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Application of a kind of tungsten disulfide in laser desorption ionization mass spectrometry detection

A technology of laser desorption ionization and tungsten disulfide, which is used in measurement devices, material analysis by electromagnetic means, instruments, etc., can solve the problems of difficult to form matrix layer, poor spectral reproducibility, background interference, etc., to avoid surface damage. Uniform, reproducible, and reproducible effects

Inactive Publication Date: 2015-09-02
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The problem in the prior art is that when using the MALDI-MS method, traditional MALDI matrices such as 2,5-dihydroxybenzoic acid (DHB) tend to produce severe background in the low molecular weight molecular segment (m / z < 500Da) Interference, and poor spectral reproducibility due to difficulty in forming a uniform matrix layer
Although the SALDI technology can be used for the detection of small organic molecules, the porous silicon, carbon nanotubes, graphene and other materials used are relatively expensive due to their complicated preparation and poor dispersion.

Method used

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  • Application of a kind of tungsten disulfide in laser desorption ionization mass spectrometry detection
  • Application of a kind of tungsten disulfide in laser desorption ionization mass spectrometry detection
  • Application of a kind of tungsten disulfide in laser desorption ionization mass spectrometry detection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Detection of benzo[k]fluoranthene with tungsten disulfide as SALDI surface material

[0026] 1) Change the concentration to 0.1mg / mLWS 2 The suspension was sonicated for 5 minutes. Take 1 μL of this suspension and quickly spot it on the sample target and dry it at room temperature.

[0027] 2) Under the same conditions, a total of twelve targets were prepared using the same method as a reference. Divide every three targets into one group for a total of four groups.

[0028] 3) On the four sets of targets, drop 1 μL of BkF solution with concentrations of 100 μg / mL, 10 μg / mL, 1 μg / mL, and 0.1 μg / mL respectively, and dry at room temperature. After drying, it is sent to the instrument for testing.

[0029] 4) Set the laser intensity to 60%, move randomly on the same sample point, continuously bombard the sample with the laser 2000 times, and superimpose the results of multiple times to form the overall picture.

[0030] figure 1 To analyze the mass spectra of different concentrat...

Embodiment 2

[0032] Use tungsten disulfide as SALDI surface material to detect pyrene

[0033] 1) The tungsten disulfide suspension with a concentration of 0.1 mg / mL is ultrasonically shaken for 5 minutes. Take 1 μL of this suspension and quickly spot it on the sample target and dry it at room temperature.

[0034] 2) Under the same conditions, use the same method to prepare a total of nine targets as references. Divide every three targets into one group for a total of three groups.

[0035] 3) On the three sets of targets, drop 1 μL of pyrene solution with concentrations of 100 μg / mL, 10 μg / mL, and 1 μg / mL respectively, and dry at room temperature. After drying, it is sent to the instrument for testing.

[0036] 4) Set the laser intensity to 60% and move randomly on the same sample point, continuously bombard the sample with the laser 2000 times, and superimpose the results of multiple times to form the overall picture.

[0037] figure 2 In order to analyze the mass spectra of different concent...

Embodiment 3

[0039] Study on Riboflavin with Tungsten Disulfide as SALDI Surface Material

[0040] 1) Using deionized water as the solvent, prepare a 200μM riboflavin solution (containing 20μM sodium chloride and 20μM potassium chloride), and adjust the pH of the solution to 5 with acetic acid to ensure that riboflavin can be Stable in aqueous solution;

[0041] 2) Take 0.5μL of tungsten disulfide solution and spot it on the sample target, dry at room temperature and form a thin matrix layer;

[0042] 3) Take 0.5μL of the prepared riboflavin sample solution and spot it on the dried tungsten disulfide film and dry it at room temperature;

[0043] 4) Send the prepared sample to the mass spectrometer for analysis.

[0044] image 3 To study the mass spectrum of riboflavin using tungsten disulfide as a surface-assisted laser desorption ionization (SALDI) surface material. The figure shows that when tungsten disulfide is used as the surface material of SALDI, riboflavin produces an alkali metal comple...

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Abstract

The invention discloses an application of tungsten disulfide in laser desorption ionization mass spectrometric detection. According to the invention, the tungsten disulfide is taken as a surface material for surface-assisted laser desorption ionization for mass spectrometric detection on small organic molecules. A tungsten disulfide suspension liquid is prepared firstly, and then subjected to ultrasonic oscillation for 5 minutes; 1 muL of the tungsten disulfide suspension liquid is dripped on sample target points; 1 muL of the small organic molecule solution to be detected is dropwisely adding on the films formed by the dried the tungsten disulfide suspension liquid; mass spectrometry is conducted after the small organic molecule solution is dried. The application has the advantages as follows: the mass spectrometric detection method is convenient in operation and low in cost; the degree of dispersion of the tungsten disulfide in the solvent is good; the sample target points are uniform in distribution; the reproducibility and the universality are high; the ionization efficiency of the organic molecules is high; the tungsten disulfide can effectively inhibit reduction reactions of riboflavin during the laser desorption ionization process and has important significance for researching the metabolic process of riboflavin in human bodies.

Description

Technical field [0001] The invention relates to organic small molecule detection technology, in particular to the application of tungsten disulfide in laser desorption ionization mass spectrometry detection. Background technique [0002] Matrix-Assisted Laser Desorption Ionization (MALDI) is a soft ionization technology that has the characteristics of simple sample preparation, few fragment ions, and high throughput. It is suitable for the analysis of polysaccharides, nucleosides, peptides and proteins. Macromolecule. α-cyano-4-hydroxycinnamic acid (CHCA), 2,5-dihydroxybenzoic acid (DHB) and sinapinic acid (SA) are currently the more commonly used traditional MALDI substrates. However, traditional MALDI matrices such as 2,5-dihydroxybenzoic acid (DHB) are in the low molecular weight range (m / z <500Da) is prone to cause serious background interference and poor spectral reproducibility. These shortcomings all limit the application of MALDI in the field of organic small molecul...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/64
Inventor 孔祥蕾张森倪彧李树奇翟伟霍翟羿
Owner NANKAI UNIV
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