High-pressure formed substrate film assisted laser desorption dissociation mass spectrum quantitative analysis method

A technology of laser analysis and high-pressure forming, which is applied in the direction of analyzing materials, conducting material analysis by electromagnetic means, measuring devices, etc. Uniformity and other issues, to achieve the effect of convenient quality control and industrialization, good reproducibility, and easy control

Inactive Publication Date: 2013-08-14
HUAZHONG NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of the existing technology is that it is difficult to form crystals with uniform size and controllable shape, so that the spectra obtained by the laser at different scanning times are not reproducible, and there is no quantitative relationship between signal intensity and sample volume
Moreover, due to the difference in crystal size and morphology, the initial velocity and direction of the ions obtained after laser bombardment of the sample molecules are different, which affects the resolution and mass accuracy of the experimental results.

Method used

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  • High-pressure formed substrate film assisted laser desorption dissociation mass spectrum quantitative analysis method
  • High-pressure formed substrate film assisted laser desorption dissociation mass spectrum quantitative analysis method
  • High-pressure formed substrate film assisted laser desorption dissociation mass spectrum quantitative analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] The preparation steps of the high-pressure forming matrix film are as follows:

[0061] 1) Use an analytical balance to weigh a certain amount of matrix, such as 50mg CHCA (α-cyano-4-hydroxycinnamic acid) and 12mg DHB (2,5-dihydroxybenzoic acid), the type and amount of matrix can be determined according to different samples ;

[0062] 2). Grind the substrate obtained in step 1) with an agate mortar to make its particle size less than 2μm;

[0063] 3) Put the matrix powder obtained in step 2) into the abrasive tool of the tablet press, and then put it in the tablet press, apply a pressure of 4800kg, and keep it under this pressure for 1 minute;

[0064] 4). Take out the matrix film (CMTF) compressed in step 3) and store it at room temperature.

[0065] Among them, the picture of the CHCA film obtained in step 4) is as Figure 1-A As shown, the picture of the obtained DHB film is as Figure 1-B As shown, the figure shows that the obtained substrate film has a smooth surface and a u...

Embodiment 2

[0067] The high-pressure forming matrix film prepared in Example 1 is used for sample analysis signal intensity stability

[0068] 1) Stick the high-pressure forming matrix film prepared in Example 1 on the sample target;

[0069] 2) Adjust the α-casein hydrolysate sample to pH 1-2, use a pipette to spot 1μl sample on different sample spots on the film, and let it dry naturally;

[0070] 3) Take 10μl of 0.1wt% TFA aqueous solution to cover the sample point, hold for 2 seconds, absorb the water droplets with dust-free paper, and repeat 3 times;

[0071] 4) Put the sample target into the mass spectrometer;

[0072] 5) Use a laser with a certain frequency to bombard the sample to vaporize and ionize the sample to be tested, and detect its signal intensity;

[0073] Among them, step 5) obtained DHB high pressure forming matrix film total ion current diagram as image 3 As shown, the total ion current diagram of CHCA high pressure forming matrix film is as Figure 5 As shown, the total ion cu...

Embodiment 3

[0077] The in-situ desalination effect of the high-pressure forming matrix film prepared in Example 1

[0078] 1) Stand the high-pressure forming substrate film prepared in Example 1 on the sample target;

[0079] 2) Adjust the α-casein hydrolysate sample to pH 1-2, use a pipette to spot 1μl of the sample on different sample spots on the film, and let it dry naturally;

[0080] 3) Take 10μl of 0.1wt% TFA aqueous solution to cover the sample point, hold for 2 seconds, absorb the water droplets with dust-free paper, and repeat 3 times;

[0081] 4) Put the sample target into the mass spectrometer;

[0082] 5) Use a laser with a certain frequency to bombard the sample to vaporize and ionize the sample to be tested, and detect its signal intensity.

[0083] Among them, the mass spectrum of the α-casein hydrolysate obtained in step 5) after in situ desalination on the DHB matrix is Figure 7 As shown, the mass spectrum of α-casein hydrolysate after in situ desalination on the CHCA matrix is ​​...

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Abstract

A high-pressure formed substrate film assisted laser desorption dissociation mass spectrum quantitative analysis method is disclosed. According to the method, an organic micro-molecular substrate is compacted under high pressure to obtain a film; the film is then adhered to a sample target of a mass spectrometer; a sample is pointed on the film to be naturally dried; the sample undergoes in situ cleaning to remove inorganic salt; and after natural drying, the sample is putted into the mass spectrometer for analysis. By the adoption of the method, size and shape inhomogeneity of crystals obtained by a crystallization process is avoided. The obtained substrate film can have an effect of a hydrophobic reverse-phase stationary phase and adsorbs sample molecules. Inorganic salt is removed by in situ cleaning, and the sample molecules are prevented from spreading on the surface of the sample target so as to raise sensitivity. The method provided by the invention has advantages of stable mass spectrum signal, good reappearance, little metal ion adduct interference, small spectra background, good linear relation between signal intensity and sample amount and feasible quantitative analysis. The method is simple, requires no complex apparatus, complex sample pretreatment or organic solvent, and is green and environmentally friendly.

Description

Technical field [0001] The invention relates to a high-pressure forming matrix film assisted-laser analytic dissociation mass spectrometry quantitative analysis method, in particular to a preparation method of a uniform, size and thickness controllable matrix film, and a sample quantitative analysis method. The principle of the present invention is based on compressing organic molecules capable of absorbing laser energy into a film (Compressed Matrix Thin Film, referred to as CMTF) under a constant high pressure. The resulting matrix film can achieve the function of absorbing laser energy by the matrix obtained by ordinary methods. It can also be used as a hydrophobic film to adsorb sample molecules, so that the inorganic salt can be washed and removed in situ, and the diffusion of the sample on the target can be eliminated, which improves the sensitivity of the method. The method can also process solid samples, which increases the scope of application. Background technique [0...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/64
Inventor 钟鸿英黄璐璐肖潇郑石
Owner HUAZHONG NORMAL UNIV
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