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A rapid evaporation electrospray ion source and analysis method

An electrospray ion source and rapid evaporation technology, which is applied in the direction of ion source/gun, material analysis and material analysis through electromagnetic means, can solve the problems of small heating area, poor heat transfer efficiency, and low heating efficiency, and achieve improvement Effect of heating area, improving heat transfer efficiency, and increasing specific area

Active Publication Date: 2021-10-22
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Problem 1: The heating area of ​​the sample droplet is small and the heat transfer efficiency is poor
Only the bottom of the vaporization chamber of the device is heated, and the wall is not heated. After the liquid is dripped into the vaporization chamber, only the part that is in contact with the bottom of the vaporization chamber, that is, the lower part of the droplet, is heated, and the part that is not in contact with the bottom is heated. For example, the upper part of the droplet and the middle part of the droplet are not heated, so the heating efficiency is very low
[0005] Problem 2: The thermal shock method results in too short contact time between the sample droplet and the heat source, reducing heat transfer
Although this effectively prevents thermal energy from being converted into molecular internal energy, thereby avoiding thermal degradation, but because the contact time between the liquid sample and the hot plate is extremely short, only a small part of the liquid droplets entering the vaporization chamber, that is, the part that is in contact with the hot plate is destroyed. Gasification, and the resulting rapid expansion, which makes the part of the droplet that is not heated is also pushed out of the gasification chamber, but this part of the sample has not been vaporized or atomized, and cannot be used for ionization and enter the mass spectrometer for detection

Method used

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  • A rapid evaporation electrospray ion source and analysis method
  • A rapid evaporation electrospray ion source and analysis method
  • A rapid evaporation electrospray ion source and analysis method

Examples

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Effect test

Embodiment 1

[0040] A fast evaporation electrospray ion source device (such as figure 1 shown): It consists of four parts: electrospray generating unit (4), heating unit (2), vaporization chamber (3) and sampling unit (5).

[0041] The mass spectrometer inlet (1) is located at the far right; the leftmost is the electrospray generator unit (4), and the tip (41) of the electrospray generator unit is located on the axis of the mass spectrometer inlet (1), and the distance from the mass spectrometer inlet (1) is about 3-10cm; the gasification chamber (3) is placed inside the heating unit (2), the outlet of the gasification chamber (3) is located below the axis of the mass spectrometer inlet (1), and the horizontal distance from the mass spectrometer inlet (1) is 0 -5cm, the vertical distance from the mass spectrometer inlet (1) axis is 0-5cm, and is located between the tip of the electrospray generation unit and the mass spectrometer inlet; the sampling unit (5) is located directly above the o...

Embodiment 2

[0048] This embodiment adopts the rapid evaporation electrospray ion source device described in Embodiment 1 ( figure 1 ) combined with a mass spectrometry system to analyze thermally unstable compounds, with mesaconitine as the detection object. The electrospray voltage was 3 KV, the spray solvent was methanol, and the spray solvent flow rate was 3 μL / min. The diameter of the gasification chamber is 3mm, the height is 3mm, and the temperature is set at 125°C.

[0049] The method of operation is the same as in Example 1. Use a pipette to draw 6.5 μL of aconitine methanol solution with a concentration of 6mg / L and drop it into the hot vaporization chamber. The sample evaporates rapidly, and the sample vapor is ionized by electrospray at the mass spectrometer inlet (1), forming ions and entering the mass spectrometer is detected. In the normal spectrum mode, the spectrum is obtained as figure 2 As shown, compared with the thermal shock gasification technology (ZL20161001882...

Embodiment 3

[0051] This embodiment adopts the rapid evaporation electrospray ion source device described in Embodiment 1 ( figure 1 ) combined with a mass spectrometry system to analyze biological macromolecules, taking myoglobin and cytochrome C as examples. The electrospray voltage was 4 KV, the spray solvent was methanol:water (30:70, v / v) solution containing 0.1% (v) acetic acid, and the spray solvent flow rate was 5 μL / min. The diameter of the gasification chamber is 5mm, the height is 5mm, and the temperature is set at 200°C. Myoglobin and cytochrome C were dissolved in water to prepare 59 μM and 100 μM aqueous solutions, respectively.

[0052] The method of operation is the same as in Example 1. Use a pipette to draw 6.5 μL of myoglobin and cytochrome C aqueous solution dropwise in the vaporization chamber, scan the mass spectrometry data, the results are as follows image 3 , 4 As shown, both myoglobin and cytochrome C produce multi-charged mass spectrum peaks, and the obtaine...

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Abstract

A rapid evaporation electrospray ion source and an analysis method, the invention relates to a rapid evaporation electrospray ion source and an analysis method, and belongs to the technical field of atmospheric pressure mass spectrometry ionization. The ionization source is composed of four parts: electrospray generating unit, heating unit, vaporization chamber and sampling unit. Put the gasification chamber into the heating unit and heat it to T B ‑T L The sample solution is dripped into the gasification chamber using the sampling unit; when the sample vapor rises to the entrance of the mass spectrometer, the sample vapor is converted into sample ions using the electrospray ionization unit, and these ions are then introduced into the mass spectrometer for detection. The operation is simple, no sample pretreatment is required, and high-throughput online detection can be realized.

Description

technical field [0001] The invention relates to a rapid evaporation electrospray ion source and an analysis method, belonging to the technical field of atmospheric pressure mass spectrometry ionization. Background technique [0002] We have developed a thermal shock gasification electrospray ionization source and mass spectrometry system (patent number: ZL201610018823.6). This method applies the sample solution to the heat source, and the sample deforms instantly when it contacts the heat source, changing from a liquid state to a gaseous state. Since the contact time between the sample solution and the heat source is very short, the heat absorbed by the sample solution is only used to overcome the intermolecular force, and is not converted into internal molecular energy, which will not lead to the degradation of the compounds in the sample. Heating technology is applied to thermal instability and mass spectrometry analysis of biological macromolecules, especially in the anal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44G01N27/68H01J49/16
CPCG01N1/44G01N27/68H01J49/165
Inventor 许庆轩刘淑莹卢佳杰
Owner HEILONGJIANG UNIV
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