CN105738463A - Method for rapidly analyzing composition of substance causing peak in ion mobility spectrometry - Google Patents
Method for rapidly analyzing composition of substance causing peak in ion mobility spectrometry Download PDFInfo
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- CN105738463A CN105738463A CN201610310817.8A CN201610310817A CN105738463A CN 105738463 A CN105738463 A CN 105738463A CN 201610310817 A CN201610310817 A CN 201610310817A CN 105738463 A CN105738463 A CN 105738463A
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- migration
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- ion mobility
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating 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
- G01N27/622—Ion mobility spectrometry
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- Spectroscopy & Molecular Physics (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for rapidly analyzing the composition of a substance causing a peak in ion mobility spectrometry. The method comprises the following steps of: (1) analyzing by using a device for ion mobility spectrometry-mass spectrometry; (2) establishing detection conditions; (3) achieving nature determination of the substance causing the peak in the ion mobility spectrometry according to mass spectrometric data. The method for rapidly analyzing the composition of the substance causing the peak in the ion mobility spectrometry, which is provided by the invention, is rapid in analysis and accurate and sensitive, the composition of components of peaks in the r ion mobility spectrometry can be accurately determined, and a good identification function can be achieved for analysis on substances which cannot be analyzed by only using the ion mobility spectrometry.
Description
Technical field
The invention belongs to analytical chemistry field, be specifically related to a kind of quickly analysis in ionic migration spectrometer and go out peak material composition
Detection method.
Background technology
Ion mobility spectrometry is applied to multiple detection field as a kind of simple detection technique of quick pretreatment method, main
The drugs of Security Inspection Office, explosive and other detection fields such as airport to be included, subway, customs.But the ion of commercialization at present
Migrate spectrum equipment and do not have the most outstanding sensitivity, and institute's detection compound cannot be carried out definite qualitative analysis,
This also results in and cannot provide measurement result accurately, it is impossible to accurately determine the kind of compound, and this also causes safety check process
Many false alarm problems of middle equipment.
As a example by the common actually detected process of drugs explosive, it is frequently run onto many insurmountable practical problems, such as:
Test paper catches after touch, can go out a Interference Peaks the strongest, again with other explosives at same migration time, Gu Huigan
Disturb and report to the police mistakenly as explosive；Easily there is multiple peak owing to being long placed in the problems such as change in purity and air in the drugs such as heroin,
The response intensity at peak is also different with sample difference, and just the generation that arranges on alarm threshold value and warning peak position affects；For another example examine
A period of time placed in atmosphere by survey sample introduction reagent paper can be to the detection generation interference of cocaine, all serious shadow of problem like this
Ring the accuracy of actually detected middle equipment Inspection result.Therefore in the urgent need to setting up a kind of efficient qualitative checking method.
The ion mobility spectrometry equipment of current domestic actual application have not been reported and has been combined with other equipment, run into due to
The highest wrong report problem caused of resolution, frequently with ameliorative way mainly include in gas circuit add adulterant generate other produce
Thing ion is used peak position change and is reached to detect smoothly, also by using the mode that other sample introduction reagent paper avoid interference instead.But
These methods the most fundamentally understand fully these problem Producing reason, by improve work that Detection results done the most usually by
In equipment or test environment difference, effect differs.So analyzing ion mobility spectrometry in the urgent need to a kind of qualitative equipment especially
Different migration peaks corresponding to the ionization process produced in operation and the ion of generation, and mass spectrum compensate for ion just
Migrate the spectrum inferior position at this part, and the ion migrating spectrum generation directly just can introduce in mass spectrum and detect, and also eliminates
Mass spectrographic ionization process, cuts out to combination.So combination mode also can inherently understand ion mobility spectrometry ionization mechanism and
The material composition that each peak is corresponding, thus preferably instruct our detection process.
Summary of the invention
Present invention aim to address that existing detection method cannot quick and precisely identify in ionic migration spectrometer and respectively go out peak
The limitation of material composition, and provide a kind of quick analysis ionic migration spectrometer to go out the detection method of peak material composition.
The present invention solves above technical problem by the following technical programs:
There is provided a kind of quick analysis ion migration to compose the detection method of peak material composition, specifically include following steps:
(1) ion mobility spectrometry-mass spectrometry device is used to be analyzed: detection sample is dissolved in ethanol or acetone solvent
In, mixing, standard substance are configured to 1 ~ 100ppm, and actual sample determines preparation sample concentration according to migrating spectrum real response intensity；
The sample drawing 1 ~ 10 microlitre during sample introduction imports in ion mobility spectrometry equipment by multiple input mode, gathers the matter of combination equipment
Spectrum and migration modal data；
(2) testing conditions of combined apparatus: ion mobility spectrometry uses positive negative mode to detect, under holotype, injector temperature
160 DEG C ~ 250 DEG C, migration tube temperature 160 DEG C ~ 200 DEG C；Under negative mode, injector temperature 100 DEG C ~ 200 DEG C, migration tube temperature
100℃~200℃；Electric field uses uniform electric field；Migrate gas and carrier gas all selects conventional drying air, gas circuit can add and mix
Miscellaneous dose.Mass spectrum all can use pattern of entirely sweeping, choice ion pattern (SIR) or the multiple-reaction monitoring pattern (MRM) of routine, needs
When obtaining fragment ion, with argon as collision gas；
(3) the different qualitative recognition migrating spectral peaks calculate with sxemiquantitative: about 1min passes through mass spectrometric data after completing analysis time
The migration peak migrating spectrum acquisition is carried out qualitative；By area normalization method, each material is carried out the mensuration of relative amount.
Above-mentioned steps (1) intermediate ion migrates ion produced by spectrum mobility spectrometer and is introduced directly in mass spectrum.
The qualitative material of institute is the material migrating and detecting to go out peak in spectrum in above-mentioned steps (1).
In above-mentioned steps (2), carrier gas and migration gas main constituent are all air.
The qualitative detection device used in above-mentioned steps (3) is mass spectrum.
In above-mentioned steps (3), the material composition identification at peak gone out to ion mobility spectrometry is according to mass spectrum institute in different modes
Obtain ion and fragment ion, by standard mass spectrometric data library searching and the checking of relevant criterion product, qualitative analysis go out from
In sub-mobility spectrometer, gone out peak is which kind of ion which kind of material produces.
It is in place of the progress of the present invention:
The present invention uses first and is introduced directly in mass spectrum by ion produced by ionic migration spectrometer, quickly analyzes ion migration
Spectrum respectively goes out the composition of peak material.Can accurately obtain the mass spectrometric data at each peak within the analysis time of 1 min, and then it is entered
Qualitative or the semi-quantitative analysis of row.Pre-treating method is simple, analyzes speed fast, qualitative accurately, with low cost.Can be used in commercial from
Such as a kind of compound that son runs into during migrating spectrum detection goes out multimodal, the interference of environmental disturbances thing causes false positive wrong report, phase
Analysis and the solution of the not equal difficult problem in peak is gone out with compound different solvents.
Accompanying drawing explanation
The ion migration spectrogram of the different conditions amphetamines sample of Fig. 1: embodiment 1.
Mass spectrum corresponding to amphetamines acetone soln in Fig. 2: embodiment 1.
Detailed description of the invention
Describe the present invention in detail below by specific embodiment, but the invention is not limited in these embodiments.
Embodiment 1:
(1) prepared by different conditions amphetamines sample
Sample 1: use amphetamines solid sample, using acetone as solvent, prepares 1000ppm amphetamines acetone soln, diluter
Release to 100ppm sample solution；Sample two: use amphetamines solid sample, with ethanol as solvent, prepares and is diluted to 100ppm
Sample solution；Sample three: amphetamines solid sample 0.5mg, after three kinds of sample preparations complete, preserves in-4 DEG C of refrigerators to be measured；
(2) ion mobility spectrometry-mass spectrometry analysis
Ion mobility spectrometry uses positive negative mode to detect, under holotype, and injector temperature 160 DEG C ~ 250 DEG C, migration tube temperature
160℃~200℃；Under negative mode, injector temperature 100 DEG C ~ 200 DEG C, migration tube temperature 100 DEG C ~ 200 DEG C；Electric field employing is even by force
Electric field；Migrate gas and carrier gas all selects conventional drying air, gas circuit can add adulterant.Mass spectrum all can use the complete of routine
Sweep pattern, choice ion pattern (SIR) or multiple-reaction monitoring pattern (MRM), when needing to obtain fragment ion, use argon conduct
Collision gas.Respectively take the variety classes amphetamines sample of 1 microlitre, drip to sampling testing paper sample introduction (solid is placed on reagent paper),
Gather data；
(3) the amphetamines qualitative analysis of samples to gained different conditions
About 1min carries out qualitative analysis by mass spectrometric data to migrating the migration peak that spectrum obtains after completing analysis time.
Data from table, under different conditions, to obtain the migration time at peak each for the ionization in migrating spectrum of amphetamines sample
Having difference, situation is complex, and the complete qualitative analysis of the present invention gone out the ion corresponding to each peak of every kind of sample and its
Compositing cause, can obtain the ion mobility spectrometry of different conditions sample and corresponding mass spectrometric data within 1min.Amphetamines
What solid, acetone soln, ethanol solution samples went out at migration time 8.46ms that peak is amphetamines adds hydrion [C9H13N+
H]+, and second migration peak that the acetone soln of amphetamines goes out at 9.14ms is that amphetamines adduction acetone molecules takes off one again
Molecular water adds the ion [C of a hydrogen again9H13N+C3H603-H20+H]+.So it is permissible by ion mobility spectrometry-mass spectrometry combination method
As qualitative migrate compose peak from molecular foundation.
Table 1 different conditions amphetamines sample determination result
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all in the spirit and principles in the present invention
Within, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (5)
1. the method that a quick analysis ion migration composes peak material composition, it is characterised in that specifically include following steps:
(1) ion mobility spectrometry-mass spectrometry device is used to be analyzed: detection sample is dissolved in ethanol or acetone solvent
In, mixing, standard substance are configured to 1 ~ 100ppm, and actual sample determines preparation sample concentration according to migrating spectrum real response intensity；
The sample drawing 1 ~ 10 microlitre during sample introduction imports in ion mobility spectrometry equipment by multiple input mode, gathers the matter of combination equipment
Spectrum and migration modal data；
(2) testing conditions of combined apparatus: ion mobility spectrometry uses positive negative mode to detect, under holotype, injector temperature
160 DEG C ~ 250 DEG C, migration tube temperature 160 DEG C ~ 200 DEG C；Under negative mode, injector temperature 100 DEG C ~ 200 DEG C, migration tube temperature
100℃~200℃；Electric field uses uniform electric field；Migrate gas and carrier gas all selects conventional drying air, gas circuit can add and mix
Miscellaneous dose；Mass spectrum all can use pattern of entirely sweeping, choice ion pattern (SIR) or the multiple-reaction monitoring pattern (MRM) of routine, needs
When obtaining fragment ion, with argon as collision gas；
(3) the different qualitative recognition migrating spectral peaks calculate with sxemiquantitative: about 1min passes through mass spectrometric data after completing analysis time
The migration peak migrating spectrum acquisition is carried out qualitative；By area normalization method, each material is carried out the mensuration of relative amount.
Method the most according to claim 1, it is characterised in that step (1) intermediate ion migrate spectrum mobility spectrometer produced from
Son is introduced directly in mass spectrum.
Method the most according to claim 1, it is characterised in that in step (1), the qualitative material of institute is permissible for detecting in migration spectrum
Go out the material at peak.
Method the most according to claim 1, it is characterised in that in step (2), carrier gas and migration gas main constituent are all air.
Method the most according to claim 1, it is characterised in that the qualitative detection device used in step (3) is mass spectrum.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109632437A (en) * | 2018-12-14 | 2019-04-16 | 北京化工大学 | A kind of sample-pretreating method of the on-site test based on ion mobility spectrometry |
| CN110412357A (en) * | 2019-07-22 | 2019-11-05 | 重庆大学 | A kind of test device and method of liquid dielectric carrier mobility |
| CN110554083A (en) * | 2018-06-04 | 2019-12-10 | 布鲁克科学有限公司 | Ion separation according to ion mobility for mass spectrometry |
| CN112649494A (en) * | 2020-12-15 | 2021-04-13 | 中国科学院大连化学物理研究所 | Multimodal quantification method based on photoionization ion mobility spectrometry |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110554083A (en) * | 2018-06-04 | 2019-12-10 | 布鲁克科学有限公司 | Ion separation according to ion mobility for mass spectrometry |
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| CN110554083B (en) * | 2018-06-04 | 2022-06-03 | 布鲁克科学有限公司 | Ion separation according to ion mobility for mass spectrometry |
| CN109632437A (en) * | 2018-12-14 | 2019-04-16 | 北京化工大学 | A kind of sample-pretreating method of the on-site test based on ion mobility spectrometry |
| CN109632437B (en) * | 2018-12-14 | 2020-07-24 | 北京化工大学 | Sample pretreatment method based on-site detection of ion mobility spectrometry |
| CN110412357A (en) * | 2019-07-22 | 2019-11-05 | 重庆大学 | A kind of test device and method of liquid dielectric carrier mobility |
| CN112649494A (en) * | 2020-12-15 | 2021-04-13 | 中国科学院大连化学物理研究所 | Multimodal quantification method based on photoionization ion mobility spectrometry |
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