CN108490107A - A kind of liquid chromatograph and working method for complex sample multi-cycle separation - Google Patents
A kind of liquid chromatograph and working method for complex sample multi-cycle separation Download PDFInfo
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- CN108490107A CN108490107A CN201810194006.5A CN201810194006A CN108490107A CN 108490107 A CN108490107 A CN 108490107A CN 201810194006 A CN201810194006 A CN 201810194006A CN 108490107 A CN108490107 A CN 108490107A
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The present invention relates to a kind of liquid chromatographs and working method for complex sample multi-cycle separation, including liquid phase separation access, liquid phase separation access end is connected with several one or six direction changeover valves and intermediate valve group in turn, the intermediate valve group is connect with the head end of liquid phase separation access, constitute multi-cycle separation circuit, it is connected with transfer tube between the intermediate valve group and liquid phase separation access, the intermediate valve group is connected to the solvent bottle for containing mobile phase, collecting pipe is set on one or six direction changeover valve, it will be in the collecting pipe access multi-cycle separation circuit of different six direction changeover valves, it can receive different cycle peaks, realize the separation of complex sample.
Description
Technical field
The present invention relates to separation equipment technical fields, and in particular to a kind of liquid chromatogram for complex sample multi-cycle separation
Instrument and working method.
Background technology
High performance liquid chromatography is the mainstream of current analysis and separation science field, is a chromatographic important branch, with
Liquid is mobile phase, using high pressure transfusion system, by the mixed solvent of single solvent or different proportion with opposed polarity, is delayed
The mobile phases such as fliud flushing are pumped into the chromatographic column equipped with stationary phase, after each ingredient is detached in column, are detected into detector, from
And realize the analysis to sample.This method has become important in the ambits such as chemistry, medicine, industry, agronomy, commodity inspection and method inspection
Analytical Separation.The fast development in simultaneous chromatographic column filler field, column effect and separative efficiency have obtained greatly
It is promoted, has separative efficiency high, selectivity is good, and detection sensitivity is high, operation automation, and the advantages such as have a wide range of application.
Although high performance liquid chromatography has many advantages in separation process, in the analysis and separation of complex sample
In：Such as Structures of Natural Products complexity, once analysis and separation are difficult to realize many in natural products to conventional high performance liquid chromatography
Compound：Analysis including the very similar compound of enantiomer, diastereomer, isomers or the similar retention time of structure and
Separation, it is difficult in aforementioned manners from complicated blending ingredients primary directly analysis with it is isolated.Above-mentioned sample is needed
When carrying out two dimension/Multidimensional HPLC analysis and separation, secondary analysis and separation, sample is picked out by pipeline, is connected to
Two-dimensional highly effective liquid phase chromatographic or chromatographic column internal solvent carry out secondary separation after rebalancing, and the instrument quantity needed is more,
Operating process is complicated, and for the inferior separating effect of multiple complex samples.
Invention content
In order to overcome above-mentioned technological deficiency, the present invention provides a kind of liquid chromatograies for complex sample multi-cycle separation
The multi-cycle separation of multicomponent complex sample may be implemented in instrument, and to achieve the goals above, the present invention adopts the following technical scheme that：
A kind of liquid chromatograph for complex sample multi-cycle separation, including liquid phase separation access, the liquid phase separation are logical
Road end is connected with several one or six direction changeover valves and intermediate valve group, the head end of the intermediate valve group and liquid phase separation access in turn
Connection constitutes multi-cycle separation circuit, transfer tube, the intermediate valve group is connected between the intermediate valve group and liquid phase separation access
It being connected to the solvent bottle for containing mobile phase, transfer tube can drive mobile phase to enter liquid phase separation access through intermediate valve group, and described the
Collecting pipe is set between one or six connectors of direction changeover valve two, and two connectors of disconnected collecting pipe are as sample inlet and sample
Product export, and the sample export of two neighboring six direction changeover valve is connected to sample inlet, and connection is arranged between remaining two connectors
Pipe can receive in the collecting pipe access multi-cycle separation circuit of different six direction changeover valves different cycle peaks, realize complex sample
Separation.
Further, the intermediate valve group is the two or six direction changeover valve, one connection of the two or six direction changeover valve
Mouth is connected to the one or six direction changeover valve as the connector of sample export, and a connector connects liquid phase separation by transfer tube and leads to
Road, a connector are connected to as sample collection mouth, a connector with the solvent bottle for containing mobile phase, remaining two connectors
Between connecting tube is set.
Further, the intermediate valve group is sequentially connected first triple valve and the second triple valve, first threeway
One connector of valve is connected to the sample export of six direction changeover valves, and a connector is as sample collection mouth, a remaining connection
Mouth is connected to a connector of the second triple valve, another connector of second triple valve connects liquid phase by transfer tube
Access is detached, one connector connection of residue of second triple valve contains the solvent bottle of mobile phase.
Further, the liquid phase separation access includes sequentially connected sampling device, liquid-phase chromatographic column and detector, institute
It states sampling device and enters separation access for sample, liquid-phase chromatographic column detaches sample, and detector is used to carry out sample
Detection.
Further, the sampling device is six-way injection valve.
The invention also discloses a kind of working method of the liquid chromatograph for complex sample multi-cycle separation, including it is following
Step：
Step 1：One or six direction changeover valve is switched to the connector being connect with collecting pipe as the connector of sample inlet
Transfer tube is connect, in the effect of transfer tube by the state of connection with the connector as sample inlet of the one or six direction changeover valve
Under, it is pumped into mobile phase, mobile phase flows successively through multiple one or six direction changeover valves, is flowed out from intermediate valve group, full of stream in collecting pipe
Dynamic phase.
Step 2：Multiple first six-way valves are switched to the connector as sample inlet and the connection as sample export
The state of mouth connection, transfer tube and six-way injection valve and intermediate valve group connect, under the action of transfer tube, the flowing in solvent bottle
Entire multi-cycle separation circuit is mutually flowed into, entire multi-cycle separation circuit is finally filled, until reaching fluid dynamic equilibrium.
Step 3：After reaching fluid dynamic equilibrium, sample injects six-way injection valve after flowing phased soln, carries out liquid phase
Chromatographic isolation.
Further, in the step 3, for the high sample of separating degree, directly the sample of intermediate valve group outflow is carried out
It collects, realizes the one-dimensional liquid chromatogram separation of sample.
Further, in the step 3, for the sample that one-dimensional liquid chromatogram is difficult to detach, intermediate valve group, detection are adjusted
The sample of device outflow is again introduced into liquid-phase chromatographic column through intermediate valve group and is detached, and realizes the multi-cycle separation of sample, detaches situation
It is detected in real time using detector, after the completion of separation, adjusts intermediate valve group, solvent bottle is made to pass through intermediate valve group and transfer tube and liquid phase
Access connection is detached, next use is facilitated.
Further, in the step 3, the separation for multicomponent complex sample, by different one or six direction changeover valves
Collecting pipe accesses in multi-cycle separation circuit, can receive different cycle peaks, realizes the multi-cycle separation of complex sample, separation situation profit
It is detected in real time with detector, after the completion of separation, adjusts intermediate valve group, so that solvent bottle is passed through and follow intermediate valve group and transfer tube and liquid phase
Access is detached, next use is facilitated.
Beneficial effects of the present invention：
1. the present invention liquid chromatograph, with intermediate valve group, it can be achieved that sample multi-cycle separation, good separating effect, and
Easy to operate, the instrument quantity used is few.
2. the present invention liquid phase stream chromatograph, separated sample can quickly be collected.
3. the liquid chromatograph of the present invention is provided with collecting pipe, different one or six direction changeover valves on the one or six direction changeover valve
Collecting pipe access multi-cycle separation circuit in, can receive different cycle peaks, realize the separation and collection of multicomponent complex sample.
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not constitute the restriction to the application for explaining the application.
Fig. 1 is 1 solvent balance schematic diagram of the embodiment of the present invention；
Fig. 2 is 1 liquid chromatogram separation schematic diagrames of the embodiment of the present invention；
Fig. 3 is 1 multi-cycle separation schematic diagram of the embodiment of the present invention；
Fig. 4 is 1 multicomponent complex sample of embodiment of the present invention access collecting pipe schematic diagram；
Fig. 5 is 1 multicomponent complex sample multi-cycle separation schematic diagram of the embodiment of the present invention；
Fig. 6 is 2 solvent balance schematic diagram of the embodiment of the present invention；
Fig. 7 is 2 liquid chromatogram separation schematic diagrames of the embodiment of the present invention；
Fig. 8 is 2 multi-cycle separation schematic diagram of the embodiment of the present invention；
Fig. 9 is 2 multicomponent complex sample of embodiment of the present invention access collecting pipe schematic diagram；
Figure 10 is 2 multicomponent complex sample multi-cycle separation schematic diagram of the embodiment of the present invention；
Wherein：1. the one or six direction changeover valve, 2. transfer tubes, 3. solvent bottles, 4. collecting pipes, 5. connecting tubes, 6. the 2nd 6 is logical
Switching valve, 7. sampling devices, 8. liquid-phase chromatographic columns, 9. detectors, 10. first triple valves, 11. second triple valves.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
As background technology is introduced, existing liquid chromatograph cannot achieve the multi-cycle separation of sample, and for
The inferior separating effect of multicomponent complex sample, in view of the above-mentioned problems, present applicant proposes one kind being used for complex sample multi-cycle separation
Liquid chromatograph.
In a kind of exemplary embodiments 1 of the application, a kind of liquid chromatograph for complex sample multi-cycle separation, including liquid
Be separated access, and liquid phase separation access end is connected with the one or six direction changeover valve 1 and intermediate valve group, the intermediate valve in turn
Group is connect with the head end of liquid phase separation access, is constituted multi-cycle separation circuit, is connected between the intermediate valve group and liquid phase separation access
It is connected to transfer tube 2, the intermediate valve group is connected to the solvent bottle 3 for containing mobile phase, and transfer tube can drive mobile phase through intermediate valve
Group enters liquid phase separation access, and collecting pipe 4, connector are arranged between the one or the six direction changeover valve connector I and connector II
III is used as sample inlet, connector IV to be used as sample export, connecting tube 5 is arranged between connector V and connector VI, by first
In the collecting pipe access multi-cycle separation circuit of six direction changeover valves, the separation of special component in sample is realized.
The intermediate valve group is the two or six direction changeover valve 6, the connector II and first of the two or six direction changeover valve
Six direction changeover valves are connected to as the connector IV of sample export, and connector I connects liquid phase separation access, connector by transfer tube
V is used as sample collection mouth, connector VI to be connected to the solvent bottle for containing mobile phase, be arranged between connector III and connector IV
Connecting tube.
The liquid phase separation access includes sequentially connected sampling device 7, liquid-phase chromatographic column 8 and detector 9, the sample introduction
Device enters separation access for sample, and liquid-phase chromatographic column detaches sample, and detector is for being detected sample, institute
It is six-way injection valve to state sampling device.
The invention also discloses a kind of working method of the liquid chromatograph for complex sample multi-cycle separation, including it is following
Step：
Step 1：One or six direction changeover valve is switched to the state that connector III is connected to connector II, by transfer tube and the
The connector III of one or six direction changeover valves connects, and under the action of transfer tube, is pumped into mobile phase, it is logical that mobile phase flows successively through the one or six
Switching valve flows out from the connector V of cycle six-way valve, mobile phase is full of in collecting pipe.
Specific mobile phase flows to III → connector of connector, the II → connector I → company for being in the one or six direction changeover valve
VI → connecting tube of interface → V → connector of connector IV passes through the connection of cycle six-way valve after the outflow of the one or six direction changeover valve
Mouth II enters cycle six-way valve, and specifically flow direction is in the two or six direction changeover valve：II → connector of connector, III → connecting tube →
IV → connector of connector V.
Step 2：As shown in Figure 1, multiple first six-way valves are switched to the state that connector III is connected to connector IV, drive
Dynamic pump is connect with the connector I of six-way injection valve and the two or six direction changeover valve, under the action of transfer tube, the flowing in solvent bottle
Entire multi-cycle separation circuit is mutually flowed into, entire multi-cycle separation circuit is finally filled, until reaching fluid dynamic equilibrium.
Mobile phase it is specific flow direction be：The direction changeover valve (VI → I) of solvent bottle → the two or six → six-way injection valve → liquid phase color
Compose direction changeover valve (III → IV) → the two or six direction changeover valve (II → III → IV → V) of column → detector → the one or six
Step 3：After reaching fluid dynamic equilibrium, sample injects six-way injection valve after flowing phased soln, carries out liquid phase
Chromatographic isolation.
As shown in Fig. 2, as shown in Fig. 2, for the high sample of separating degree, the direct connector V to the two or six direction changeover valve
The sample of outflow is collected, and realizes the one-dimensional liquid chromatogram separation of sample.
As shown in figure 3, for the sample that one-dimensional liquid chromatogram is difficult to detach, the two or six direction changeover valve is adjusted, makes the two or six
The connector II of direction changeover valve is connected to connector I, and the sample of detector outflow is through the one or six direction changeover valve, the two or six logical switching
Valve is again introduced into liquid-phase chromatographic column and is detached, and realizes that the multi-cycle separation of sample, separation situation are detected in real time using detector, point
From after the completion, the connector II of the two or six direction changeover valve of adjustment is connected to connector III, and solvent bottle is made to pass through the two or six logical switching
Valve and transfer tube are connect with liquid phase separation access, facilitate next use.
As illustrated in figures 4-5, for the separation of multicomponent complex sample, the collecting pipe of the one or six direction changeover valve is accessed into cycle
In separating circuit, the cycle peak of special component is can receive, realizes the multi-cycle separation of complex sample, specifically, switching six by first
The connector III of port valve is connected to connector II, sample through connector III, connector II enter collecting pipe, from collecting pipe flow out into
Enter the two or six direction changeover valve, adjust the two or six direction changeover valve, connect circulation loop, then carries out multi-cycle separation, separation situation profit
It is detected in real time with detector, after the completion of separation, adjusts the two or six direction changeover valve, solvent bottle is made to pass through the two or six direction changeover valve and drive
Dynamic pump is connect with liquid phase separation access, adjusts the one or six direction changeover valve, collecting pipe is not accessed to multi-cycle separation circuit, facilitates next time
It uses.
Can multiple one or six direction changeover valves be set according to sample situation, the collecting pipe of different one or six direction changeover valves is accessed
In multi-cycle separation circuit, the cycle peak of heterogeneity is can receive, realizes the separation of multicomponent complex sample.
Because sample composition to be collected can not necessarily be completely filled with collecting pipe, when switching over separation, bubble meeting
Into adverse current chromatogram, to influence to detach, so being pre-filled with mobile phase in collecting pipe, elimination bubble ensure that.
In another embodiment of the application, as illustrated in figures 6-10, intermediate valve group uses sequentially connected first triple valve
10 and second triple valve 11, the connector as sample export of first triple valve one connector I and six direction changeover valves
IV connection, a connector III are used as sample collection mouth, a connector I company of a remaining connector II and the second triple valve
Logical, another connector II of second triple valve connects liquid phase separation access by transfer tube, second triple valve
A remaining connector III connection contains the solvent bottle of mobile phase.
Application method is roughly the same with embodiment, difference lies in when, solvent balance, connection of the mobile phase from the first triple valve
Mouth III flows out, and when carrying out one-dimensional liquid phase separation, the connector I of the first triple valve is connected to connector III, utilizes the first threeway
The connector III of valve carries out sample collection, and when carrying out multi-cycle separation, the connector I of the second triple valve is connected to connector III,
Connect multi-cycle separation circuit.
Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not protects model to the present invention
The limitation enclosed, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not
Need to make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (9)
1. a kind of liquid chromatograph for complex sample multi-cycle separation, which is characterized in that including liquid phase separation access, the liquid
Phase separation access end is connected with several one or six direction changeover valves in turn and intermediate valve group, the intermediate valve group are logical with liquid phase separation
The head end on road connects, and constitutes multi-cycle separation circuit, transfer tube is connected between the intermediate valve group and liquid phase separation access, described
Intermediate valve group with contain mobile phase solvent bottle be connected to, transfer tube can drive mobile phase through intermediate valve group enter liquid phase separation lead to
Collecting pipe is arranged between described one or six direction changeover valve, two connectors in road, and two connectors of disconnected collecting pipe are as sample
The sample export of product import and sample export, two neighboring six direction changeover valve is connected to sample inlet, remaining two connectors it
Between connecting tube is set, by the collecting pipe access multi-cycle separation circuit of different six direction changeover valves, can receive different cycle peaks, it is real
The separation of existing complex sample.
2. a kind of liquid chromatograph for complex sample multi-cycle separation as described in claim 1, which is characterized in that in described
Between valve group be the two or six direction changeover valve, described two or six direction changeover valve, one connector and the one or six direction changeover valve are as sample
The connector connection of product outlet, a connector connect liquid phase separation access by transfer tube, and a connector is received as sample
Ji Kou, a connector are connected to the solvent bottle for containing mobile phase, and connecting tube is arranged between remaining two connectors.
3. a kind of liquid chromatograph for complex sample multi-cycle separation as described in claim 1, which is characterized in that in described
Between valve group be sequentially connected first triple valve and the second triple valve, first triple valve, one connector and six direction changeover valves
Sample export connection, a connector is used as sample collection mouth, and one of residue one connector and the second triple valve connect
Mouth connection, another connector of second triple valve pass through transfer tube and connect liquid phase separation access, second triple valve
Residue one connector connection contain the solvent bottle of mobile phase.
4. a kind of liquid chromatograph for complex sample multi-cycle separation as described in claim 1, which is characterized in that the liquid
Phase separation access includes sequentially connected sampling device, liquid-phase chromatographic column and detector, and the sampling device enters for sample
Access is detached, liquid-phase chromatographic column detaches sample, and detector is for being detected sample.
5. a kind of liquid chromatograph for complex sample multi-cycle separation as claimed in claim 4, which is characterized in that it is described into
Sampling device is six-way injection valve.
6. the working method of the liquid chromatograph as described in any one in claim 1-5 for complex sample multi-cycle separation,
It is characterized in that, includes the following steps：
Step 1：One or six direction changeover valve is switched to the connector connection being connect with collecting pipe as the connector of sample inlet
State, transfer tube is connect with the connector as sample inlet of the one or six direction changeover valve, under the action of transfer tube, pump
Enter mobile phase, mobile phase flows successively through multiple one or six direction changeover valves, is flowed out from intermediate valve group, and mobile phase is full of in collecting pipe；
Step 2：Multiple first six-way valves are switched to the connector as sample inlet with the connector as sample export to connect
Logical state, transfer tube and six-way injection valve and intermediate valve group connection, under the action of transfer tube, the mobile phase stream in solvent bottle
Enter entire multi-cycle separation circuit, finally fill entire multi-cycle separation circuit, until reaching fluid dynamic equilibrium；
Step 3：After reaching fluid dynamic equilibrium, sample injects six-way injection valve after flowing phased soln, carries out liquid chromatogram
Separation.
7. the working method for the liquid chromatograph of complex sample multi-cycle separation as claimed in claim 6, which is characterized in that
In the step 3, for the high sample of separating degree, directly the sample of intermediate valve group outflow is collected, realizes the one of sample
Tie up liquid chromatogram separation.
8. the working method for the liquid chromatograph of complex sample multi-cycle separation as claimed in claim 6, which is characterized in that
In the step 3, for the sample that one-dimensional liquid chromatogram is difficult to detach, intermediate valve group is adjusted, in the sample warp that detector flows out
Between valve group be again introduced into liquid-phase chromatographic column and detached, realize that the multi-cycle separation of sample, separation situation are examined in real time using detector
It surveys, after the completion of separation, adjusts intermediate valve group, solvent bottle is made to be connect with liquid phase separation access by intermediate valve group and transfer tube.
9. the working method for the liquid chromatograph of complex sample multi-cycle separation as claimed in claim 6, which is characterized in that
In the step 3, the collecting pipe of different one or six direction changeover valves is accessed multi-cycle separation by the separation for multicomponent complex sample
In circuit, different cycle peaks is can receive, realizes that the multi-cycle separation of complex sample, separation situation are detected in real time using detector,
After the completion of separation, intermediate valve group is adjusted, so that solvent bottle is passed through and follows intermediate valve group and transfer tube and connect with liquid phase separation access.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810194006.5A CN108490107A (en) | 2018-03-09 | 2018-03-09 | A kind of liquid chromatograph and working method for complex sample multi-cycle separation |
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| CN201810194006.5A CN108490107A (en) | 2018-03-09 | 2018-03-09 | A kind of liquid chromatograph and working method for complex sample multi-cycle separation |
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| CN116203167A (en) * | 2023-04-27 | 2023-06-02 | 广东省农业科学院蚕业与农产品加工研究所 | Circulating type multidimensional liquid chromatographic separation system and application thereof |
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