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Application of tungsten disulfide in laser desorption ionization mass spectrometric detection

A technology of laser desorption ionization and tungsten disulfide, applied in measuring devices, material analysis through electromagnetic means, instruments, etc., can solve the problems of difficult formation of matrix layer, poor spectrum reproducibility, complicated preparation, etc., and avoid surface irregularities. Uniform, reproducible, uniform surface layer effect

Inactive Publication Date: 2014-02-19
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The problem with the prior art is that traditional MALDI matrices such as 2,5-dihydroxybenzoic acid (DHB) are The molecular segment (m / z < 500Da) tends to produce serious background interference, and at the same time, it is difficult to form a uniform matrix layer, resulting in poor spectral reproducibility
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 tungsten disulfide in laser desorption ionization mass spectrometric detection
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  • Application of tungsten disulfide in laser desorption ionization mass spectrometric detection

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Detection of Benzo[k]fluoranthene Using Tungsten Disulfide as SALDI Surface Material

[0027] 1) Add a concentration of 0.1mg / mLWS 2 Suspension, ultrasonic vibration for 5 minutes. Take 1 μL of the suspension and quickly spot it on the sample target, and dry it at room temperature.

[0028] 2) Under the same conditions, use the same method to prepare a total of twelve targets as a reference. Divide every three targets into one group, a total of four groups.

[0029] 3) Add 1 μL of BkF solutions with concentrations of 100 μg / mL, 10 μg / mL, 1 μg / mL, and 0.1 μg / mL dropwise on the four groups of targets, and dry at room temperature. After drying, it is sent to the instrument for detection.

[0030] 4) Set the laser intensity to 60%, move randomly on the same sample point, bombard the sample with laser 2000 times continuously, and superimpose the results of multiple times to get the general picture.

[0031] figure 1 To analyze the mass spectra of benzo[k]fluoranthene ...

Embodiment 2

[0033] Detection of Pyrene Using Tungsten Disulfide as SALDI Surface Material

[0034] 1) The concentration of 0.1mg / mL tungsten disulfide suspension, ultrasonic vibration for 5 minutes. Take 1 μL of the suspension and quickly spot it on the sample target, and dry it at room temperature.

[0035] 2) Under the same conditions, use the same method to prepare a total of nine targets as a reference. Every three targets were divided into one group, a total of three groups.

[0036] 3) Add 1 μL of pyrene solutions with concentrations of 100 μg / mL, 10 μg / mL, and 1 μg / mL dropwise on the three groups of targets, and dry at room temperature. After drying, it is sent to the instrument for detection.

[0037] 4) Set the laser intensity to 60%, move randomly on the same sample point, bombard the sample with laser 2000 times continuously, and superimpose the results of multiple times to get the general picture.

[0038] figure 2 In order to analyze the mass spectrograms of different c...

Embodiment 3

[0040] Study on Riboflavin Using Tungsten Disulfide as SALDI Surface Material

[0041] 1) Using deionized water as a solvent, prepare a riboflavin solution with a concentration of 200 μM (containing 20 μM sodium chloride and 20 μM potassium chloride), and adjust the pH of the solution to 5 with acetic acid to ensure that riboflavin can Stable in aqueous solution;

[0042] 2) Take 0.5 μL tungsten disulfide solution and spot on the sample target, dry at room temperature and form a thin layer of matrix;

[0043] 3) Take 0.5 μL of the prepared riboflavin sample solution and spot it on the dried tungsten disulfide film, and dry it at room temperature;

[0044] 4) Send the prepared sample to the mass spectrometer for analysis.

[0045] image 3 To study the mass spectrum of riboflavin with tungsten disulfide as surface-assisted laser desorption ionization (SALDI) surface material. The figure shows that when tungsten disulfide is used as the surface material of SALDI, riboflavin ...

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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 small organic 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 technique, which has the characteristics of simple sample preparation, less 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 more commonly used traditional matrices for MALDI. However, traditional MALDI matrices such as 2,5-dihydroxybenzoic acid (DHB) tend to produce serious background interference in the low-molecular-weight molecular segment (m / z < 500Da), and at the same time, the reproducibility of the spectrum is poor. These shortcomings limit the Application of ...

Claims

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Application Information

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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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