CN116613052B - Electrospray ion source with external magnetic field and mass spectrometer - Google Patents
Electrospray ion source with external magnetic field and mass spectrometer Download PDFInfo
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- CN116613052B CN116613052B CN202310884323.0A CN202310884323A CN116613052B CN 116613052 B CN116613052 B CN 116613052B CN 202310884323 A CN202310884323 A CN 202310884323A CN 116613052 B CN116613052 B CN 116613052B
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- 239000007788 liquid Substances 0.000 claims abstract description 82
- 239000007921 spray Substances 0.000 claims abstract description 48
- 238000009718 spray deposition Methods 0.000 claims abstract description 28
- 238000004807 desolvation Methods 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims description 19
- 238000005070 sampling Methods 0.000 claims description 8
- 229910001172 neodymium magnet Inorganic materials 0.000 claims description 4
- 230000035945 sensitivity Effects 0.000 abstract description 18
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000005507 spraying Methods 0.000 abstract description 4
- 230000002776 aggregation Effects 0.000 abstract description 2
- 238000004220 aggregation Methods 0.000 abstract description 2
- 150000002500 ions Chemical class 0.000 description 50
- 239000007789 gas Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 230000009471 action Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 238000001819 mass spectrum Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000000523 sample Substances 0.000 description 5
- 238000004949 mass spectrometry Methods 0.000 description 4
- 229920001451 polypropylene glycol Polymers 0.000 description 4
- BGPVFRJUHWVFKM-UHFFFAOYSA-N N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] Chemical compound N1=C2C=CC=CC2=[N+]([O-])C1(CC1)CCC21N=C1C=CC=CC1=[N+]2[O-] BGPVFRJUHWVFKM-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000006978 adaptation Effects 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- -1 ions in solution) Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000005499 meniscus Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/04—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components
- H01J49/0431—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples
- H01J49/0445—Arrangements for introducing or extracting samples to be analysed, e.g. vacuum locks; Arrangements for external adjustment of electron- or ion-optical components for liquid samples with means for introducing as a spray, a jet or an aerosol
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/10—Ion sources; Ion guns
- H01J49/16—Ion sources; Ion guns using surface ionisation, e.g. field-, thermionic- or photo-emission
- H01J49/165—Electrospray ionisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/02—Details
- H01J49/20—Magnetic deflection
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J49/00—Particle spectrometers or separator tubes
- H01J49/26—Mass spectrometers or separator tubes
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides an electrospray ion source and a mass spectrometer, wherein the electrospray ion source is provided with an external magnetic field, and at least comprises a spray forming part with an internal liquid channel, and liquid flows through the internal liquid channel to form charged liquid drop spray at an outlet of the spray forming part; and a magnetic field generating device for generating a magnetic field in which the liquid flowing through the internal liquid passage and/or the charged droplet spray formed at the outlet of the spray forming section is/are placed. The invention is provided with the magnetic field generating device in the electrospray ion source, can effectively optimize the spraying effect, is beneficial to aggregation and desolvation of charged liquid drops, and finally improves the ionization efficiency of the ion source, thereby improving the sensitivity of the mass spectrometer.
Description
Technical Field
The invention relates to the field of mass spectrometry, in particular to an electrospray ion source with an external magnetic field and a mass spectrometer.
Background
Mass spectrometry is one of the analysis methods with highest sensitivity at present, and is widely applied to various fields such as chemistry, environment, food, life science and the like. Mass spectrometers typically consist of a sample introduction system, an ion source that functions to ionize the sample, a vacuum system, a mass analyzer, a detector, a data processing system, and the like. Sample ionization is a precondition for mass spectrometry and is directly related to the range of application of the mass spectrometer.
ESI sources (Electrospray ioniation, electrospray ion sources) are one commonly used ion source. ESI sources have the characteristics of multi-charge ionization, high ionization efficiency for certain polar compounds, and soft ionization, making them widely used for ionization of polar compounds (including ions in solution), readily decomposable, and macromolecular compounds. The operating principle of the ESI source is as follows: the sample solution is sprayed out at high speed through an ESI nozzle, and tiny liquid drops are formed under the action of spray gas. The compounds in the ionic state in the droplets move in opposite directions under the action of an electric field, and thus an initially charged droplet (charged dorplet) is generated. The charged droplets are broken down during the continuous evaporation of the solvent, the surface charge density increases continuously, and when the Rayleigh limit is reached, the droplets are broken up (i.e. coulomb explosion) and the process is repeated continuously, and finally the resolved ions enter the vacuum zone. Referring to FIG. 1, a schematic diagram of the formation of positive ions for an ESI source is shown. See [ Rojie hong ] and some theoretical discussion of the principle of electrospray ion source, guangdong chemical industry, volume 47, 13 in 2020.
Sensitivity is an important parameter in measuring the performance of a mass spectrometer, and sensitivity is closely related to ionization efficiency of an ion source. Conventional ESI sources, while having a relatively high sensitivity, have yet to be further improved in sensitivity for very small amounts of samples or micro-components.
Disclosure of Invention
Based on the background, the invention provides an electrospray ion source provided with an externally applied magnetic field and a mass spectrometer provided with the electrospray ion source, so that the electrospray ion source has higher sensitivity.
The technical purpose of the invention is realized by the following technical scheme:
the first aspect of the present invention provides an electrospray ion source provided with an externally applied magnetic field, the electrospray ion source comprising at least a spray forming section having an internal liquid passage through which liquid flows to form a spray of charged droplets at an outlet of the spray forming section; and a magnetic field generating device for generating a uniform or non-uniform magnetic field such that the liquid flowing through the internal liquid passage and/or the charged droplet spray formed at the outlet of the spray forming section is in the magnetic field.
In some embodiments, the spray formation is a spray needle or a liquid capillary.
In some embodiments, the direction of the magnetic field at the spray formation is at an angle of 0-5 ° to the direction of flow of liquid in the internal liquid channel.
In some embodiments, the direction of the magnetic field at the spray formation is parallel to the flow direction of the liquid in the internal liquid channel.
In some embodiments, the magnetic field generating device is disposed around the spray formation or is configured to be distributed over the area where the charged droplet spray is located.
In some embodiments, the magnetic component in the magnetic field generating device is a permanent magnet or an electromagnet.
In some embodiments, the magnetic field generating device is at least one ring magnet that fits over the spray forming section.
In some embodiments, the ring magnet is a neodymium-iron-boron magnet or an N35 magnet.
In some embodiments, the magnetic field generating device is a coil that is sleeved over the spray forming section, the coil generating an adjustable magnetic field by a current flowing therethrough.
In some embodiments, a negative or positive voltage is applied to the spray needle or liquid capillary.
Preferably, the negative voltage is-2 KV to-5.5 KV, and the positive voltage is +2KV to +5.5KV.
In some embodiments, the liquid has a flow rate in the spray formation section of 5 μl/min and the electrospray ion source has an atomizing gas flow rate of 15L/min.
In a second aspect the invention provides a mass spectrometer comprising an electrospray ion source as described in the first aspect above.
In some embodiments, the spray formation is not on the same axis as the sampling port of the mass spectrometer, and the charged droplets enter the sampling port of the mass spectrometer after desolvation through a curved path.
The beneficial technical effects of the invention are as follows:
the invention is provided with the magnetic field generating device in the electrospray ion source, and the device can enable positive and negative ions or charged liquid drops formed in or by the spray forming part to be in the magnetic field, and enable the positive and negative ions or the charged liquid drops to be subjected to the action of Lorentz force, thereby being beneficial to the separation of the positive and negative ions and the formation of the charged liquid drops, and enabling the charged liquid drops to collide with each other to form the charged liquid drops with smaller volume, and optimizing the spray effect. Meanwhile, the magnetic field can change the motion track of the charged liquid drops, thereby being beneficial to aggregation and desolvation of the charged liquid drops, and finally improving the ionization efficiency of the ion source and further improving the sensitivity of the mass spectrometer.
Drawings
FIG. 1 is a schematic diagram of a conventional ESI source for generating positive ions.
FIG. 2 is a simplified schematic diagram of an ESI source.
Fig. 3 is a schematic diagram of the movement of charged droplets or ions in a magnetic field.
Fig. 4 is a schematic diagram of an electrospray ion source and a mass spectrometer with a magnetic field according to an embodiment of the present invention.
Fig. 5 is a mass spectrum of PPG measured by a triple quadrupole mass spectrometer with a conventional TurboV ™ ion source.
Fig. 6 is a mass spectrum of PPG measured by a triple quadrupole mass spectrometer with a TurboV ™ ion source equipped with a magnetic field generating device according to an embodiment of the present invention.
Detailed Description
The invention is further described below with reference to the drawings and examples. It should be noted that the examples are only detailed description of the present invention and are not intended to limit the scope of the present invention. All of the features disclosed in the embodiments of the invention, or all of the steps of the methods or processes disclosed, except for mutually exclusive features and/or steps, can be combined in any way and are within the scope of the invention. Any modification made by the technical idea of the present invention without making any creative effort by those of ordinary skill in the art should be within the protection scope of the present invention. The technology not related to the invention can be realized by the prior art.
Referring to fig. 2, which is a simplified schematic diagram of an ESI source, spray needle 1 is comprised of a liquid capillary 2 and a gas passage. The gas channel is located at the periphery of the liquid capillary 2 for the passage of gas, which may be one or more turns, for the passage of one or more auxiliary gases. The liquid capillary 2 is used for the passage of a sample, typically a liquid. The liquid capillary 2 is provided with high-voltage electricity, and when the liquid passes through the liquid capillary 2, the liquid is subjected to the action of a high-voltage electric field, and positive and negative ions therein start to move. If the capillary is positive, positive ions move towards the meniscus at the tip and negative ions move in the opposite direction (see fig. 1). A taylor cone is formed at the outlet end, the liquid at the cone tip is unstable under the action of coulomb repulsion and breaks up into charged liquid drops 3 quickly, and the charged liquid drops 3 are distributed into umbrella-shaped or jet-shaped sprays. The assist gas can assist in the formation of charged droplets, accelerate charged droplets, aggregate, and the like. The final resolution of ions by charged droplets is described in the background section of the specification. The sensitivity of a mass spectrometer is closely related to the ionization efficiency of the ion source. Although the existing ESI source has higher sensitivity, the sensitivity of the existing ESI source is still to be further improved for very trace samples or trace components.
The inventors of the present application have unexpectedly found during the experiment that the sensitivity of the mass spectrometer is significantly higher by adding a magnetic field to the periphery of the spray needle 1 or the liquid capillary 2 and the charged droplets, i.e. providing a magnetic field generating means.
Based on this, the present invention provides an electrospray ion source provided with an externally applied magnetic field. The electrospray ion source comprises at least a spray forming part with an internal liquid channel, typically a spray needle or a liquid capillary, through which liquid flows to form a spray of charged droplets at the outlet of the spray forming part. In order to increase the sensitivity, the electrospray ion source is further provided with magnetic field generating means for generating a magnetic field such that the liquid flowing through the liquid channel inside the spray forming section and/or the charged droplet spray formed at the outlet of the spray forming section is in the magnetic field.
As a preferred embodiment, in this example, a magnetic field generating device is disposed around the spray forming section or is configured to surround the region where the charged droplet spray is formed.
As a preferred embodiment, in this example, the direction of the magnetic field at the spray formation section is parallel to the flow direction of the liquid in the liquid passage inside the spray formation section.
In other embodiments, the direction of the magnetic field at the spray forming section is at an angle (0-5 ° angle) to the direction of the flow of the liquid in the liquid passage inside the spray forming section, provided that the technical object of the present invention can be achieved to some extent, and is not particularly limited herein.
The principle of the electrospray ion source provided with an externally applied magnetic field of the invention with reference to fig. 2 and 3 can be discussed below with greater sensitivity.
Referring to fig. 2 and 3, when a spray of liquid flowing through the liquid passage inside the spray formation section (i.e., the spray needle) or charged droplets formed at the outlet of the spray formation section is subjected to a magnetic field:
(1) Positive or negative ions in the liquid channel (liquid capillary) inside the spray forming part (i.e. the spray needle) can also receive the action of Lorentz force in the magnetic field B, and the directions of Lorentz received by the positive ions and the negative ions are different, and the movement directions are different, so that the separation of the positive ions and the negative ions is facilitated, and the formation of Taylor cones and the formation of charged liquid drops are facilitated.
(2) Taking positively charged droplets as an example, if the droplets are on the periphery of the umbrella-shaped spray in fig. 2, the movement direction is denoted as V, the angle between B and V is denoted as θ when subjected to the magnetic field B, and V is divided into a velocity component (Vx) in the parallel B direction and a velocity component (Vy) in the perpendicular direction to B, and the lorentz force applied to the droplets has a magnitude of f=qvyb. If B is a uniform magnetic field, the droplet moves linearly at a constant speed in the direction parallel to B and moves circularly at a constant speed in the direction perpendicular to B, and the trajectory resembles a spring (as shown in fig. 3) with a radius of rotation r= mVy/qb=mv×sin θ/qB. In this way, further spreading of the charged droplets to the periphery of the "umbrella-like or jet-like" can be prevented, so that the charged droplets are gathered toward the middle, and peripheral loss is reduced. The charged droplets are easy to collide with each other to generate smaller droplets, which is beneficial to desolvation and coulomb explosion to generate charged ions. Meanwhile, the movement track of the charged liquid drops is increased, so that the charged liquid drops can be fully contacted with the drying gas, and the desolvation process is facilitated. The magnetic field B may be a non-uniform magnetic field, and in this case, the charged droplet performs non-uniform circular motion in the vertical direction B, and its motion track is in an irregular spring shape or spiral shape.
In some embodiments of the invention, the magnetic field generating device may be a permanent magnet or an electromagnet, such as a NdFeB magnet of model N35, which may be elongated, annular, or other irregular shape.
In a specific example, referring to fig. 4, the magnetic field generating device is a ring magnet 4 sleeved on the spray needle 1, and the ring magnet 4 is preferably an N35 neodymium iron boron magnet, and has a width of 7mm and a thickness of 4.7mm. The magnetic field B formed by the liquid spraying needle is unevenly distributed, the liquid in the spraying needle 1 and the formed charged liquid drops are all in the magnetic field B, and the magnetic field of the liquid channel in the spraying needle 1 is approximately parallel to the flow direction of the liquid.
Meanwhile, a negative voltage or a positive voltage is applied to the spray needle or the liquid capillary. Preferably, the negative voltage is minus 2KV to minus 5.5KV, and the positive voltage is +2KV to +5.5KV.
Referring to FIGS. 5 and 6, when the electrospray ion source was a TurboV ™ ion source, a ternary quadrupole mass spectrometer (AB SCIEX mass spectrometer TRIPLE QUAD 5500) was used to detect PPG (polypropylene glycol) samples at a sample flow rate of 5. Mu.L/min, a voltage applied by a spray needle of 5.5kV, an assist gas (N) 2 ) The flow rate was 15L/min, and the mass spectrum was shown in FIG. 5.
Under the same conditions, the mass spectrum of the ring magnet 4 was measured as shown in fig. 6 by sleeving the outer wall of the spray needle of the TurboV ™ ion source with the ring magnet according to the example. As can be seen from comparing fig. 5 and fig. 6, after the ring magnet is added, the mass spectrum response value is obviously improved, which indicates that the ring magnet obviously improves the sensitivity of the mass spectrometer.
It should be noted that the sensitivity of the mass spectrometer can be obviously improved by adding a small annular permanent magnet around the spray needle 1, which is of great importance to the miniaturization of the mass spectrometer and is beneficial to the development of the miniature high-sensitivity mass spectrometer. However, the magnetic field size, direction, etc. of the small annular permanent magnet are relatively fixed, and the parameter adjustment and optimization are inconvenient in the practical process. For a large mass spectrometer, the device for providing the magnetic field can be an electromagnet capable of adjusting the size or direction of the magnetic field, so that the device can be conveniently adjusted according to different samples, detection requirements and the like in the use process, and the sensitivity of the mass spectrometer can be maximally improved.
For example, the ring magnet in the above example may be replaced by a ring coil that can generate a magnetic field by a current flowing therethrough, and adjust the magnitude and distribution of the magnetic field by adjusting the magnitude of the current, thereby achieving optimal parameters.
The above examples only show the manner of attaching the magnetic member to the spray needle 1. In other examples, the magnetic component may be further configured so that the magnetic field generated by the magnetic component is distributed in the area where the charged droplet sprays, so that the magnetic component sleeved on the spray needle 1 independently or cooperatively acts together to achieve a better ionization effect and improve the sensitivity of the mass spectrometer.
Further embodiments of the invention provide a mass spectrometer comprising an electrospray ion source as described in the previous embodiments.
In some embodiments, the spray needle or liquid capillary is on the same axis as the sampling port of the mass spectrometer (see fig. 1).
In a further preferred embodiment, the spray needle 1 or liquid capillary 2 is not on the same axis as the sampling port 5 of the mass spectrometer (see fig. 4), and the charged droplets enter the sampling port of the mass spectrometer after desolvation by a curved path. Thus, non-volatile impurities, uncharged neutral ions and the like can be prevented from reaching the sampling port to cause pollution or blockage.
The electrospray ion source can be an electrospray ion source of a mass spectrometer sold in the market of common mass spectrometry factories, such as Agilent, siemens, AB SCIEX, shimadzu and the like, and can also be an electrospray ion source shown in patents CN201920942187.5, CN201811403019.5, CN201210207369.0 and the like.
The above description of the embodiments is only for aiding in the understanding of the method of the present invention and its core ideas. It should be noted that it will be apparent to those skilled in the art that various modifications and adaptations of the invention can be made without departing from the principles of the invention and these modifications and adaptations are intended to be within the scope of the invention as defined in the following claims.
Claims (10)
1. An electrospray ion source provided with an externally applied magnetic field and applied to a mass spectrometer is characterized by at least comprising a spray forming part with an internal liquid channel, wherein the spray forming part is a spray needle or a liquid capillary, and liquid flows through the internal liquid channel to form charged liquid drop spray at an outlet of the spray forming part; the liquid spray generating device comprises a spray forming part, a magnetic field generating device and a liquid spray forming part, wherein the spray forming part is provided with a plurality of liquid inlets, the liquid inlets are connected with the liquid spray forming part, the liquid spray forming part is provided with a plurality of liquid inlets, and the liquid spray forming part is provided with a plurality of liquid inlets; the magnetic field direction at the spray forming part forms an included angle of 0-5 degrees with the flow direction of the liquid in the internal liquid channel.
2. The electrospray ion source provided with an externally applied magnetic field as recited in claim 1, wherein a magnetic field direction at the spray formation portion is parallel to a flow direction of liquid in the internal liquid channel.
3. The electrospray ion source according to claim 1, wherein the magnetic component in the magnetic field generating device is a permanent magnet or an electromagnet.
4. An electrospray ion source as recited in claim 3, wherein said magnetic field generating means is at least one ring magnet sleeved on the spray forming portion.
5. The electrospray ion source according to claim 4, wherein said ring magnet is a neodymium-iron-boron magnet or an N35 magnet.
6. An electrospray ion source as claimed in claim 3, wherein said magnetic field generating means is a coil which is fitted over the spray formation part and generates an adjustable magnetic field by means of a current flowing through it.
7. The electrospray ion source according to claim 1, wherein a negative or positive voltage is applied to the spray needle or the liquid capillary.
8. The electrospray ion source provided with an externally applied magnetic field as recited in claim 1, wherein a flow rate of the liquid in the spray formation section is 5 μl/min, and an atomizing gas flow rate of the electrospray ion source is 15L/min.
9. A mass spectrometer comprising the electrospray ion source as recited in any one of claims 1-8.
10. The mass spectrometer of claim 9, wherein the spray formation is not on the same axis as the sampling port of the mass spectrometer, and the charged droplets enter the sampling port of the mass spectrometer after desolvation through a curved path.
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| CN112224450A (en) * | 2020-10-21 | 2021-01-15 | 中国人民解放军国防科技大学 | Low-voltage electrospray emission device |
| CN113410120A (en) * | 2021-05-28 | 2021-09-17 | 清华大学深圳国际研究生院 | Method and device for generating spray ions |
| CN218939593U (en) * | 2022-07-15 | 2023-04-28 | 杭州凯莱谱质造科技有限公司 | Ion source |
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