CN112951699B - Separation method of ion mobility spectrometry overlapping peaks - Google Patents

Separation method of ion mobility spectrometry overlapping peaks Download PDF

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Publication number
CN112951699B
CN112951699B CN201911249555.9A CN201911249555A CN112951699B CN 112951699 B CN112951699 B CN 112951699B CN 201911249555 A CN201911249555 A CN 201911249555A CN 112951699 B CN112951699 B CN 112951699B
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ion
metal ring
migration
potential
metal
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CN112951699A (en
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李海洋
陈红
厉梅
陈创
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Dalian Institute of Chemical Physics of CAS
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Dalian Institute of Chemical Physics of CAS
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J49/00Particle spectrometers or separator tubes
    • H01J49/0027Methods for using particle spectrometers
    • H01J49/0031Step by step routines describing the use of the apparatus
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/622Ion mobility spectrometry

Abstract

The invention discloses a separation method of ion mobility spectrometry overlapping peaks. The ion migration tube is close to one end of the detection electrode, and is sequentially provided with a first metal ring, a second metal ring, a third metal ring and a fourth metal ring which are parallel to each other, insulated and coaxial along the ion migration direction. The ions implanted into the migration region migrate toward the detection electrode under the action of the electric field in the migration region. When the back edge of the ion cluster with high mobility reaches the position of the second metal ring, the potential on the second metal ring is increased, the potential on the third metal ring is reduced, an electric potential barrier and an electric potential well are formed at the positions of the second metal ring and the third metal ring respectively, ions with high mobility speed enter the electric potential well, ions with low mobility speed are blocked at the electric potential barrier, so that adjacent ion clusters are separated, then the potentials on the second metal ring and the third metal ring are reduced, the electric field is recovered uniformly, and the separated ion clusters continue to migrate to the detection electrode.

Description

Separation method of ion mobility spectrometry overlapping peaks
Technical Field
The invention relates to a separation method of ion mobility spectrometry overlapping peaks.
Background
The ion mobility spectrometry is widely applied to detection of chemical toxicants, explosives, drugs and the like due to the advantages of high analysis speed, high sensitivity, small volume, simple operation and the like. In addition, ion mobility spectrometry can separate isomers, and is often used in combination with mass spectrometry to detect biological samples. In recent years, the application of ion mobility spectrometry has been advanced to the field of medical diagnosis, such as the detection of small molecule metabolites in exhaled breath, anesthetics in blood, and the like. However, the ion mobility spectrum has low resolution, the resolution of the current commercial mobility tube is generally not more than 60, and when a complex sample is detected or the current commercial mobility tube is used for field detection, overlapping peaks are easily generated, so that interference is brought to field analysis, qualitative and quantitative analysis. The space focusing ion gate component and the space focusing ion migration tube, which are applied by the institute of chemistry and physics of the college of China academy of sciences in 2012, realize ion compression distributed in the direction of an ion axis by changing the structure and space distribution of an ion gate and applying pulse acceleration voltage to a migration region, thereby improving the resolution and peak capacity of an ion migration spectrum. If the ions with high speed are accelerated by the pulse acceleration voltage and blocked by the pulse deceleration voltage in the ion cluster migration process, the separation of the overlapped peaks is facilitated.
Disclosure of Invention
The invention aims to provide a method for separating overlapped peaks of a mobility spectrum.
In order to realize the purpose, the invention adopts the technical scheme that:
a first metal ring R1, an insulating metal ring R2, a metal ring R3 and a metal ring R4 which are mutually parallel, insulated, equally spaced and coaxial are sequentially arranged at one end of an ion migration region, which is close to a detection electrode, of the ion migration tube along the ion migration direction; the distance between adjacent metal rings in the four metal rings is not less than (greater than or equal to) the thickness of ion clusters injected into the migration zone when the ion gate is opened; the four metal rings and other conducting rings on the migration pipe are parallel, coaxial and arranged in an insulating way. Voltages are respectively applied to the four metal rings, the same potential difference is formed between the adjacent metal rings, and positive ions or negative ions injected into the migration area migrate towards the detection electrode; when the back edge of the ion cluster with high moving speed in the direction of the detection electrode reaches the position of the second metal ring R2, the positive potential of R2 is increased in a positive ion mode, the positive potential of R3 is reduced at the same time, the negative potential of R2 is reduced in a negative ion mode, the negative potential of R3 is increased at the same time, so that the potential difference between the second metal ring and the third metal ring is increased, potential barriers and potential wells are formed at the positions of the second metal ring and the third metal ring respectively, ions with high moving speed enter the potential wells, ion clusters with low moving speed are blocked at the potential barriers, and intersecting (partially overlapping) or adjacent ion clusters are separated,
the ion transfer tube is a hollow cylindrical cavity formed by coaxially stacking a plurality of conducting rings and insulating rings. An ion source of an ion generating device is arranged at one end of the cavity, an ion detecting electrode is arranged at the other end of the cavity, an ion gate is arranged in the cavity, and the migration tube is divided into two parts, wherein a reaction area is arranged between the ion source and the ion gate, and a migration area is arranged between the ion gate and the detecting electrode. And applying certain voltage to each conductive ring of the migration tube, so that positive ions or negative ions generated by the ion source can migrate to the detection electrode when the ion door is opened.
The invention has the advantages that:
on the premise of not reducing sensitivity, the overlapping peaks of the migration spectrum can be separated, and the qualitative and quantitative accuracy of the migration spectrum can be improved.
Drawings
Fig. 1 is a schematic view of an ion mobility tube of the present invention. Wherein (1) the ion source, (2) the conductive ring, (3) the ion gate, (4) R1, (5) R2, (6) R3, (7) R4, (8) the detection electrode
Fig. 2 is a schematic diagram of the potential change and ion cluster separation process involved in the present invention. Wherein (a) is the potential and ion cluster state at the moment before the potential change, (b) is the potential and ion cluster state at the moment after the potential change, (c) is the potential and ion cluster state at the moment before the potential reduction, and (d) is the potential and ion cluster state at the moment after the potential reduction
Fig. 3 migration profiles of methadone obtained before and after using the process of the present invention in example 1.
Detailed Description
Referring to fig. 1, a schematic diagram of an ion mobility tube according to the present invention is shown, and fig. 2 is a schematic diagram of a potential change and ion cluster separation process according to the present invention.
The migration pipe is a hollow cylindrical cavity formed by coaxially stacking a plurality of conducting rings and insulating rings, the length of the cavity is 100mm, the inner diameter of the cavity is 22mm, the thickness of each conducting ring is 3.5mm, and the thickness of each insulating ring is 1.5 mm. The ion source of the ion generating device is arranged at one end of the cavity, the ion detecting electrode is arranged at the other end of the cavity, the BN type ion gate is arranged in the cavity, and the migration tube is divided into two parts, wherein a reaction zone is arranged between the ion source and the ion gate, the length of the reaction zone is 25mm, a migration zone is arranged between the ion gate and the detecting electrode, and the length of the migration zone is 75 mm. In the migration area, four metal rings R1, R2, R3 and R4 which are parallel to each other, insulated and coaxial are sequentially arranged along the axial direction of the migration pipe, the thickness of each metal ring is 0.1mm, the inner diameter of each metal ring is 14mm, the outer diameter of each metal ring is 28mm, the distance between every two adjacent metal rings is 1mm, and the distance between the metal ring closest to the detection pole and the detection pole is 5 mm. The electrode on the right side of the Faraday cup is grounded, and certain voltages are respectively applied to other conducting rings and the four metal rings, so that a uniform electric field of 600V/cm can be formed in the migration tube. When the ion gate is opened, mixed ion clusters with the thickness not more than 1mm are injected into the migration region, the injected ion clusters continue to migrate to the detection electrode, and meanwhile, ions of different types in the ion clusters gradually start to be separated due to different migration rates. When the trailing edge of the ion cluster formed by the ion with the highest mobility reaches the position of R2, the potential of R2 is increased by 800V, and the potential of R2 is decreased by 800V, so that the potential barrier and the potential well are formed at the positions corresponding to R2 and R3, respectively. And after the stage is maintained for 300 mu s, reducing the potentials on the second metal ring and the third metal ring to restore the electric field to be uniform, and enabling the separated ion clusters to continuously migrate to the detection pole.
Example 1
And injecting a sample by a thermal desorption mode, and detecting 2ng of methadone by using an ion mobility spectrometry. The migration spectrum pairs of methadone obtained before and after using the present invention are shown in fig. 3. It can be seen that the separation of the two peaks of methadone becomes significantly better after the invention of the present method.

Claims (4)

1. A method for separating ion peaks having partially overlapping ion mobility spectra, comprising:
a first metal ring, a second metal ring, a third metal ring and a fourth metal ring are sequentially arranged at one end, close to a detection electrode, of a migration area of the ion migration tube along the ion migration direction, and the total number of the four metal rings is four, namely, the four metal rings are parallel, insulated, equally spaced and coaxial; voltages are respectively applied to the four metal rings, the same potential difference is formed between the adjacent metal rings, and positive ions or negative ions injected into the migration area migrate towards the detection electrode; when the back edge of the ion cluster moving fast towards the detection electrode reaches the position of the second metal ring, in a positive ion mode, the positive potential on the second metal ring is increased, and simultaneously the positive potential on the third metal ring is reduced, in a negative ion mode, the negative potential on the second metal ring is reduced, and simultaneously the negative potential on the third metal ring is increased, so that the potential difference between the second metal ring and the third metal ring is increased, potential barriers and potential wells are respectively formed at the positions of the second metal ring and the third metal ring, ions with fast migration speed enter the potential wells, the ion cluster with slow migration speed is blocked at the potential barriers, so that the partially overlapped or adjacent ion clusters are separated, then the potentials on the second metal ring and the third metal ring are reduced, so that the electric field is recovered to be uniform, and the separated ion cluster continuously migrates towards the detection electrode.
2. The method of claim 1, wherein:
the distance between adjacent metal rings in the four metal rings is not less than the thickness of ion clusters injected into the migration region when the ion gate is opened; the four metal rings and other conducting rings on the migration pipe are parallel, coaxial and arranged in an insulating way.
3. The method of claim 1, wherein:
when the ion cluster with high migration speed completely enters the potential well, the potential on the second and third metal rings is reduced to reduce the ion loss.
4. The method of claim 1, wherein:
the ion migration tube is a hollow cylindrical cavity formed by coaxially stacking a plurality of conducting rings and insulating rings; an ion source of an ion generating device is arranged at one end of the cavity, an ion detecting electrode is arranged at the other end of the cavity, an ion gate is arranged in the cavity, and the migration tube is divided into two parts, wherein a reaction area is arranged between the ion source and the ion gate, and a migration area is arranged between the ion gate and the detecting electrode; and applying certain voltage to each conductive ring of the migration tube, so that positive ions or negative ions generated by the ion source can migrate to the detection electrode when the ion door is opened.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4130810C1 (en) * 1991-09-17 1992-12-03 Bruker Saxonia Analytik Gmbh, O-7050 Leipzig, De
CN102568995A (en) * 2010-12-16 2012-07-11 塞莫费雪科学(不来梅)有限公司 Ion mobility spectrometry device and method
CN108091544A (en) * 2016-11-21 2018-05-29 中国科学院大连化学物理研究所 A kind of mass spectrum chemical ionization source based on differential mobility spectrum ion screening

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6586732B2 (en) * 2001-02-20 2003-07-01 Brigham Young University Atmospheric pressure ionization ion mobility spectrometry
CN101937824B (en) * 2009-06-30 2012-06-27 同方威视技术股份有限公司 Ion mobility spectrometry and detection method using same
JP6027239B2 (en) * 2012-07-31 2016-11-16 レコ コーポレイションLeco Corporation Ion mobility spectrometer with high throughput

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4130810C1 (en) * 1991-09-17 1992-12-03 Bruker Saxonia Analytik Gmbh, O-7050 Leipzig, De
CN102568995A (en) * 2010-12-16 2012-07-11 塞莫费雪科学(不来梅)有限公司 Ion mobility spectrometry device and method
CN108091544A (en) * 2016-11-21 2018-05-29 中国科学院大连化学物理研究所 A kind of mass spectrum chemical ionization source based on differential mobility spectrum ion screening

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
"飞行时间质谱的离子峰形模拟分析方法和应用";李海洋等;《质谱学报》;20060228;全文 *

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