CN105355535B - Ion source and ioning method - Google Patents
Ion source and ioning method Download PDFInfo
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- CN105355535B CN105355535B CN201510599393.7A CN201510599393A CN105355535B CN 105355535 B CN105355535 B CN 105355535B CN 201510599393 A CN201510599393 A CN 201510599393A CN 105355535 B CN105355535 B CN 105355535B
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- insulation tube
- ion source
- openend
- grounding
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000009413 insulation Methods 0.000 claims abstract description 68
- 239000012159 carrier gas Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 11
- 230000005611 electricity Effects 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 150000002500 ions Chemical class 0.000 description 34
- 239000000523 sample Substances 0.000 description 18
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 4
- 229920000877 Melamine resin Polymers 0.000 description 4
- 229960001948 caffeine Drugs 0.000 description 4
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- HNDVDQJCIGZPNO-UHFFFAOYSA-N histidine Natural products OC(=O)C(N)CC1=CN=CN1 HNDVDQJCIGZPNO-UHFFFAOYSA-N 0.000 description 4
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 4
- 238000004451 qualitative analysis Methods 0.000 description 4
- 238000004445 quantitative analysis Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 239000012472 biological sample Substances 0.000 description 3
- 230000008602 contraction Effects 0.000 description 3
- 230000007812 deficiency Effects 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 238000000688 desorption electrospray ionisation Methods 0.000 description 3
- 238000000375 direct analysis in real time Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000001307 helium Substances 0.000 description 3
- 229910052734 helium Inorganic materials 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 238000005984 hydrogenation reaction Methods 0.000 description 3
- 230000003595 spectral effect Effects 0.000 description 3
- 238000010183 spectrum analysis Methods 0.000 description 3
- 150000001413 amino acids Chemical class 0.000 description 2
- 238000001601 dielectric barrier discharge ionisation Methods 0.000 description 2
- 238000010265 fast atom bombardment Methods 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920001184 polypeptide Polymers 0.000 description 2
- 102000004196 processed proteins & peptides Human genes 0.000 description 2
- 108090000765 processed proteins & peptides Proteins 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 1
- 238000000451 chemical ionisation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005686 electrostatic field Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Abstract
The present invention provides a kind of ion source and ioning method, the ion source includes：Insulation tube, the insulation tube both ends open；First electrode, the first electrode are arranged on the outside of the insulation tube, and the first electrode has the first terminals；Second electrode, the second electrode are arranged on the inside of the insulation tube or are arranged on the outside of the insulation tube, and on the extending direction of the insulation tube, the second electrode is in the right side of the first electrode, and the second electrode has the second terminals；Grounding electrode, the grounding electrode are arranged on the openend of the insulation tube.The present invention has many advantages, such as high sensitivity.
Description
Technical field
The present invention relates to ion sources, more particularly to ion source and ioning method.
Background technology
Mass-spectrometric technique is one of most wide analysis method of the most sensitive and application range being currently known.In mass-spectrometric technique,
Ion source is the Primary Component of sample ionization technology.
At present, there are many ion source, such as electron impact ion source (EI), chemical ionization source (CI), field-ionization/field
Desorption ionization source (FI/FD), fast atom bombardment source (FAB), electron spray ionisation source (ESI), laser desorption source (LD), atmospheric pressure
Learn ionization source (APCI) etc..For these ion sources, sample must pass through cumbersome pretreatment before ionization, therefore, these
The common deficiency of ion source is：Sample directly the attached ionization of fast desorption namely can not cannot realize the continuous, real of target components
When monitoring and high throughput analysis or imaging analysis.
In recent years, desorption electro-spray ionization (DESI), Direct Analysis in Real Time (DART) ionization and dielectric impedance are put
The appearance of electric (DBDI) ion source, these Ionization modes directly quick in the case where sample surfaces realize normal pressure can be analyzed, sample
Without pretreatment.These ion sources have deficiency, such as：
DESI ion sources make electron spray capillary front end that corona easily occur, it is necessary to high voltage power supply structure high-voltage electrostatic field,
High pressure, which also limits to develop into ion source, holds and directly human skin surface is made the lossless possibility quickly analyzed；Institute
The ionizing solvent and the gas of high flow rate used, it is not only of high cost but also certain pollution can be caused to environment.
DART ion sources eliminate solvent, but need the ionized gas of high-voltage electricity and high flow rate, and in order to obtain
Stable, efficient ionising effect is obtained, it is necessary to using electrode, right multi-electrode (high-field electrode, gate electrode, grounding electrode) design is again
It is miscellaneous, it should not realize the miniaturization of instrument.
DBDI ion sources can not realize the qualitative and quantitative analysis of the biological species sample such as amino acid, polypeptide；And mass spectral analysis
Noise it is higher, constrain further improving for Mass Spectrometer Method sensitivity.
The content of the invention
To solve the deficiency in above-mentioned prior art, the present invention provides a kind of ion sources, realize biological sample
Qualitative and quantitative analysis, and improve the sensitivity of mass spectral analysis.
The purpose of the present invention is what is be achieved through the following technical solutions：
A kind of ion source, the ion source include：
Insulation tube, the insulation tube both ends open；
First electrode, the first electrode are arranged on the outside of the insulation tube, and the first electrode has the first wiring
End；
Second electrode, the second electrode are arranged on the outside of the insulation tube, and in the extending direction of the insulation tube
On, first electrode, second electrode and grounding electrode are set gradually or second electrode is arranged on the inside of the insulation tube；Institute
Second electrode is stated with the second terminals；
Grounding electrode, the grounding electrode are arranged on the openend of the insulation tube.
According to above-mentioned ion source, it is preferable that the insulation tube has internal diametric reduction；The grounding electrode is arranged on institute
State the openend of internal diametric reduction side.
According to above-mentioned ion source, it is preferable that the first electrode and/second electrode is annular electrode.
According to above-mentioned ion source, it is preferable that the grounding electrode is annular electrode or needle electrode or sieve electrode.
The present invention also aims to provide a kind of ioning method, the qualitative and quantitative analysis of biological sample is realized,
And the sensitivity of mass spectral analysis is improved, which is achieved by the following technical programs：
Ioning method, the ioning method comprise the following steps：
(A1) sample to be tested is placed in the first openend of insulation tube；
(A2) alternating voltage is applied between first electrode and second electrode；The first electrode is arranged on the outer of the insulation tube
Portion, the second electrode are arranged on the outside of the insulation tube, and on the extending direction of the insulation tube, first electrode,
Two electrodes and grounding electrode are set gradually or second electrode is arranged on the inside of the insulation tube；
Carrier gas is passed through into insulation tube from the second openend of the insulation tube, generates plasma beam；
(A3) plasma beam forms ionized gas after the grounding electrode of first open end side is flowed out, described
Ionized gas ionizes the sample to be tested.
According to above-mentioned ioning method, it is preferable that the insulation tube has internal diametric reduction；The grounding electrode is set
In the openend of the internal diametric reduction side.
According to above-mentioned ioning method, it is preferable that the flow velocity of the carrier gas is 0.02-10L/min.
According to above-mentioned ioning method, it is preferable that the power of the alternating current be 5-30W, voltage 1-20kV, frequency
For 10-1000Hz.
According to above-mentioned ioning method, it is preferable that be arranged on the second electrode of the inside of the insulation tube as plate electricity
Pole.
Compared with prior art, the device have the advantages that being：
1. creatively make use of grounding electrode, for eliminating a large amount of electronics of ion source plasma beam, make amino acid,
The biological samples such as polypeptide realize soft ionization, and molecule peak is obtained in mass spectrum, realize the qualitative and quantitative analysis of biological species sample；
2. by grounding electrode, a large amount of electronics of ion source plasma beam can be eliminated, reduce electronics to object in environment
The ionization of matter reduces mass spectrum noise, improves detection sensitivity；
3. insulation tube has internal diametric reduction, designed instead of individual nozzle, it is simple in structure, reduce cost.
Description of the drawings
Referring to the drawings, the disclosure will be easier to understand.Skilled addressee readily understands that be：This
A little attached drawings are used only for the technical solution illustrated the present invention, and are not intended to and protection scope of the present invention is construed as limiting.
In figure：
Fig. 1 is the sectional view of according to embodiments of the present invention 1 ion source；
Fig. 2 is the sectional view of according to embodiments of the present invention 2 ion source；
Fig. 3 is the mass spectrogram of according to embodiments of the present invention 3 caffeine；
Fig. 4 is the mass spectrogram of according to embodiments of the present invention 4 melamine
Fig. 5 is the mass spectrogram of according to embodiments of the present invention 5 histidine.
Specific embodiment
Fig. 1-5 and following description describe the present invention optional embodiment to instruct how those skilled in the art implement
It is of the invention with reproducing.In order to instruct technical solution of the present invention, simplified or some conventional aspects be omitted.Those skilled in the art
It should be appreciated that modification or replacement from these embodiments will within the scope of the invention.Those skilled in the art should understand that
Following characteristics can combine to form multiple modifications of the present invention in various ways.As a result, the invention is not limited in it is following can
Embodiment is selected, and is only limited by the claims and their equivalents.
Embodiment 1：
Fig. 1 schematically illustrates the sectional view of the ion source of the embodiment of the present invention 1, as shown in Figure 1, the ion source bag
It includes：
Insulation tube 11, the insulation tube both ends open；
First electrode 21, the first electrode are arranged on the outside of the insulation tube, and the first electrode has first to connect
Line end；Preferably, the first electrode is annular electrode；
Second electrode 22, the second electrode are arranged on the inside of the insulation tube, and the second electrode has second to connect
Line end；It is preferable to use plate electrodes for the second electrode；Apply alternating current between the first terminals and the second terminals；
Grounding electrode 31, the grounding electrode are arranged on the openend of the insulation tube.Preferably, the grounding electrode is
Annular electrode or needle electrode or sieve electrode.
In order to reduce the complexity of structure, it is preferable that the insulation tube has internal diametric reduction；The grounding electrode is set
In the openend of 12 side of internal diametric reduction, so as to eliminate individual nozzle.
The ioning method of the embodiment of the present invention, the ioning method comprise the following steps：
(A1) sample to be tested is placed in the first openend of insulation tube；
(A2) alternating voltage is applied between first electrode and second electrode；The first electrode is arranged on the outer of the insulation tube
Portion, the second electrode are arranged on the inside of the insulation tube；
Carrier gas is passed through into insulation tube from the second openend of the insulation tube, generates plasma beam；Preferably, it is described
The flow velocity of carrier gas is 0.02-10L/min；The power of the alternating current is 5-30W, voltage 1-20kV, frequency 10-
1000Hz；
(A3) plasma beam forms ionized gas after the grounding electrode of first open end side is flowed out, described
Ionized gas ionizes the sample to be tested.
In order to reduce the complexity of structure, it is preferable that the insulation tube has internal diametric reduction；The grounding electrode is set
In the openend of 12 side of internal diametric reduction, so as to eliminate individual nozzle.
Embodiment 2：
Fig. 2 schematically illustrates the sectional view of the ion source of the embodiment of the present invention 2, as shown in Fig. 2, the ion source bag
It includes：
Insulation tube 11, the insulation tube both ends open；Insulating sleeve is using the insulating materials such as ceramics, quartz, glass；
First electrode 21, the first electrode are arranged on the outside of the insulation tube, and the first electrode has first to connect
Line end；Preferably, the first electrode is annular electrode；
Second electrode 22, the second electrode are arranged on the outside of the insulation tube, and in the extension side of the insulation tube
Upwards, the first electrode, second electrode and grounding electrode are set gradually, and the second electrode has the second terminals；It is described
It is preferable to use annular electrodes for second electrode；Apply alternating current between the first terminals and the second terminals；
Grounding electrode 31, the grounding electrode are arranged on the openend of the insulation tube.Preferably, the grounding electrode is
Annular electrode or needle electrode or sieve electrode.
In order to reduce the complexity of structure, it is preferable that the insulation tube has internal diametric reduction；The grounding electrode is set
In the openend of 12 side of internal diametric reduction, so as to eliminate individual nozzle.
The ioning method of the embodiment of the present invention, the ioning method comprise the following steps：
(A1) sample to be tested is placed in the first openend of insulation tube；
(A2) alternating voltage is applied between first electrode and second electrode；The first electrode is arranged on the outer of the insulation tube
Portion, the second electrode are arranged on the outside of the insulation tube, and on the extending direction of the insulation tube, first electricity
Pole, second electrode and grounding electrode are set gradually；
Carrier gas is passed through into insulation tube from the second openend of the insulation tube, generates plasma beam；Preferably, it is described
The flow velocity of carrier gas is 0.02-10L/min；The power of the alternating current is 5-30W, voltage 1-20kV, frequency 10-
1000Hz；
(A3) plasma beam forms ionized gas after the grounding electrode of first open end side is flowed out, described
Ionized gas ionizes the sample to be tested.
In order to reduce the complexity of structure, it is preferable that the insulation tube has internal diametric reduction；The grounding electrode is set
In the openend of 12 side of internal diametric reduction, so as to eliminate individual nozzle.
Embodiment 3：
Application examples of according to embodiments of the present invention 1 ion source and ioning method in caffeine detection.
In the application examples, 2 millimeters of dielectric thickness of pipe wall, 4 millimeters of internal diameter；Insulated dielectric tube has internal diametric reduction,
Contraction section internal diameter is 2 millimeters, and grounding electrode is arranged on the openend of the internal diametric reduction side；AC high voltage source power is
7W, maximum voltage 5kV, frequency 50Hz；The caffeine standards sample (concentration 100ppb) that 100uL is dissolved in methanol is taken to be placed in ion source
Sample area, carrier gas are helium, gas flow 1.2L/min, 250 DEG C of heating temperature.In mass spectral results obtain caffeine hydrogenation from
Sub- peak [M+H]+, m/z values are 195.18, and mass spectrogram is as shown in Figure 3.
Embodiment 4：
Application examples of according to embodiments of the present invention 2 ion source and ioning method in melamine detection.
In the application examples, 1 millimeter of dielectric thickness of pipe wall, 2 millimeters of internal diameter；Insulated dielectric tube has internal diametric reduction,
Contraction section internal diameter is 1 millimeter, and grounding electrode is arranged on the openend of the internal diametric reduction side；AC high voltage source power is
7W, maximum voltage 5kV, frequency 50Hz；The melamine standard sample (concentration 250ppb) that 100uL is dissolved in methanol is taken to be placed in ion
Source sample area, carrier gas are helium, flow 2.0L/min, 500 DEG C of heating temperature.The hydrogenation of melamine is obtained in mass spectral results
Quasi-molecular ions [M+H]+, m/z values are 127.09, and mass spectrogram is as shown in Figure 4.
Embodiment 5：
Application examples of according to embodiments of the present invention 1 ion source and ioning method in histidine detection.
In the application examples, 2 millimeters of dielectric thickness of pipe wall, 4 millimeters of internal diameter；Insulated dielectric tube has internal diametric reduction,
Contraction section internal diameter is 2 millimeters, and grounding electrode is arranged on the openend of the internal diametric reduction side；AC high voltage source power is
20W, maximum voltage 20kV, frequency 50Hz；The histidine samples (concentration 0.5ppm) that 100uL is dissolved in methanol-water is taken to be placed in ion source
Sample area, carrier gas are helium, flow 1.2L/min, 250 DEG C of heating temperature.The hydrogenation of histidine molecule is obtained in mass spectral results
Quasi-molecular ions [M+H]+, m/z values are 156.4, and mass spectrogram is as shown in Figure 5.
Claims (9)
1. a kind of ion source, it is characterised in that：The ion source includes：
Insulation tube, the insulation tube both ends open；
First electrode, the first electrode are arranged on the outside of the insulation tube, and the first electrode has the first terminals；
Second electrode, the second electrode are arranged on the outside of the insulation tube, and on the extending direction of the insulation tube, the
One electrode, second electrode and grounding electrode are set gradually or second electrode is arranged on the inside of the insulation tube；Described second
Electrode has the second terminals；
Grounding electrode, the grounding electrode are arranged on the openend of the insulation tube.
2. ion source according to claim 1, it is characterised in that：The insulation tube has internal diametric reduction；The ground connection
Electrode is arranged on the openend of the internal diametric reduction side.
3. ion source according to claim 1, it is characterised in that：The first electrode and/or second electrode are annular electros
Pole.
4. ion source according to claim 1, it is characterised in that：The grounding electrode be annular electrode or needle electrode or
Sieve electrode.
5. ioning method, the ioning method comprises the following steps：
(A1) sample to be tested is placed in the first openend of insulation tube；
(A2) alternating voltage is applied between first electrode and second electrode；The first electrode is arranged on the outside of the insulation tube,
The second electrode is arranged on the outside of the insulation tube, and on the extending direction of the insulation tube, first electrode, the second electricity
Pole and grounding electrode are set gradually or second electrode is arranged on the inside of the insulation tube；
Carrier gas is passed through into insulation tube from the second openend of the insulation tube, generates plasma beam；
(A3) plasma beam forms ionized gas, the ion after the grounding electrode of first open end side is flowed out
Gas ionizes the sample to be tested.
6. ioning method according to claim 5, it is characterised in that：The insulation tube has internal diametric reduction；It is described
Grounding electrode is arranged on the first openend of the internal diametric reduction side.
7. ioning method according to claim 5, it is characterised in that：The flow velocity of the carrier gas is 0.02-10L/min.
8. ioning method according to claim 5, it is characterised in that：The power of the alternating current is 5-30W, and voltage is
1-20kV, frequency 10-1000Hz.
9. ioning method according to claim 5, it is characterised in that：It is arranged on the second electricity of the inside of the insulation tube
Extremely plate electrode.
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| CN201510599393.7A CN105355535B (en) | 2015-09-18 | 2015-09-18 | Ion source and ioning method |
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|---|---|---|---|
| CN201510599393.7A CN105355535B (en) | 2015-09-18 | 2015-09-18 | Ion source and ioning method |
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| CN105355535B true CN105355535B (en) | 2018-05-22 |
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| CN106898538B (en) * | 2017-03-31 | 2019-10-22 | 广东联捷生物科技有限公司 | Mass ion source |
| CN110010444B (en) * | 2019-03-29 | 2024-02-09 | 广州安诺科技股份有限公司 | Ion source of multi-electric-field mass spectrometer |
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| WO2009157312A1 (en) * | 2008-06-27 | 2009-12-30 | 国立大学法人山梨大学 | Ionization analysis method and device |
| CN101510493B (en) * | 2008-11-18 | 2010-06-02 | 清华大学 | Method and ion source for direct ionization of sample by low-temperature plasma |
| CN101770924B (en) * | 2008-12-30 | 2013-07-03 | 株式会社岛津制作所 | Desorbing ionization device |
| CN102938361B (en) * | 2011-08-15 | 2016-03-16 | 中国科学院大连化学物理研究所 | A kind of mass spectrum ionization source of highly sensitive on-line analysis explosive and application thereof |
| CN103094050B (en) * | 2013-01-08 | 2016-03-23 | 中国科学院化学研究所 | A kind of sensitive glow discharge direct ionization method and device thereof |
| CN103545165B (en) * | 2013-10-29 | 2016-03-30 | 清华大学 | A kind of mass ions method based on cold-plasma jet and ion source device |
| CN104064429B (en) * | 2014-07-16 | 2017-02-22 | 昆山禾信质谱技术有限公司 | Mass spectrum ionization source |
| CN204991648U (en) * | 2015-09-18 | 2016-01-20 | 宁波华仪宁创智能科技有限公司 | Ion source |
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Address after: West side of 1st floor, 1st floor, Building A, No. 288 Jingu Middle Road (East), Yinzhou District, Ningbo City, Zhejiang Province, 315000 Patentee after: CHINA INNOVATION INSTRUMENT Co.,Ltd. Country or region after: China Address before: Room 304-311, Building D, Kexin Building, No. 655 Bachelor's Road, Yinzhou District, Ningbo City, Zhejiang Province, 310012 Patentee before: CHINA INNOVATION INSTRUMENT Co.,Ltd. Country or region before: China |