CN103871824A - Electrospray ion source ion migration tube and application thereof - Google Patents
Electrospray ion source ion migration tube and application thereof Download PDFInfo
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- CN103871824A CN103871824A CN201210538911.0A CN201210538911A CN103871824A CN 103871824 A CN103871824 A CN 103871824A CN 201210538911 A CN201210538911 A CN 201210538911A CN 103871824 A CN103871824 A CN 103871824A
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Abstract
The invention relates to an ion migration tube, one of the core devices in the ion mobility spectrometry, and particularly relates to an electrospray ion source ion migration tube. An electrospray ion source is used as a sample ionization source of the ion migration tube, and direct injection analysis of liquid samples can be realized. The novel ion migration tube overcomes the defect that a traditional beta radiation ion source ion migration tube can only detect volatile and semi-volatile samples, and the range of samples which can be detected by the use of the ion mobility spectrometry is extended to the field of thermally-instable and non-volatile analytes and biological macromolecules.
Description
Technical field
The present invention relates to Instrumental Analysis field, be specially a kind of transference tube of ion mobility spectrometry.
Background knowledge
Traditional transference tube adopts radioactivity
63ni ionization source, such transference tube general analysis gaseous sample, for the sample of half volatilization or fixedness, needs to use thermal analysis apparatus to gasify in advance to be just sent to transference tube inside and detects.This limitation, is difficult to use in traditional transference tube non-volatile thermal instability sample and large biological molecule sample is detected.
Electron spray phenomenon is used as ionization source and originates from the thirties in 20th century, and in late 1970s, electron spray ionisation technology starts to be used to field of mass spectrometry and is used for biological sample to study.Electron spray ionisation technology can direct ionization fluid sample, and analyte ions is converted into gaseous ion for follow-up compartment analysis.By this technology, for ion mobility spectrometry, the expanded range that Ion mobility spectrometry can be able to be detected to sample is to thermal instability, non-volatile analyte and large biological molecule field.
Patent content
Object of the present invention: a kind of electron spray ionisation transference tube is provided and shows its application in fluid sample analysis, expand the range of application of Ion mobility spectrometry.
For realizing above-mentioned object, the technical solution used in the present invention is:
A kind of electric spray ion source transference tube, comprises ion gate, ion migration area, is provided with an electric spray ion source in ion gate left side, and ion gate right side is ion migration area; Electric spray ion source is made up of electrode capillary pipe spray pin, focusing electrode and electron spray;
Centered by focusing electrode, locate to be provided with the Metal Flake electrode of through hole, the right lateral surface of focusing electrode is the spherical interior surface of indent, central through hole is positioned at the center of spherical interior surface, electron spray is ring electrode to electrode, electron spray is placed in focusing electrode right side to electrode, between to electrode and focusing electrode, be provided with ying-shaped insulator, be placed with fog-spray nozzle fixed mount in focusing electrode left side, the tip of capillary pipe spray pin is passed focusing electrode central through hole and is fixed on fog-spray nozzle fixed mount through permanent joint; Focusing electrode central through hole is with coaxial to electrode; Be connected with conduction two away from the capillary pipe spray pin end of capillary pipe spray needle tip logical, the two logical other ends that conduct electricity are connected with sample introduction capillary, conduction two is logical, focusing electrode is all directly connected with external power source electrode with electron spray, wherein electron spray is to added voltage on electrode lower than added voltage on focusing electrode, and the logical added voltage of conduction two is not less than added voltage on focusing electrode;
Between electron spray is to electrode and ion gate, be provided with desolvation cavity; Desolvation cavity is made up of alternately coaxial superimposed ring electrode and ying-shaped insulator, and the cavity at ring electrode and ying-shaped insulator middle part is desolvation cavity.Desolvation cavity and ion migration area lay respectively at the left and right sides of ion gate;
Ion migration area is made up of alternately coaxial superimposed ring electrode and ying-shaped insulator, and the cavity at ring electrode and ying-shaped insulator middle part is ion migration area; Electron spray is coaxial to electrode, desolvation cavity, ion gate, ion migration area.Be provided with air inlet in ion migration area away from ion gate one end, in electric spray ion source, electrode one side is provided with to gas outlet away from the electron spray of ion gate.The all parts junction of transference tube is all used sealing O type circle to seal, and guarantees transference tube air-tightness.
Advantage of the present invention is:
Electron spray ionisation transference tube can be realized the direct injected of fluid sample, electron spray solvent flow rate is restricted to and receives the magnitude of Liter Per Minute, can realize the abundant desolvation to ion that electron spray produces, guarantee that transference tube still has high resolution capability at lower temperature, expand thermal instability, non-volatile analyte and large biological molecule field to thereby Ion mobility spectrometry can be detected to sample.
Accompanying drawing explanation:
Fig. 1. electron spray ionisation transference tube design diagram;
Fig. 2. the From Spectral Signal while using this migration tube to detect triethylamine;
Fig. 3. the From Spectral Signal while using this migration tube to detect methamphetamine;
Fig. 4. use this migration tube to detect the dynamic response curve of methamphetamine.
Embodiment:
The present invention use electric spray ion source transference tube as shown in fig. 1,
A kind of electric spray ion source transference tube, comprises ion gate 4, ion migration area 3; Be provided with an electric spray ion source 1 in ion gate 4 left sides, ion gate 4 right sides are ion migration area 3; Electric spray ion source 1 is made up of electrode 1-6 capillary pipe spray pin 1-3, focusing electrode 1-5 and electron spray;
Centered by focusing electrode 1-5, locate to be provided with the Metal Flake electrode of through hole, the right lateral surface of focusing electrode 1-5 is the spherical interior surface of indent, central through hole is positioned at the center of spherical interior surface, electron spray is ring electrode to electrode 1-6, electron spray is placed in focusing electrode 1-5 right side to electrode 1-6, between to electrode 1-6 and focusing electrode 1-5, be provided with ying-shaped insulator, be placed with fog-spray nozzle fixed mount 1-4 in focusing electrode 1-5 left side, the tip of capillary pipe spray pin 1-3 is passed focusing electrode 1-5 central through hole and is fixed on fog-spray nozzle fixed mount 1-4 through permanent joint 1-7; Focusing electrode 1-5 central through hole is with coaxial to electrode 1-6;
Be connected with the logical 1-2 of conduction two away from the capillary pipe spray pin 1-3 end at capillary pipe spray pin 1-3 tip, the other end of conduction two logical 1-2 is connected with sample introduction capillary 1-1, conduction two logical 1-2, focusing electrode 1-5 are all directly connected with external power source electrode 1-6 with electron spray, wherein electron spray is to the upper added voltage of electrode 1-6 lower than the upper added voltage 500V of focusing electrode 1-5, and the upper added voltage of the logical 1-2 of conduction two is higher than the upper added voltage 1500V of focusing electrode 1-5;
Between electron spray is to electrode 1-6 and ion gate 4, be provided with desolvation cavity 2; Desolvation cavity 2 is made up of alternately coaxial superimposed ring electrode and ying-shaped insulator, and the cavity at ring electrode and ying-shaped insulator middle part is desolvation cavity 2.Desolvation cavity 2 and ion migration area 3 lay respectively at the left and right sides of ion gate 4;
Be provided with air inlet 6 in ion migration area 3 away from ion gate 4 one end, in electric spray ion source 1, electrode 1-6 mono-side is provided with to gas outlet 5 away from the electron spray of ion gate 4; In experimentation, make-up gas enters from air inlet 6, flows out from gas outlet 5, and testing liquid sample is pushed into electron spray ionisation transference tube by stepping injector from sample introduction capillary.
In addition,, in order to guarantee the air-tightness of transference tube, between each several part, all use sealing O type circle to seal.
In Fig. 2, show that above-mentioned transference tube is detecting the ion mobility spectrometry figure forming while using 80% methanol-water as the triethylamine solution of solvent configuration.The flow velocity of solution in capillary pipe spray pin is 120nl/min.The signal peak that transit time is 14.88ms as we can see from the figure, this peak is the peak that triethylamine forms.In addition, the peak that the signal peak that transit time is 13.65ms forms for methanol-water solvent.This result has tentatively been shown the ability of the electron spray ionisation transference tube in the present invention aspect detection liquid phase sample.
In Fig. 3, show the ion mobility spectrometry figure that above-mentioned transference tube obtains in the time detecting methamphetamine.Methamphetamine is dissolved in 80% methanol aqueous solution, and the flow velocity of solution in capillary pipe spray pin is 120nl/min.Except having the solvent peak of 13.62ms, methamphetamine has formed the single quasi-molecular ions of oneself at 18.25ms place as we can see from the figure.In Fig. 4, shown the dynamic response trend that uses this transference tube to detect methamphetamine in 80% methanol-water, can see concentration range be 60ng/ml in the scope of 1000ng/ml, have good linear response.This result has been shown the potential ability of this transference tube analyte concentration in to fluid sample aspect quantitative.
Claims (4)
1. an electric spray ion source transference tube, comprises ion gate (4), ion migration area (3), it is characterized in that:
Be provided with an electric spray ion source (1) in ion gate (4) left side, ion gate (4) right side is ion migration area (3);
Electric spray ion source (1) is made up of electrode (1-6) capillary pipe spray pin (1-3), focusing electrode (1-5) and electron spray;
Centered by focusing electrode (1-5), locate to be provided with the Metal Flake electrode of through hole, the spherical interior surface that the right lateral surface of focusing electrode (1-5) is indent, central through hole is positioned at the center of spherical interior surface, electron spray is ring electrode to electrode (1-6), electron spray is placed in focusing electrode (1-5) right side to electrode (1-6), between to electrode (1-6) and focusing electrode (1-5), be provided with ying-shaped insulator, be placed with fog-spray nozzle fixed mount (1-4) in focusing electrode (1-5) left side, the tip of capillary pipe spray pin (1-3) is passed focusing electrode (1-5) central through hole and is fixed on fog-spray nozzle fixed mount (1-4) through permanent joint (1-7), focusing electrode (1-5) central through hole is with coaxial to electrode (1-6),
Capillary pipe spray pin (1-3) end most advanced and sophisticated away from capillary pipe spray pin (1-3) is connected with conduction two logical (1-2), the other end of conduction two logical (1-2) is connected with sample introduction capillary (1-1), conduction two logical (1-2), focusing electrode (1-5) are all directly connected with external power source electrode (1-6) with electron spray, wherein electron spray is to the upper added voltage of electrode (1-6) lower than the upper added voltage of focusing electrode (1-5), and the upper added voltage of conduction two logical (1-2) is not less than the upper added voltage of focusing electrode (1-5);
Between electron spray is to electrode (1-6) and ion gate (4), be provided with desolvation cavity (2);
Desolvation cavity (2) is made up of alternately coaxial superimposed ring electrode and ying-shaped insulator, and the cavity at ring electrode and ying-shaped insulator middle part is desolvation cavity (2).
2. transference tube as claimed in claim 1, is characterized in that:
Desolvation cavity (2) and ion migration area (3) lay respectively at the left and right sides of ion gate (4);
Ion migration area (3) is made up of alternately coaxial superimposed ring electrode and ying-shaped insulator, and the cavity at ring electrode and ying-shaped insulator middle part is ion migration area (3); Electron spray to electrode (1-6), desolvation cavity (2), ion gate (4), ion migration area (3) coaxially.
3. transference tube as claimed in claim 1, is characterized in that:
Be provided with air inlet (6) in ion migration area (3) away from ion gate (4) one end, in electric spray ion source (1), electrode (1-6) side is provided with to gas outlet (5) away from the electron spray of ion gate (4).
4. transference tube as claimed in claim 1, is characterized in that:
The all parts junction of transference tube is all used sealing O type circle to seal, and guarantees transference tube air-tightness.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210538911.0A CN103871824A (en) | 2012-12-12 | 2012-12-12 | Electrospray ion source ion migration tube and application thereof |
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| CN201210538911.0A CN103871824A (en) | 2012-12-12 | 2012-12-12 | Electrospray ion source ion migration tube and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792854A (en) * | 2015-03-31 | 2015-07-22 | 广州禾信分析仪器有限公司 | System and method for real-time and on-line rapid mass spectrometry analysis on chemical compositions of sub-micron aerosol |
| CN105047519A (en) * | 2015-08-20 | 2015-11-11 | 中国检验检疫科学研究院 | In-situ spraying ionization device |
| CN105181784A (en) * | 2015-08-20 | 2015-12-23 | 中国检验检疫科学研究院 | Method for rapidly screening 40 prohibited antibiotics in cosmetics |
| CN106653558A (en) * | 2017-03-20 | 2017-05-10 | 天津大学 | Proton transfer reaction ion source for ion migration spectrum |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090078861A1 (en) * | 2003-10-14 | 2009-03-26 | Hill Jr Herbert Henderson | Ion Mobility Spectrometry Method and Apparatus |
| US7960711B1 (en) * | 2007-01-22 | 2011-06-14 | Chem-Space Associates, Inc. | Field-free electrospray nebulizer |
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2012
- 2012-12-12 CN CN201210538911.0A patent/CN103871824A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090078861A1 (en) * | 2003-10-14 | 2009-03-26 | Hill Jr Herbert Henderson | Ion Mobility Spectrometry Method and Apparatus |
| US7960711B1 (en) * | 2007-01-22 | 2011-06-14 | Chem-Space Associates, Inc. | Field-free electrospray nebulizer |
Non-Patent Citations (4)
| Title |
|---|
| DOUG WITTMER ER AL.: "Electrospray Ionization Ion Mobility Spectrometry", 《ANALYTICAL CHEMISTRY》 * |
| M.T. JAFARI: "Improved design for high resolution electrospray", 《TALANTA》 * |
| N. ARABZADEH ET AL.: "Pneumatically assisted electrospray-ion mobility spectrometry for quantitative analysis of intact proteins", 《TALANTA》 * |
| YONG HONG CHEN ET AL: "Thermal effects on electrospray ionization ion mobility spectrometry", 《INTERNATIONAL JOURNAL OF MASS SPECTROMETRY AND ION PROCESSES》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792854A (en) * | 2015-03-31 | 2015-07-22 | 广州禾信分析仪器有限公司 | System and method for real-time and on-line rapid mass spectrometry analysis on chemical compositions of sub-micron aerosol |
| CN105047519A (en) * | 2015-08-20 | 2015-11-11 | 中国检验检疫科学研究院 | In-situ spraying ionization device |
| CN105181784A (en) * | 2015-08-20 | 2015-12-23 | 中国检验检疫科学研究院 | Method for rapidly screening 40 prohibited antibiotics in cosmetics |
| CN105047519B (en) * | 2015-08-20 | 2017-03-22 | 中国检验检疫科学研究院 | In-situ spraying ionization device |
| CN106653558A (en) * | 2017-03-20 | 2017-05-10 | 天津大学 | Proton transfer reaction ion source for ion migration spectrum |
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Application publication date: 20140618 |