CN221238744U - Double-channel on-line enrichment and analysis system - Google Patents

Double-channel on-line enrichment and analysis system Download PDF

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CN221238744U
CN221238744U CN202322773363.6U CN202322773363U CN221238744U CN 221238744 U CN221238744 U CN 221238744U CN 202322773363 U CN202322773363 U CN 202322773363U CN 221238744 U CN221238744 U CN 221238744U
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channel
analysis
pump
enrichment
control valve
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陈应庄
周聪
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Hunan Lingfeng Instrument Equipment Co ltd
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Hunan Lingfeng Instrument Equipment Co ltd
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Abstract

The utility model discloses a double-channel online enrichment analysis system, which comprises: the sample injector alternately injects sample to the first processing channel and the second processing channel, and then alternately introduces the target objects enriched and separated by the first processing channel and the second processing channel into the mass spectrum detector for analysis; the first treatment channel and the second treatment channel respectively comprise a trapping column, a separation column, a control valve and a pump, and the trapping column is switched to an analysis stage after balancing, sample loading and enrichment are completed through the linkage of the control valve and the pump. The utility model has the advantages of strong enrichment capability, capability of effectively overcoming the incompatible effect of solvents, high automation degree, capability of greatly improving the treatment efficiency and the like.

Description

Double-channel on-line enrichment and analysis system
Technical Field
The utility model mainly relates to the technical field of chemical analysis equipment, in particular to a two-channel on-line enrichment and analysis system which is suitable for various chemical analysis fields, such as clinical analysis, environmental analysis and the like.
Background
High throughput analysis of the index compounds in large quantities of samples is often required in clinical, environmental, etc. fields. Because of the complex background of these samples and the generally low content of the target, sample pretreatment such as liquid-liquid extraction, solid-phase extraction, enrichment concentration, etc. is required.
The sample analysis process adopts an off-line analysis mode conventionally, and the traditional off-line method has the problems of error introduced by human intervention, long time, complex process and the like.
In the prior art, practitioners have proposed some online analysis device products, which can be used to realize multi-channel high-throughput continuous direct analysis, and also can be used to realize online enrichment analysis of samples, but the enrichment analysis is more suitable for solvent compatible sample analysis, that is, the sample solvent needs to be a weak elution solvent of a trapping column (here, "weak elution solvent" refers to the polarity of the trapping column, and the same applies below). For example, the trapping column is a common reverse phase column, the sample solvent is preferably weak eluent water, and is preferably not strong eluting organic solvent, especially when the target object needs to be enriched by a large-volume sample injection, the large-volume organic solvent can not be trapped effectively by the reverse phase column due to the incompatibility of the solvent.
In other words, the existing system samples and enriches a large-volume sample, which cannot simultaneously adapt to a sample dissolved by weak eluting solvent water and a sample dissolved by strong eluting organic solvent, and has poor compatibility. In addition, in the desorption process of the sample from the trapping column, the prior art solutions are slow desorption along with the gradient, which can lead to the reduction of the separation efficiency.
Disclosure of utility model
The utility model aims to solve the technical problems that: aiming at the technical problems existing in the prior art, the utility model provides the double-channel online enrichment analysis system which has strong enrichment capacity, can effectively overcome the incompatible effect of solvents and has high automation degree.
Furthermore, the utility model can solve the problem of poor treatment efficiency of separation, analysis and the like.
In order to solve the technical problems, the utility model adopts the following technical scheme:
A dual channel online enrichment analysis system, comprising: the sample injector alternately injects sample to the first processing channel and the second processing channel, and then alternately introduces the target object separated by the first processing channel and the second processing channel into the mass spectrum detector for analysis; the first treatment channel and the second treatment channel respectively comprise a channel trapping column, a separation column, a control valve and a pump, and the trapping column is switched to an analysis stage after balancing, sample loading and enrichment are completed through the control valve.
As a further improvement of the process of the utility model: and a balance pump is arranged between the first processing channel and the second processing channel and is used for completing a pre-balance process before analysis of the two analysis columns in the first processing channel and the second processing channel.
As a further improvement of the process of the utility model: and the first processing channel and the second processing channel respectively undergo three stages of system balance, sample injection + enrichment and analysis, and separated target objects are alternately introduced into a mass spectrum for further analysis.
As a further improvement of the process of the utility model: the flow paths of the first and second process channels are isolated from each other at any stage.
As a further improvement of the process of the utility model: the first treatment channel comprises a pump A, a pump B, a first treatment channel trapping column TC1, a first separation column SC1 and a second control valve V2; the pump A and the pump B form a gradient pump in the first treatment channel, and the second control valve V2 is used for controlling the trapping column on the first treatment channel to complete balance-loading-enrichment and then switch to an analysis stage.
As a further improvement of the process of the utility model: the second treatment channel comprises a pump C, a pump D, a second treatment channel trapping column TC2, a second separation column SC2 and a third control valve V3; the pump C and the pump D form a gradient pump in the second treatment channel, and the third control valve V3 is used for controlling the trapping column on the second treatment channel to switch to an analysis stage after balance-loading-enrichment is completed.
As a further improvement of the process of the utility model: the device further comprises a first control valve V1, wherein the first control valve V1 is used for realizing alternating sample injection of the sample injector to the first processing channel and the second processing channel.
As a further improvement of the process of the utility model: a fourth control valve V4 is also included, said fourth control valve V4 being used to realize a pre-balancing of the balance pump before the separation of the two analytical columns, alternately connected to the analytical columns of the first and second process channels.
As a further improvement of the process of the utility model: and a fifth control valve V5, wherein the fifth control valve V5 is used for alternately introducing the target objects separated by the first processing channel and the second processing channel into the mass spectrum detector for analysis.
As a further improvement of the process of the utility model: two ten-way valves are adopted, wherein one ten-way valve is used for controlling the trapping column on the first treatment channel to complete balance-loading-enrichment and then switching to an analysis stage, and the other ten-way valve is used for controlling the trapping column on the second treatment channel to complete balance-loading-enrichment and then switching to the analysis stage; the other ten-way valve is used for realizing the pre-balancing before the balance pump is alternately connected to the analysis columns of the first processing channel and the second processing channel and separates the two analysis columns, and is used for alternately introducing the target objects separated by the first processing channel and the second processing channel into the mass spectrum detector for analysis.
Compared with the prior art, the utility model has the advantages that:
1. The dual-channel online enrichment analysis system has strong enrichment capacity, can effectively overcome the incompatible effect of solvents and has high automation degree, and the trapping column can be switched to an analysis stage after balancing, loading and enrichment through the linkage of the control valve and the pump by alternately feeding samples through the first treatment channel and the second treatment channel.
2. The two-channel on-line enrichment analysis system can greatly improve the treatment efficiency, and the flow path structure can enable the sample to eliminate the solvent effect through on-line dilution so as to realize high-efficiency enrichment, and simultaneously, during analysis, the sample can be simultaneously diluted while being desorbed and transferred to the analysis column, so that the focusing of a target object on the analysis column is realized, and further, the high-efficiency separation of subsequent analytes is ensured.
3. The dual channel on-line enrichment analysis system of the present utility model combines HPLC analysis and multiplexing techniques, which can synchronize 2 parallel LC systems to a single mass spectrometer. Each system operates independently, allowing 2 methods to operate simultaneously in interleaved, parallel formations, yielding 2 times the throughput of a conventional LC/MS or LC/MS system, while maximizing the throughput of the mass spectrometer. The construction of a high throughput rapid analysis system is of great importance, providing efficient analysis of samples with complex matrices and low levels of targets, including plasma, urine and food matrices.
4. The dual-channel online enrichment analysis system can realize online enrichment and analysis of target objects in a large-volume water phase sample and an organic phase sample on the premise of not changing the system and the method by improving the flow path structure.
Drawings
Fig. 1 is a schematic diagram of the structural principle of the system of the present utility model.
Fig. 2 is a schematic diagram of the operation sequence of the present utility model in a specific application example.
Fig. 3 is a schematic diagram of the present utility model in a workflow in a specific application example.
Fig. 4 is a schematic diagram of the structural principle of the present utility model in another embodiment.
Legend description:
101. A pump A; 102. b, a pump; 103. a first process channel trap column TC1; 104. a first control valve V1; 105. a first process channel mixer; 106. a first separation column SC1; 201. c, a pump; 202. a pump D; 203. a second process channel trap column TC1; 204. a second control valve V2; 205. a second process channel mixer; 206. a second separation column SC2; 301. a sample injector; 302. a third control valve V3; 303. a fourth control valve V4; 304. a balance pump; 305. a fifth control valve V5; 306. a mass spectrum detector.
Detailed Description
The utility model will be described in further detail with reference to the drawings and the specific examples.
In the description of the present application, it should be understood that the terms "length," "width," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the present application and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the present application.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. In the description of the present application, the meaning of "a plurality" is two or more, unless explicitly defined otherwise.
In the present application, unless explicitly specified and limited otherwise, the terms "mounted," "connected," "secured," and the like are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally formed; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art according to the specific circumstances.
As shown in fig. 1 to 3, the dual-channel on-line enrichment analysis system of the present utility model includes: the sample injector 301 alternately injects sample to the first processing channel and the second processing channel, and then alternately introduces the separated target object of the first processing channel and the second processing channel into the mass spectrum detector for analysis; the first treatment channel and the second treatment channel respectively comprise a channel trapping column, a separation column, a control valve and a pump, and the trapping column is switched to an analysis stage after balancing, sample loading and enrichment are completed through the control valve.
In a specific application example, a balance pump is arranged between the first processing channel and the second processing channel, and the balance pump is used for completing a pre-balance process before analysis of the two analysis columns in the first processing channel and the second processing channel.
In a specific application example, the first processing channel and the second processing channel respectively undergo three stages of system balancing, sample injection+enrichment and analysis, and separated target objects are alternately introduced into a mass spectrum for further analysis.
As a preferred embodiment, the flow paths of the first processing channel and the second processing channel are isolated from each other in any stage, but the two first processing channels and the second processing channels are not completely independent, part of the flow paths and the valves are shared by the two systems, and the common part is switched by the valves to be distributed.
Referring to fig. 1, the present utility model is in one specific application example:
The first treatment channel comprises a pump A101, a pump B102, a first treatment channel trapping column TC1 103, a first separation column SC1 106 and a second control valve V2 204; the pump A101 and the pump B102 form a gradient pump in the first processing channel, and the second control valve V2 204 is used for controlling the trapping column TC1 103 on the first processing channel to switch to an analysis stage after the balance-loading-enrichment is completed.
The second treatment channel comprises a pump C201, a pump D202, a second treatment channel trapping column TC2 203, a second separation column SC2 206 and a third control valve V3 302; the pump C201 and the pump D202 form a gradient pump in the second processing channel, and the third control valve V3 302 is used for controlling the TC2 203 on the second processing channel trapping column to switch to the analysis stage after the balance-loading-enrichment is completed.
And the balance pump is used for completing the pre-balance process before analysis of the two analysis columns.
The first control valve V1 104 is used to implement the alternating sampling of the sampler 1 into the first processing channel and the second processing channel.
The fourth control valve V4 303 is used to realize a pre-balancing before the balance pump is alternately connected to the analytical columns of the first and second processing channels and the separation of the two analytical columns.
The fifth control valve V5 is used to alternately introduce the separated target object in the first processing channel and the second processing channel to the mass spectrum detector for analysis.
In another embodiment of the present utility model, referring to fig. 4, two ten-way valves may be used, one ten-way valve is used instead of the functions of the second control valve V2 204 and the third control valve V3 302, and the other ten-way valve is used instead of the functions of the fourth control valve V4 303 and the fifth control valve V5 305.
Referring to fig. 2 and 3, in order to illustrate the time sequence of the system of the present utility model when the first processing channel and the second processing channel are operated, the operation time sequence of the first processing channel is: balancing, sample injection and enrichment, analysis, balancing, sample injection and enrichment … …; the working time sequence of the second processing channel is as follows: waiting, balancing, feeding + enriching, analyzing … …; that is, the second process channel is one step behind the first process channel, and each is repeatedly circulated.
The system of the utility model can realize the on-line enrichment and analysis of large-volume water phase and organic phase samples, and the working process is described in detail below by combining a specific application example. The system of the utility model is constructed according to a conventional reverse phase analysis mode, wherein A, C is an aqueous phase mobile phase, B, D is an organic phase methanol or acetonitrile, an equilibrium pump is a water-rich phase (such as an aqueous solution containing 5% methanol or acetonitrile) trapping column and an analysis column are reverse phase columns, and the implementation of specific technical effects is explained in connection with steps 1-4 in the time sequence of fig. 2.
In step 1, the first treatment channel is in an equilibrium stage, and the balance pump enters the first separation column SC1 106 through the fourth control valve V4 and the second control valve V2 204 to balance the first treatment channel so as to prepare for the next analysis of the first treatment channel, meanwhile, on the premise that the total flow is unchanged, the pump a 101 and the pump B102 enter the initial state of gradient, that is, the low-flow organic phase pumped by the pump B102 passes through the injector and the second control valve V2 204, and the high-flow water from the pump a 101 enters the first treatment channel trapping column TC1 103 after being converged by the first treatment channel mixer to pre-balance the first treatment channel trapping column TC 1. Meanwhile, the second treatment channel is in the first half of the analysis stage, the low-flow organic solvent from the pump D202 of the second treatment channel rapidly desorbs the target analyte trapped in the previous step on the second treatment channel trapping column TC2 203 in a recoil mode, and then the low-flow organic solvent and the high-flow aqueous phase from the pump C201 of the second treatment channel are mixed and diluted in the second channel mixer and then enter the second treatment channel trapping column TC2 203 to realize column head focusing, so that high-efficiency separation is realized under the subsequent gradient elution, and the effluent from the second separation column SC2 206 enters a detector 306 (such as mass spectrum) for detection through a fifth control valve V5.
In step 2, the first treatment channel is in the sample injection enrichment stage, the low-flow organic phase pumped by the pump B102 of the first treatment channel takes away a large volume of sample through the sample injector, and enters the second control valve V2 204, and the high-flow aqueous phase mixed and diluted with the pump a 101 from the first treatment channel in the first treatment channel mixer enters the first treatment channel trapping column TC 1103, so that the sample can achieve the reduction of the solvent strength (if the sample solvent is the organic phase) under the dilution of the pump a 101 aqueous phase of the first treatment channel, thereby facilitating the efficient trapping of the sample seed target on the first treatment channel trapping column TC1 103. Meanwhile, the second processing channel is in the latter half of the analysis stage, the state of the second processing channel is consistent with that of the previous step, and the gradient solvent from the pump C201 and the pump D202 of the second processing channel enables the target analyte to be separated on the second separation column SC2 206, and the separated target analyte enters the mass spectrum detector 306 for detection through the fifth control valve V5 305.
In step 3, the first treatment channel is in the first half of the analysis stage, the low-flow organic solvent from the pump B102 of the first treatment channel rapidly desorbs the target analyte trapped in the previous step on the first treatment channel trapping column TC 1103 in a recoil mode, and then the low-flow organic solvent and the high-flow aqueous phase from the pump a 101 of the first treatment channel are mixed and diluted in the first channel mixer and enter the first separation column SC1 106 to realize column head focusing, so that efficient separation is realized under the subsequent gradient elution, and the effluent from the first separation column SC1 106 enters the mass spectrum detector 306 for detection through the fifth control valve V5 305. At the same time, the second processing channel is in an equilibrium stage, and the equilibrium pump enters the second separation column SC2 206 through the fourth control valve V4 and the second control valve V3 302 to balance the second separation channel so as to prepare for the next analysis of the second separation channel, in addition, the pump C201 and the pump D202 of the second processing channel enter the initial state of gradient, that is, the low-flow organic phase pumped by the pump D202 of the second processing channel passes through the sample injector to enter the third control valve V3 302, and the high-flow water from the pump C201 of the second processing channel enters the second processing channel trapping column TC2 203 after being converged by the second processing channel mixer to pre-balance the second processing channel trapping column TC2 so as to prepare for the enrichment of target analytes in the next step.
In step 4, the first processing channel is in the latter half of the analysis stage, the state of the first processing channel is consistent with that of the previous step, and the gradient solvents from the first processing channel pump a 101 and the pump B102 enable the target analyte to be separated on the first separation column SC1 106, and the separated target analyte enters the mass spectrum detector 306 for detection through the fifth control valve V5305. Meanwhile, the second treatment channel is in a sample injection enrichment stage, a low-flow organic phase pumped by a pump B102 of the second treatment channel takes away a large volume of sample through a sample injector, the large-volume sample enters a third control valve V3 302, the large-flow organic phase and a high-flow water phase from a pump C201 of the second treatment channel are mixed and diluted in a second treatment channel mixer and then enter a second treatment channel trapping column TC2 203, and the sample is diluted by the water phase of the pump C201 of the second treatment channel to reduce the solvent strength (if the sample solvent is the organic phase), so that target analytes in the sample can be trapped on the second treatment channel trapping column TC2 203 with high efficiency.
The four steps are the process of completing one complete cycle of the whole system, and the subsequent processes are sequentially circulated.
The flow path structure designed in the utility model can eliminate the solvent effect through dilution when the sample is enriched, and can dilute the sample when the sample is desorbed and transferred to the analysis column during analysis, thereby realizing the focusing of the target object on the analysis column and further ensuring the efficient separation of the subsequent analytes.
The above is only a preferred embodiment of the present utility model, and the protection scope of the present utility model is not limited to the above examples, and all technical solutions belonging to the concept of the present utility model belong to the protection scope of the present utility model. It should be noted that modifications and adaptations to the utility model without departing from the principles thereof are intended to be within the scope of the utility model as set forth in the following claims.

Claims (10)

1. A dual channel on-line enrichment and analysis system, comprising: the sample injector alternately injects sample to the first processing channel and the second processing channel, and then alternately introduces the target object separated by the first processing channel and the second processing channel into a mass spectrum for analysis; the first treatment channel and the second treatment channel respectively comprise a channel trapping column, a separation column, a control valve and a pump, and the trapping column is switched to an analysis stage after balancing, sample loading and enrichment are completed through the control valve.
2. The dual-channel on-line enrichment and analysis system according to claim 1, wherein a balance pump is arranged between the first processing channel and the second processing channel, and the balance pump is used for completing a pre-balance process before analysis of two analysis columns in the first processing channel and the second processing channel.
3. The dual-channel on-line enrichment and analysis system according to claim 2, wherein the first processing channel and the second processing channel are respectively subjected to three stages of system balancing, sample injection + enrichment and analysis, and separated target objects are alternately introduced into a mass spectrum detector for further analysis.
4. The dual channel on-line enrichment and analysis system according to claim 3, wherein the flow paths of the first and second processing channels are isolated from each other during any stage.
5. The dual channel on-line enrichment and analysis system according to any of claims 1-4, wherein the first processing channel comprises a pump a, a pump B, a first processing channel trapping column TC1, a first separation column SC1, a second control valve V2; the pump A and the pump B form a gradient pump in the first treatment channel, and the second control valve V2 is used for controlling the trapping column on the first treatment channel to complete balance-loading-enrichment and then switch to an analysis stage.
6. The two-channel on-line enrichment and analysis system according to any of claims 1-4, wherein the second processing channel comprises a pump C, a pump D, a second processing channel trapping column TC2, a second separation column SC2, and a third control valve V3; the pump C and the pump D form a gradient pump in the second treatment channel, and the third control valve V3 is used for controlling the trapping column on the second treatment channel to switch to an analysis stage after balance-loading-enrichment is completed.
7. The dual channel on-line enrichment and analysis system according to any of claims 1-4, further comprising a first control valve V1, wherein the first control valve V1 is configured to implement an alternating sample introduction of the sample injector into the first processing channel and the second processing channel.
8. The dual channel on-line enrichment and analysis system according to any of the claims 2-4, further comprising a fourth control valve V4, wherein the fourth control valve V4 is used to realize a pre-balancing before the balance pump is alternately connected to the analysis columns of the first and second processing channels and the separation of the two analysis columns.
9. The dual channel on-line enrichment and analysis system according to any of claims 1-4, further comprising a fifth control valve V5, wherein the fifth control valve V5 is configured to alternately introduce the separated targets of the first and second processing channels to the mass spectrum detector for analysis.
10. The two-channel on-line enrichment and analysis system according to any of claims 2-4, wherein two ten-way valves are used, one of which is used to switch to the analysis stage after the completion of the balance-load-enrichment by controlling the trapping column on the first process channel and to switch to the analysis stage after the completion of the balance-load-enrichment by controlling the trapping column on the second process channel; the other ten-way valve is used for realizing the pre-balancing before the balance pump is alternately connected to the analysis columns of the first processing channel and the second processing channel and separates the two analysis columns, and is used for alternately introducing the target objects separated by the first processing channel and the second processing channel into the mass spectrum detector for analysis.
CN202322773363.6U 2023-10-16 2023-10-16 Double-channel on-line enrichment and analysis system Active CN221238744U (en)

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CN202322773363.6U CN221238744U (en) 2023-10-16 2023-10-16 Double-channel on-line enrichment and analysis system

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Application Number Priority Date Filing Date Title
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CN221238744U true CN221238744U (en) 2024-06-28

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