching step of the second step changes the output of the mobile phase.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Other technical features than those described in the specification are known to those skilled in the art, and are not described herein in detail in order to highlight the innovative features of the present invention.
Claims (7)
1. A multi-element liquid chromatogram flowing phase switching system is characterized by comprising an upper computer, a sample introduction system and a plurality of flowing phase systems, wherein the sample introduction system comprises a quantifying device and a liquid suction pump, and the liquid suction pump sucks the flowing phases in the flowing phase systems into the quantifying device;
the mobile phase system comprises a sample bottle and a sample introduction pipeline, wherein the sample bottle is filled with a mobile phase, and the mobile phase is sucked into the quantitative device through the sample introduction pipeline;
the sample introduction pipeline comprises a first pipeline, a second pipeline and a third pipeline, the third pipeline is connected with the sample bottle, and the first pipeline and the third pipeline are connected with the second pipeline through a flowing phase switching valve;
in the plurality of mobile phase systems, the second pipeline of the first mobile phase system is connected to the sample introduction system, and the second pipelines of the rest mobile phase systems are respectively connected to the first pipeline of the previous mobile phase system.
2. The multiple liquid chromatography flow phase switching system of claim 1, wherein a mobile phase degassing assembly is installed in a third line in a sample line of the mobile phase system.
3. The multiple component liquid chromatography phase flow switching system of claim 2, wherein in a plurality of said phase flow systems, said phase flow switching valves are each connected to an upper computer such that a plurality of said phase flow switching valves are each controlled by the upper computer.
4. The multiple liquid chromatography flow phase switching system of claim 3, wherein, among the plurality of mobile phase systems, a first line of the mobile phase system located at the last position is in a normally closed state.
5. The multiple-component liquid chromatography flow phase switching system of claim 4, wherein a plurality of the flow phase systems are arranged and distributed in a one-sided binary tree.
6. A multi-component liquid chromatography mobile phase switching method is characterized in that the mobile phase is switched by the multi-component liquid chromatography mobile phase switching system as claimed in any one of claims 1-5 when the sample is fed.
7. The multiple liquid chromatography flow phase switching method of claim 6, wherein the switching is performed in two steps in switching the mobile phase, wherein,
switching a flowing phase switching valve in a flowing phase system with switching to a third pipeline;
and secondly, switching a flowing phase switching valve in a flowing phase system currently carrying out sample injection to a first pipeline.
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| CN201911425291.8A CN111122741A (en) | 2019-12-31 | 2019-12-31 | Multi-liquid-phase chromatography mobile phase switching system and switching method |
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| CN201911425291.8A CN111122741A (en) | 2019-12-31 | 2019-12-31 | Multi-liquid-phase chromatography mobile phase switching system and switching method |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240936A (en) * | 1998-06-19 | 2000-01-12 | 株式会社岛津制作所 | Liquid chromatograph |
| JP2002168842A (en) * | 2000-11-30 | 2002-06-14 | Hitachi Ltd | Liquid chromatograph and analyzing method using the same |
| CN1468369A (en) * | 2000-10-04 | 2004-01-14 | Air samplers | |
| US20090220385A1 (en) * | 2005-11-01 | 2009-09-03 | Brown Jeffrey A | Liquid dispensing for high-throughput experimentation |
| US20130233060A1 (en) * | 2012-03-08 | 2013-09-12 | Shimadzu Corporation | Solvent delivery device and liquid chromatograph |
| CN104634912A (en) * | 2015-01-20 | 2015-05-20 | 大连依利特分析仪器有限公司 | Liquid phase chromatographic sample manager |
| CN109283138A (en) * | 2018-09-30 | 2019-01-29 | 宁波万泽微测环境科技股份有限公司 | A kind of quantitative sample injection system |
-
2019
- 2019-12-31 CN CN201911425291.8A patent/CN111122741A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240936A (en) * | 1998-06-19 | 2000-01-12 | 株式会社岛津制作所 | Liquid chromatograph |
| CN1468369A (en) * | 2000-10-04 | 2004-01-14 | Air samplers | |
| JP2002168842A (en) * | 2000-11-30 | 2002-06-14 | Hitachi Ltd | Liquid chromatograph and analyzing method using the same |
| US20090220385A1 (en) * | 2005-11-01 | 2009-09-03 | Brown Jeffrey A | Liquid dispensing for high-throughput experimentation |
| US20130233060A1 (en) * | 2012-03-08 | 2013-09-12 | Shimadzu Corporation | Solvent delivery device and liquid chromatograph |
| CN104634912A (en) * | 2015-01-20 | 2015-05-20 | 大连依利特分析仪器有限公司 | Liquid phase chromatographic sample manager |
| CN109283138A (en) * | 2018-09-30 | 2019-01-29 | 宁波万泽微测环境科技股份有限公司 | A kind of quantitative sample injection system |
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