CN116008022A - Mass spectrum detection method and device based on chemical ionization technology - Google Patents
Mass spectrum detection method and device based on chemical ionization technology Download PDFInfo
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- CN116008022A CN116008022A CN202211133534.2A CN202211133534A CN116008022A CN 116008022 A CN116008022 A CN 116008022A CN 202211133534 A CN202211133534 A CN 202211133534A CN 116008022 A CN116008022 A CN 116008022A
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Abstract
The invention provides a mass spectrum detection method and a device based on a chemical ionization technology, wherein the method comprises the following steps: a pre-scanning stage; multiple reagent molecules are ionized in an ion source, reagent ions with different mass numbers are released from an ion screening unit in time, and the reagent ions pass through an ion-molecule reaction zone without a sample and enter a mass spectrometer to obtain the mapping relation between the reagent ions and the release time; a sample detection stage; the sample enters an ion-molecule reaction area, a plurality of reagent molecules are ionized in an ion source, reagent ions with different mass numbers are released in time, and the release time is adjusted according to the mapping relation; in the ion-molecule reaction zone, reagent ions with different mass numbers react with a sample in time, and the sample ions enter a mass spectrum to obtain mass spectrograms which respectively correspond to various reagent ions and contain sample information; and screening the mass spectrogram to obtain the information of the analyte in the sample. The invention has the advantages of accurate detection and the like.
Description
Technical Field
The invention relates to mass spectrometry, in particular to a mass spectrometry detection method and device based on chemical ionization technology.
Background
The chemical ionization ion source ionizes a specific reagent gas to generate gas-phase reagent ions, and then the generated reagent ions and the analyte undergo gas-phase ion/molecule reaction to make the analyte become charged ions.
When the chemical ionization ion source is used, a single kind of reagent molecules are adopted, and certain specific reagent ions are generated to react with a target object. This solution has drawbacks such as:
1. the specific reagent ions can only have good ionization effect (ion-molecule reaction) on a certain class of target objects due to the specific ionization characteristics of the reagent ions, so that the detection types of the substances are limited. When this type of chemical ionization ion source is applied to complex unknown analysis, there is a risk of undetectable.
2. Chemical ionization sources have high requirements for reagent ion purity, and impure reagent molecules can easily introduce other hetero ions, which can affect ion-molecule reactions with analytes.
In order to solve the above problems, the existing solutions are
For the analysis of unknowns, the reaction was engaged by trying to change different reagent molecules according to the experience of the experimenter. The method is complex in operation, and after different reagent molecules are replaced, reagent ions need to wait for a plurality of hours to reach the strength required by ionization. For real-time on-line monitoring of complex volatile organic compounds in ambient air, the time for switching reagent ions is very likely to cause a supervision blind spot.
Disclosure of Invention
In order to solve the defects in the prior art, the invention provides a mass spectrum detection method based on a chemical ionization technology.
The invention aims at realizing the following technical scheme:
the mass spectrum detection method based on the chemical ionization technology comprises the following steps:
a pre-scanning stage; a plurality of reagent molecules are ionized within the ion source;
adjusting parameters of an ion screening unit so that reagent ions with different mass numbers are released from the ion screening unit in time, enabling the reagent ions to pass through an ion-molecule reaction zone without a sample, entering a mass spectrometer, obtaining a mass spectrogram corresponding to each reagent ion, and obtaining a mapping relation between the reagent ions and release time according to the mass spectrogram;
a sample detection stage; a sample enters the ion-molecule reaction zone, the plurality of reagent molecules are ionized in the ion source, the ion screening unit is adjusted so that reagent ions with different mass numbers are released from the ion screening unit in time, and the release time is adjusted according to the mapping relation;
in the ion-molecule reaction zone, reagent ions with different mass numbers react with a sample in time, and the sample ions enter a mass spectrum to obtain mass spectrograms which respectively correspond to various reagent ions and contain sample information;
and screening the mass spectrogram containing the sample information, and obtaining the analyte information in the sample according to the screened mass spectrogram.
The invention also aims to provide a mass spectrum detection device, which is realized by the following technical scheme:
a mass spectrum detection device for the mass spectrum detection method based on the chemical ionization technology, which comprises an ion source and a mass spectrometer; the mass spectrum detection device is characterized by further comprising:
an ion screening unit disposed between the ion source and the mass spectrometer;
an ion-molecule reaction unit disposed between the ion screening unit and the mass spectrometer.
Compared with the prior art, the invention has the following beneficial effects:
1. the detection result is accurate;
the mapping relation between reagent ions and release time is obtained in the pre-scanning stage and is used for subsequent sample detection, so that the ion strength is ensured, and the detection accuracy is improved;
by utilizing the ion screening function, the influence of impurity ions generated by the impurity of the reagent is avoided, and the detection accuracy is further improved;
2. the detection range is large;
meanwhile, a plurality of reagent molecules are adopted, reagent ions are screened in time to participate in the reaction, so that a mass spectrum of the reaction participated by the plurality of reagent ions is obtained, the detection range of the substances is improved, and unknown substances with complex real time analysis are obtained.
Drawings
The present disclosure will become more readily understood with reference to the accompanying drawings. As will be readily appreciated by those skilled in the art: the drawings are only for illustrating the technical scheme of the present invention and are not intended to limit the scope of the present invention. In the figure:
fig. 1 is a flow chart of a mass spectrometry detection method based on chemical ionization technology according to an embodiment of the present invention.
Detailed Description
Fig. 1 and the following description depict alternative embodiments of the invention to teach those skilled in the art how to make and reproduce the invention. In order to teach the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will appreciate variations or alternatives derived from these embodiments that fall within the scope of the invention. Those skilled in the art will appreciate that the features described below can be combined in various ways to form multiple variations of the invention. Thus, the invention is not limited to the following alternative embodiments, but only by the claims and their equivalents.
Example 1:
fig. 1 schematically shows a flow chart of a mass spectrum detection method based on a chemical ionization technology according to an embodiment of the present invention, as shown in fig. 1, the mass spectrum detection method based on the chemical ionization technology is as follows:
a pre-scanning stage; a plurality of reagent molecules are ionized within a chemical ionization ion source;
adjusting parameters of an ion screening unit so that reagent ions with different mass numbers are released from the ion screening unit in time, enabling the reagent ions to pass through an ion-molecule reaction zone without a sample, entering a mass spectrometer, obtaining a mass spectrogram corresponding to each reagent ion, and obtaining a mapping relation between the reagent ions and release time according to the mass spectrogram;
a sample detection stage; a sample enters the ion-molecule reaction zone, the plurality of reagent molecules are ionized in the ion source, the ion screening unit is adjusted so that reagent ions with different mass numbers are released from the ion screening unit in time, and the release time is adjusted according to the mapping relation;
in the ion-molecule reaction zone, reagent ions with different mass numbers react with a sample in time, and the sample ions enter a mass spectrum to obtain mass spectrograms which respectively correspond to various reagent ions and contain sample information;
and screening the mass spectrogram containing the sample information, and obtaining the analyte information in the sample according to the screened mass spectrogram.
In order to accurately obtain the mapping relation, further, in the pre-scanning stage, reagent ions with various mass numbers are released from the ion screening unit at the same release time, a mass spectrogram corresponding to each reagent ion is obtained, and the reagent ion peak intensity is obtained according to the mass spectrogram;
and adjusting the release time of the reagent ions with different mass numbers so that the peak intensities of the reagent ions are the same, thereby obtaining the mapping relation between the reagent ions and the release time.
In order to reduce the structural complexity and the adjustment difficulty, further, the ion screening unit adopts a quadrupole rod filter.
The mass spectrum detection device of the embodiment of the invention, that is, the device for realizing the mass spectrum detection method based on the chemical ionization technology of the embodiment, comprises:
a chemical ionization ion source and a mass spectrometer;
an ion screening unit, such as a quadrupole, disposed between the ion source and the mass spectrometer;
an ion-molecule reaction unit disposed between the ion screening unit and the mass spectrometer.
Example 2:
the mass spectrum detection method and the application example of the method based on the chemical ionization technology in the seawater detection according to the embodiment 1 of the invention.
In this application example, as shown in fig. 1, the mass spectrum detection method based on the chemical ionization technology is:
a pre-scanning stage; multiple reagent molecules, such as nitrogen, oxygen, water vapor, are ionized by a hollow cathode power supply within a chemical ionization ion source, e.g. to form NO + 、O 2 + 、H 3 O + Reagent ions and other possible hetero ions, e.g. N 2 + ；
Reagent ions pass through the extraction cone and enter the ion screening unit, and a quadrupole mass filter is adopted;
adjusting voltage parameters of an ion screening unit, and releasing reagent ions with different mass numbers from the ion screening unit with the same release time: sequentially releasing the mass numbers from small to large to obtain mass spectrograms corresponding to each reagent ion, and obtaining the peak intensity of the reagent ion according to the mass spectrograms;
adjusting the release time of each mass number of reagent ions so that the peak intensities of each reagent ion are the same, thereby obtaining the mapping relation between the reagent ions and the (adjusted) release time, wherein the larger the mass number is, the longer the release time is;
a sample detection stage; sample is entered into the ion-molecule reaction zone, the plurality of reagent molecules are ionized within the ion source, and the ion screening unit is adjusted such that reagent ions of different mass numbers are released from the ion screening unit in time periods: sequentially releasing the mass numbers from small to large, and adjusting the release time according to the mapping relation;
in the ion-molecule reaction zone, reagent ions with different mass numbers react with a sample in time, and the sample ions enter a mass spectrum to obtain mass spectrograms which respectively correspond to various reagent ions and contain sample information;
and screening the mass spectrogram containing the sample information, and obtaining the analyte information in the sample according to the screened mass spectrogram.
The mass spectrum detection device of the embodiment of the invention, that is, the device for realizing the mass spectrum detection method based on the chemical ionization technology of the embodiment, comprises:
a chemical ionization ion source and a mass spectrometer, the chemical ionization ion source using a hollow cathode discharge source;
the extraction cone and the ion screening unit are sequentially arranged between the ion source and the mass spectrometer;
an ion-molecule reaction unit disposed between the ion screening unit and the mass spectrometer.
Claims (7)
1. The mass spectrum detection method based on the chemical ionization technology comprises the following steps:
a pre-scanning stage; a plurality of reagent molecules are ionized within the ion source;
adjusting parameters of an ion screening unit so that reagent ions with different mass numbers are released from the ion screening unit in time, enabling the reagent ions to pass through an ion-molecule reaction zone without a sample, entering a mass spectrometer, obtaining a mass spectrogram corresponding to each reagent ion, and obtaining a mapping relation between the reagent ions and release time according to the mass spectrogram;
a sample detection stage; a sample enters the ion-molecule reaction zone, the plurality of reagent molecules are ionized in the ion source, the ion screening unit is adjusted so that reagent ions with different mass numbers are released from the ion screening unit in time, and the release time is adjusted according to the mapping relation;
in the ion-molecule reaction zone, reagent ions with different mass numbers react with a sample in time, and the sample ions enter a mass spectrum to obtain mass spectrograms which respectively correspond to various reagent ions and contain sample information;
and screening the mass spectrogram containing the sample information, and obtaining the analyte information in the sample according to the screened mass spectrogram.
2. The mass spectrometry detection method according to claim 1, wherein in the pre-scan stage, reagent ions of respective mass numbers are released from the ion screening unit at the same release time, a mass spectrum corresponding to each reagent ion is obtained, and a reagent ion peak intensity is obtained from the mass spectrum;
and adjusting the release time of the reagent ions with different mass numbers so that the peak intensities of the reagent ions are the same, thereby obtaining the mapping relation between the reagent ions and the release time.
3. The method of claim 2, wherein the ion screening unit employs a quadrupole mass filter.
4. The method of claim 1, wherein the reagent molecules are ionized by a hollow cathode discharge source.
5. The method of claim 1, wherein reagent ions pass through an extraction cone and then enter the ion screening unit.
6. The method of claim 1, wherein the reagent molecule is a nitrogen molecule, an oxygen molecule, or a water vapor molecule.
7. A mass spectrometry detection apparatus for carrying out the chemical ionization technique-based mass spectrometry detection method of any one of claims 1 to 6, the mass spectrometry detection apparatus comprising an ion source and a mass spectrometer; the mass spectrum detection device is characterized by further comprising:
an ion screening unit disposed between the ion source and the mass spectrometer;
an ion-molecule reaction unit disposed between the ion screening unit and the mass spectrometer.
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| CN202211133534.2A CN116008022A (en) | 2022-09-18 | 2022-09-18 | Mass spectrum detection method and device based on chemical ionization technology |
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| CN202211133534.2A CN116008022A (en) | 2022-09-18 | 2022-09-18 | Mass spectrum detection method and device based on chemical ionization technology |
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