CN114166927A - Mass spectrum device detection method for detecting multi-component sample - Google Patents
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- 238000001514 detection method Methods 0.000 title claims abstract description 31
- 238000001819 mass spectrum Methods 0.000 title abstract description 12
- 150000002500 ions Chemical class 0.000 claims abstract description 40
- 230000005540 biological transmission Effects 0.000 claims abstract description 35
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims description 18
- 238000002347 injection Methods 0.000 claims description 2
- 239000007924 injection Substances 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
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- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012356 Product development Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
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- 238000003912 environmental pollution Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 229910052743 krypton Inorganic materials 0.000 description 1
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
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- 230000000153 supplemental effect Effects 0.000 description 1
- 239000013076 target substance Substances 0.000 description 1
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- 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
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Abstract
The invention provides a mass spectrum device detection method for detecting a multi-component sample, which comprises the following steps: step S1, introducing a sample through a sample introduction device; step S2, ionizing low ionization energy sample molecules in the sample through a single photon ionization source, thereby obtaining corresponding positive ions; step S3, leading the obtained positive ions into a mass analyzer through a first electrostatic transmission focusing electrode; step S4, ionizing the high ionization energy sample molecules in the sample by an ionization gauge; step S5, introducing the obtained positive ions into the mass analyzer through a second electrostatic transmission focusing electrode; and step S6, the mass analyzer leads the obtained positive ions to a detector according to the mass-to-charge ratio for mass spectrometry to obtain a mass spectrogram, and qualitatively and quantitatively analyzes each component and the corresponding content in the sample according to the obtained mass spectrogram. The invention adopts the ionization gauge and the single photon ionization source as the double ionization source at the same time, thereby improving the detection sensitivity and widening the range of analyzing samples.
Description
Technical Field
The invention relates to the field of mass spectrometry, in particular to a mass spectrometry device detection method for detecting a multi-component sample.
Background
The on-line detection technology is one of the rapidly developed technologies in recent years, can detect the environmental quality in real time, discover pollution precursors as early as possible, and has a good early warning effect on sudden environmental pollution accidents, so that people pay more attention to the technology. In addition, the online detection technology is widely applied to the aspects of environmental safety, food safety, chemical product process detection and the like. Therefore, the research of fast online detection and analysis instruments with portability is becoming one of the important trends in analytical chemistry.
Spectroscopic, chromatographic, sensor and mass spectrometric methods can all be used for on-line detection techniques. The spectrum and the sensor are not high in specificity, only specific target substances can be detected, the detection limit is insufficient, and quantitative analysis cannot be carried out. The detection method of the chromatogram can carry out quantitative analysis on the substances to be detected, but the detection period is too long. Therefore, none of the above spectroscopic, sensor and chromatographic methods can meet the needs of on-site real-time on-line detection.
The mass spectrometry is one of important methods in the detection field, can qualitatively and quantitatively analyze complex compounds, can realize in-situ second-level response detection, and becomes a novel method of an online detection technology. However, due to the influence of ionization capability of the ionization source, for complex sample analysis, the conventional Electron Ionization (EI) source needs to be combined with a pre-separation device (such as GC, HPLC) to obtain a good qualitative and quantitative effect, and the drug consumption and long separation time of the pre-separation device restrict the application of online mass spectrometry. In recent years, with the development of soft ionization technology, especially the breakthrough of light source in photo ionization source, it is gradually possible to directly realize on-line detection of sample by using soft ionization technology. The Single Photon Ionization (SPI) is applied to the online detection of mass spectrum, and the real-time online detection of a sample can be realized.
Although SPI can be used well in real-time online monitoring of most organic substances, the species ionized by SPI is often limited because substances with ionization energies higher than photon energies cannot be ionized and are limited by the photon energies currently available. For substances with ionization energy higher than photon energy, SPI does not hold. For example, using vacuum ultraviolet (Krypton) as the SPI ionization source, samples with ionization energies greater than 10.6eV, such as water, nitrogen and oxygen, cannot be ionized. The solution is to combine a hard ionization source EI with an SPI ionization source, namely a 'hard ionization' mode and a 'soft ionization' mode, so as to expand the range of SPI ionization species.
The ionization gauge is a tool for reading vacuum degree and is manufactured according to the principle that the pressure of gas to be measured and ion current generated by sample ionization are in a direct proportion relation under a certain condition. In contrast to the "soft ionization" ionization mode of the SPI source, the ionization gauge itself has a "hard ionization" mode similar to that of the EI source, and thus can serve as a supplemental ionization source that ionizes substances that are not ionized by the SPI source, such as water and oxygen. Chinese patent CN 201910759283.0 invented a mass spectrum device and method using ionization gauge as EI source and SPI source combination, not only able to read vacuum degree in mass spectrum instrument, but also able to detect water and silicone oil sample in freeze-drying process.
However, this method has the following drawbacks:
1. the sensitivity of the measured portion of the sample is too low. In chinese patent CN 201910759283.0, the ionization gauge is placed at one side of the sample inlet and far away from the mass analyzer, and the sample ionized by the ionization gauge is collided with the transmission of the transmission focusing electrode through the ionization chamber, so that the loss of ion number is large and the sensitivity is greatly reduced.
2. There is a photon competition effect. After the sample enters the ionization chamber, the sample with ionization energy higher than that of the SPI source can still absorb photons to obtain energy after being ionized by the ionization gauge, so that the loss of the photons of the SPI source is increased, the efficiency of ionizing the sample with low ionization energy by the SPI source is reduced, and the detection range and sensitivity of a mass spectrum are influenced.
3. The ionization gauge itself is provided with a grid mesh to prevent the ionized positive ions from escaping, which would reduce the ionized sample entering the mass analyzer, reducing the instrument sensitivity.
Therefore, it is desirable to provide a method for solving the problems of photon competition effect and low sensitivity in the detection device.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a mass spectrometry device detection method for detecting a multi-component sample.
The invention provides a mass spectrometry device detection method for detecting a multi-component sample, which comprises the following steps: step S1, introducing a sample through a sample introduction device;
step S2, ionizing low ionization energy sample molecules in the sample through a single photon ionization source, thereby obtaining corresponding positive ions;
step S3, leading the obtained positive ions into a mass analyzer through a first electrostatic transmission focusing electrode;
step S4, ionizing high ionization energy sample molecules in the sample by an ionization gauge, and reading out the vacuum degree of the system;
step S5, introducing the obtained positive ions into the mass analyzer through a second electrostatic transmission focusing electrode;
and step S6, the mass analyzer leads the obtained positive ions to a detector according to the mass-to-charge ratio for mass spectrometry to obtain a mass spectrogram, and qualitatively and quantitatively analyzes each component and the corresponding content in the sample according to the obtained mass spectrogram.
Preferably, in step S1, one end of the sample introduction device is connected to the ionization chamber and introduces the sample into the ionization chamber.
Preferably, in step S2, the single photon ionization source is vertically mounted on the ionization chamber.
Preferably, in step S3, the ionization chamber is provided with the mass analyzer at an end facing away from the sample introduction device;
the first electrostatic transmission focusing electrode is arranged between the mass analyzer and the ionization chamber;
positive ions within the ionization chamber are introduced into the mass analyzer through the first electrostatically transported focusing electrode.
Preferably, in step S5, the mass analyzer is mounted with the ionization gauge facing away from one end of the ionization chamber;
the ionization gauge is provided with a second electrostatic transmission focusing electrode between the ionization gauge and the mass analyzer after the grates in the ionization gauge are removed;
the ionization gauge introduces positive ions through the second electrostatically transported focusing electrode to the mass analyzer.
Preferably, the ionization gauge, the mass analyser, the ionization chamber and the sample introduction device are arranged along a coaxial line.
Preferably, the second electrostatically transporting focus electrode, the mass analyser, the first electrostatically transporting focus electrode and the ionisation chamber are all voltage loadable.
Preferably, the mass analyser is a quadrupole mass analyser;
the quadrupole mass analyzer is used for carrying out mass spectrometry on positive ions introduced by the second electrostatic transmission focusing electrode and the first electrostatic transmission focusing electrode.
Preferably, the second electrostatically transporting focus electrode is detachable.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention effectively improves the sensitivity of the instrument, eliminates photon competition effect and realizes the measurement and detection of various component samples;
2. the ionization gauge can read the vacuum degree, and can avoid the defect that the service life of the ionization gauge is rapidly reduced because the heating wire of the ionization gauge is oxidized due to oxidizing samples such as air of the traditional EI source;
3. the invention does not need lower working air pressure, and the lower working air pressure needs a more complex and expensive vacuum system, thereby limiting the real-time online detection application of the instrument;
4. the invention adopts the ionization gauge and the single-photon ionization source as the double ionization source at the same time, improves the detection sensitivity, widens the range of analyzing samples, takes the quadrupole mass analyzer as the core and combines the two advantages of different ionization characteristics and high sensitivity of the quadrupole mass spectrum.
5. The device and the method can be applied to in-situ detection of mass spectrum, realize real-time online detection of multi-component complex samples, can be used as the first choice of a mass spectrum instrument in a laboratory, analyze and research multi-component compounds, expand the application range of products, open up multiple application directions and have pioneering significance for product development.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic diagram of a mass spectrometer;
FIG. 2 is a mass spectrum of a sample.
Shown in the figure:
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
As shown in fig. 1 and 2, a mass spectrometry apparatus detection method for detecting a multi-component sample includes the following steps: step S1, introducing a sample through a sample introduction device 7, wherein one end of the sample introduction device 7 is connected with the ionization chamber 6 and introduces the sample into the ionization chamber 6;
step S2, ionizing low ionization energy sample molecules in the sample through the single photon ionization source 5 to obtain corresponding positive ions, and vertically installing the single photon ionization source 5 on the ionization chamber 6;
step S3, leading the obtained positive ions into an ionization chamber 6 of a mass analyzer 3 through a first electrostatic transmission focusing electrode 4, and mounting the mass analyzer 3 at one end of a sample injection device 7;
a first electrostatic transmission focusing electrode 4 is arranged between the mass analyzer 3 and the ionization chamber 6;
positive ions in the ionization chamber 6 are introduced into the mass analyzer 3 through the first electrostatic transmission focusing electrode 4;
step S4, ionizing high ionization energy sample molecules in the sample by the ionization gauge 1, and reading out the vacuum degree of the system;
step S5, introducing the obtained positive ions into the mass analyzer 3 through the second electrostatic transmission focusing electrode 2; an ionization gauge 1 is arranged at one end of the mass analyzer 3, which is back to the ionization chamber 6, a second electrostatic transmission focusing electrode 2 is arranged between the ionization gauge 1 and the mass analyzer 3 after the ionization gauge 1 is detached from the grid, the second electrostatic transmission focusing electrode 2 is detachable, and positive ions are introduced into the mass analyzer 3 through the ionization gauge 1 by the second electrostatic transmission focusing electrode 2;
and step S6, the mass analyzer 3 leads the obtained positive ions to a detector according to the mass-to-charge ratio for mass spectrometry to obtain a mass spectrogram, and qualitatively and quantitatively analyzes each component and the corresponding content in the sample according to the obtained mass spectrogram.
The ionization gauge 1, the mass analyzer 3, the ionization chamber 6 and the sample introduction device 7 are arranged along a coaxial line. The second electrostatically transported focusing electrode 2, the mass analyser 3, the first electrostatically transported focusing electrode 4 and the ionisation chamber 6 may all be subjected to voltages. The mass analyzer 3 adopts a quadrupole mass analyzer which carries out mass spectrometry on positive ions introduced by the second electrostatic transmission focusing electrode 2 and the first electrostatic transmission focusing electrode 4.
Example 2
Example 2 is a preferred example of example 1.
As shown in fig. 1 and 2, the present embodiment includes: the device comprises an ionization gauge 1, a second electrostatic transmission focusing electrode 2, a mass analyzer 3, a first electrostatic transmission focusing electrode 4, a single photon ionization source 5, an ionization chamber 6 and a sample introduction device 7; one end of the sample introduction device 7 faces the ionization chamber 6, and a sample is introduced into the ionization chamber 6; the single photon ionization source 5 faces the ionization chamber 6, and ionizes the sample to obtain corresponding positive ions; a first electrostatic transmission focusing electrode 4 is arranged between the mass analyzer 3 and the ionization chamber 6; a first electrostatic transmission focusing electrode 4 and a mass analyzer 3 are arranged between the second electrostatic transmission focusing electrode 2 and the ionization chamber 6; a first electrostatic transmission focusing electrode 4, a mass analyzer 3 and a second electrostatic transmission focusing electrode 2 are arranged between the ionization gauge 1 and the ionization chamber 6, the ionization gauge 1 reads the vacuum degree of the instrument, and the ionization sample obtains corresponding positive ions.
Wherein the sample ions are drawn by the electric field forces generated by the ionization chamber 6 and the positive ions are introduced into the mass analyser 3 via the first electrostatically transported focussing electrode 4. The sample ions ionized by the ionization gauge 1 pass through the second electrostatic delivery focusing electrode 2 to introduce positive ions into the mass analyzer 3. The single photon ionization source 5 is vertical to the ionization chamber 6, and the single photon ionization source 5 is vertical to the ionization gauge 1. The second electrostatic transfer focusing electrode 2 is detachable from the ionization gauge 1 for use and the mass analyser 3 comprises a quadrupole mass analyser. The ionization chamber 6, the first electrostatically transporting focus electrode 4, the mass analyzer 3 and the second electrostatically transporting focus electrode 2 can be charged with a voltage.
In this embodiment, the execution includes the steps of: step T1, introducing the sample into the ionization chamber 6 through the sample introduction device 7; step T2, ionizing low ionization energy sample molecules in the sample by the single photon ionization source 5 to obtain corresponding positive ions; step T3, introducing the obtained positive ions into the mass analyzer 3 through the first electrostatic transmission focusing electrode 4; step T4, ionizing the high ionization energy sample molecules in the sample by the ionization gauge 1; step T5, introducing the obtained positive ions into the mass analyzer 3 through the second electrostatic transmission focusing electrode 2; and step T6, the mass analyzer 3 leads the obtained positive ions to a detector according to the mass-to-charge ratio for mass spectrometry to obtain a mass spectrogram, and qualitatively/quantitatively analyzes each component and corresponding content in the sample according to the obtained mass spectrogram.
Example 3
As shown in fig. 2, first, a sample is introduced into the apparatus through the sample introduction device 7. Secondly, the ionization gauge 1 and the single photon ionization source 5 ionize the sample to be measured into positive ions. Again, positive ions are introduced to the quadrupole mass analyser via the second electrostatic transmitting focusing electrode 2 and the first electrostatic transmitting focusing electrode 4. Next, the quadrupole mass analyzer obtains a mass spectrum peak of the sample by mass analysis. And finally, quantitatively analyzing the corresponding content of each substance according to the mass spectrogram of the sample.
Those skilled in the art will appreciate that, in addition to implementing the system and its various devices, modules, units provided by the present invention as pure computer readable program code, the system and its various devices, modules, units provided by the present invention can be fully implemented by logically programming method steps in the form of logic gates, switches, application specific integrated circuits, programmable logic controllers, embedded microcontrollers and the like. Therefore, the system and various devices, modules and units thereof provided by the invention can be regarded as a hardware component, and the devices, modules and units included in the system for realizing various functions can also be regarded as structures in the hardware component; means, modules, units for performing the various functions may also be regarded as structures within both software modules and hardware components for performing the method.
In the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present application and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (9)
1. A mass spectrometry device detection method for detecting a multi-component sample is characterized by comprising the following steps: step S1, introducing a sample through a sample introduction device (7);
step S2, ionizing low ionization energy sample molecules in the sample through the single photon ionization source (5) to obtain corresponding positive ions;
step S3, leading the obtained positive ions into a mass analyzer (3) through a first electrostatic transmission focusing electrode (4);
step S4, ionizing high ionization energy sample molecules in the sample through an ionization gauge (1), and reading back the vacuum degree;
step S5, leading the obtained positive ions into the mass analyzer (3) through a second electrostatic transmission focusing electrode (2);
and step S6, the mass analyzer (3) leads the obtained positive ions to a detector according to the mass-to-charge ratio for mass spectrometry to obtain a mass spectrogram, and qualitatively and quantitatively analyzes each component and corresponding content in the sample according to the obtained mass spectrogram.
2. The method of claim 1, wherein the mass spectrometer is configured to detect a multicomponent sample by: in step S1, one end of the sample injection device (7) is connected with the ionization chamber (6) and the sample is introduced into the ionization chamber (6).
3. The method of claim 2, wherein the mass spectrometer is configured to detect a multicomponent sample by: in step S2, the single photon ionization source (5) is vertically mounted on the ionization chamber (6).
4. The method of claim 3, wherein the mass spectrometer is configured to detect a multicomponent sample by: in step S3, the ionization chamber (6) is equipped with the mass analyzer (3) at the end opposite to the sample feeding device (7);
the first electrostatic transmission focusing electrode (4) is installed between the mass analyzer (3) and the ionization chamber (6);
positive ions within the ionization chamber (6) are introduced into the mass analyser (3) through the first electrostatically transported focussing electrode (4).
5. The method of claim 4, wherein the mass spectrometer is configured to detect a multicomponent sample by: in step S5, the mass analyser (3) is mounted with the ionization gauge (1) at the end facing away from the ionization chamber (6);
the second electrostatic transmission focusing electrode (2) is arranged between the ionization gauge (1) and the mass analyzer (3);
the ionization gauge (1) introduces positive ions through the second electrostatically transporting focus electrode (2) to the mass analyser (3).
6. The method of claim 5, wherein the mass spectrometer is configured to detect a multicomponent sample by: the ionization gauge (1), the mass analyzer (3), the ionization chamber (6) and the sampling device (7) are arranged along a coaxial line.
7. The method of claim 5, wherein the mass spectrometer is configured to detect a multicomponent sample by: the second electrostatically transporting focus electrode (2), the mass analyser (3), the first electrostatically transporting focus electrode (4) and the ionisation chamber (6) are all voltage loadable.
8. The method of claim 5, wherein the mass spectrometer is configured to detect a multicomponent sample by: the mass analyzer (3) adopts a quadrupole mass analyzer;
the quadrupole mass analyzer is used for carrying out mass spectrometry on positive ions introduced by the second electrostatic transmission focusing electrode (2) and the first electrostatic transmission focusing electrode (4).
9. The method of claim 5, wherein the mass spectrometer is configured to detect a multicomponent sample by: the second electrostatic transmission focusing electrode (2) is detachable.
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Cited By (2)
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| CN117147673A (en) * | 2023-10-24 | 2023-12-01 | 广州源古纪科技有限公司 | Method, system and equipment for detecting breath mass spectrum |
| CN117995647A (en) * | 2024-04-07 | 2024-05-07 | 宁波华仪宁创智能科技有限公司 | Mass spectrometry apparatus and method based on multiple ionization techniques |
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