CN112147264A - Combined system of chromatography and mass spectrometry - Google Patents

Combined system of chromatography and mass spectrometry Download PDF

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Publication number
CN112147264A
CN112147264A CN202010992378.XA CN202010992378A CN112147264A CN 112147264 A CN112147264 A CN 112147264A CN 202010992378 A CN202010992378 A CN 202010992378A CN 112147264 A CN112147264 A CN 112147264A
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ion
module
source
chromatography
ion source
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尹伊君
俞晓峰
陈悠
杨继伟
李锐
韩双来
雷鑫槐
王强
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Concentrating Technology Hangzhou Co ltd
Focused Photonics Hangzhou Inc
Hangzhou Puyu Technology Development Co Ltd
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Concentrating Technology Hangzhou Co ltd
Hangzhou Puyu Technology Development Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers

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Abstract

The invention provides a chromatography and mass spectrometry combined system, which comprises an ion source, a chromatography module and a mass analyzer, wherein the ion source is connected with the chromatography module; the ion source comprises a first ion source and a second ion source; the combined chromatography and mass spectrometry system further comprises: the first ion transmission module and the second ion transmission module are sequentially arranged on an ion emergent line of the first ion source; the isolation valve is arranged on an ion travel route between the first ion transmission module and the second ion transmission module; the ions emitted by the second ion source are deflected by the ion deflection module and then enter the second ion transmission module; the first ion transmission module, the isolation valve, the second ion transmission module and the ion deflection module are arranged in the vacuum module. The invention has the advantages of small volume, simple operation, low cost and the like.

Description

Combined system of chromatography and mass spectrometry
Technical Field
The invention relates to mass spectrometry, in particular to a combined chromatography and mass spectrometry system.
Background
Both liquid chromatography and gas chromatography systems are commonly used analytical instruments. In liquid chromatography, the fluid may be an organic liquid solvent, an aqueous liquid solvent or a mixture of organic and aqueous solvents, and the effluent is a liquid. In gas chromatography, the fluid is a carrier gas and the effluent is gaseous.
The samples that can be directly separated by GC are volatile and thermally stable, with boiling points generally not exceeding 500 ℃. According to statistics, 20-25% of the currently known compounds can be directly analyzed by GC, and the rest can be analyzed by LC in principle.
The chromatographic analysis may be performed on a gaseous sample or a liquid sample. Once the samples are separated, they may require further analysis to determine what the different components are. Generally, the most effective method of analyzing the separated components is to use a mass spectrometer. Mass spectrometers are complex and sophisticated instruments that are always specifically designed for one of LC-MS and GC-MS, i.e., the mass spectrometers required to perform liquid chromatography and gas chromatography are different and cannot be used interchangeably, so that two different instruments are required to perform different analyses.
In order to solve the problem of different interchange of liquid chromatography and gas chromatography, the solution provided by the prior art is as follows:
1. switching between GC-MS and LC-MS is realized by changing the instrument ion source. The technical problems brought are that:
handover is very time consuming and often comes at the cost of compromising the performance of one or the other of the two technologies;
for vacuum GC-MS systems that utilize electron impact ionization (EI), an additional vacuum pump at the ion source is required, increasing cost.
2. An APCI ion source was used. APCI is an ionization method that can be used for both liquid and gaseous samples. The advantage of using APCI is that both LC-MS and GC-MS operate at the same pressure and no MS changes are required except to replace the ion chamber instead of the conical gas nozzle. The technical problems that are brought about are that:
the APCI ion source has a narrow application range and cannot meet most LC and GC applications. Even in these cases, changing its mode of operation requires hardware changes, such as some showerhead hardware changes in the APCI ion source.
Disclosure of Invention
In order to overcome the defects in the prior art scheme, the invention provides a chromatograph-mass spectrometer system which is short in switching time, small in size and low in cost, and can be used for analyzing more extensive compounds.
The purpose of the invention is realized by the following technical scheme:
the system comprises a chromatography and mass spectrometry combined system, a mass spectrometer and a mass spectrometer, wherein the ion source is connected with the chromatography module; the ion source comprises a first ion source and a second ion source;
the combined chromatography and mass spectrometry system further comprises:
the ion source comprises a first ion transmission module and a second ion transmission module, wherein the first ion transmission module and the second ion transmission module are sequentially arranged on an ion emergent line of the first ion source;
an isolation valve disposed on an ion travel path between the first ion transport module and the second ion transport module;
the ion deflection module deflects ions emitted by the second ion source and then enters the second ion transmission module;
and the first ion transmission module, the isolation valve, the second ion transmission module and the ion deflection module are arranged in the vacuum module.
Compared with the prior art, the invention has the beneficial effects that:
1. the structure is simple and the volume is small;
corresponding ion sources are respectively configured on the gas chromatography and the liquid chromatography, only one set of mass spectrum module is configured, and ions are deflected by the ion deflection module, so that ions emitted by the two ion sources enter the same set of mass spectrum module, the volume of the whole system is reduced, and the precious laboratory working space is saved;
the LC does not need back flushing in a standby state, so that the aim of saving the air consumption is fulfilled, and the operation cost is reduced;
2. the operation is simple, and the maintenance amount is small;
the switching between the liquid chromatography and the gas chromatography is realized by switching the first ion source and the second ion source, the switching is simple and quick, the manual disassembly of a liquid chromatography module and a gas chromatography module is not needed, and the workload is low;
3. the first ion source is an EI source or a CI source and is connected with the liquid chromatography module; the second ion source is either an ESI source or an APCI source, connected to the gas chromatography module, allowing a wider range of compounds to be analyzed on a single set of co-usage systems.
Drawings
The disclosure of the present invention will become more readily understood with reference to the accompanying drawings. As is readily understood by those skilled in the art: these drawings are only for illustrating the technical solutions of the present invention and are not intended to limit the scope of the present invention. In the figure:
FIG. 1 is a schematic diagram of a combined chromatography and mass spectrometry system according to an embodiment of the invention;
FIG. 2 is another schematic diagram of a combined chromatography and mass spectrometry system according to an embodiment of the invention.
Detailed Description
Fig. 1-2 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. Some conventional aspects have been simplified or omitted for the purpose of teaching the present invention. Those skilled in the art will appreciate that variations or substitutions from these embodiments will be within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the present invention is not limited to the following alternative embodiments, but is only limited by the claims and their equivalents.
Example 1:
fig. 1 shows a schematic structural diagram of a chromatography-mass spectrometry system according to an embodiment of the present invention, and as shown in fig. 1, the chromatography-mass spectrometry system includes:
the ion source is connected with the chromatography module; the ion source comprises a first ion source and a second ion source, wherein the first ion source is connected with the liquid chromatography module, and the second ion source is connected with the gas chromatography module;
a first ion transmission module and a second ion transmission module, such as ion transmission rods, which are sequentially arranged on an ion exit path of the first ion source;
an isolation valve 3 disposed on an ion travel path between the first and second ion transport modules for selectively isolating and passing the emergent ions of the first ion source; the isolation valve serves two purposes: 1. when the system is in standby, the isolation valve is closed, so that the vacuum system can be effectively protected, the load of the vacuum pump is reduced, the service life of the vacuum pump is prolonged, equipment in the vacuum module is protected, and equipment pollution caused by continuous vacuum pumping is avoided; 2. when the system is operating in the GC mode, the isolation valve is closed so that the ion transport, ion deflection module, second ion source (EI/CI source) and mass filter are in the same vacuum state;
the ion deflection module 5 deflects ions emitted by the second ion source and then enters the second ion transmission module, so that the ions emitted by the first ion source and the second ion source enter the same mass analyzer at different times, and the liquid chromatogram and the gas chromatogram share the same mass spectrometer;
the first ion transmission module, the isolation valve, the second ion transmission module and the ion deflection module are arranged in the vacuum module;
the mass filter and the collision reaction cell are sequentially arranged on a forehead ion travel route between the second ion transmission module and the mass analyzer.
The first ion source is preferably an EI or CI source working under normal pressure, the second ion source is preferably an ESI source or an APCI source working under vacuum, correspondingly, a vacuum interface is arranged between the first ion source and the vacuum module and is used for providing a primary vacuum environment for extracting and transmitting the ion beam emitted by the first ion source; the second ion source is disposed within the vacuum module.
The application mode of the combined system of chromatography and mass spectrometry in the embodiment is as follows:
Figure RE-GDA0002794262560000041
Figure RE-GDA0002794262560000051
in the above manner, the first ion source can be switched among four ionization modes of ESI +/ESI-/APCI +/APCI-, and the second ion source can be switched among two ionization modes of EI/CI.
Example 2:
an example of an application of the system for the combination of chromatography and mass spectrometry according to example 1 of the present invention.
In this application example, as shown in fig. 2, a third ion transmission module is provided between the first ion transmission module and the isolation valve 3, and the three ion transmission modules employ ion transmission rods; the ion deflection module 5 adopts a transmission device in CN 2020100844706; the first ion source is an ESA or APCI source and is connected with the liquid chromatogram; the second ion source is an EI or CI source and is connected with the gas chromatograph; the second ion source, the three ion transport modules, the ion deflection module, and the mass filter are in the same vacuum module.
The working mode of the combined system of chromatography and mass spectrometry of the embodiment is as follows:
when the GC mode (namely the second ion source) works, the vacuum isolation valve is closed, ion beams are generated in the EI/CI source, the direct-current bias voltage is applied to the third ion transmission module, and the third ion transmission module and the ion deflection module jointly act to guide the ion beams emitted by the second ion source to the shared first-stage mass filter, the collision reaction tank, the mass analyzer and the signal acquisition module for gas chromatography mass spectrometry.
When the LC mode (namely the first ion source) works, the vacuum isolation valve is opened, ion beams are generated in the ESI/APCI source, the ion beams are extracted through the vacuum interface and transmitted to the three ion transmission modules, at the moment, the ion deflection module does not work, bias voltage and radio frequency voltage are applied to the ion transmission modules, the ion beams are guided to the shared first-stage mass filter, the collision reaction pool, the mass analyzer and the signal acquisition module, and liquid chromatography mass spectrometry is carried out.
When the system is in standby, the vacuum isolation valve is closed, so that the vacuum system is protected, and the back-flushing gas consumption is saved.

Claims (4)

1. The system comprises a chromatography and mass spectrometry combined system, a mass spectrometer and a mass spectrometer, wherein the ion source is connected with the chromatography module; wherein the ion source comprises a first ion source and a second ion source;
the combined chromatography and mass spectrometry system further comprises:
the ion source comprises a first ion transmission module and a second ion transmission module, wherein the first ion transmission module and the second ion transmission module are sequentially arranged on an ion emergent line of the first ion source;
an isolation valve disposed on an ion travel path between the first ion transport module and the second ion transport module;
the ion deflection module deflects ions emitted by the second ion source and then enters the second ion transmission module;
and the first ion transmission module, the isolation valve, the second ion transmission module and the ion deflection module are arranged in the vacuum module.
2. The combined chromatography and mass spectrometry system of claim 1, wherein the first ion source is an EI source or a CI source coupled to a liquid chromatography module; the second ion source is an ESI source or an APCI source coupled to the gas chromatography module.
3. The system of claim 2, wherein the second ion source is disposed within the vacuum module and a vacuum interface is disposed between the first ion transport module and the first ion source.
4. The system according to claim 1, wherein the ion deflection module and the mass analyzer are configured with a mass filter and a collision cell in sequence along the ion path.
CN202010992378.XA 2020-09-21 2020-09-21 Combined system of chromatography and mass spectrometry Pending CN112147264A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112798677A (en) * 2020-12-31 2021-05-14 杭州谱育科技发展有限公司 Multi-mode mass spectrometry system and method

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112798677A (en) * 2020-12-31 2021-05-14 杭州谱育科技发展有限公司 Multi-mode mass spectrometry system and method

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