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Method for analyzing and dissociating lipid molecules by laser-induced electron capture mass spectrum

A laser desorption and dissociation technology, applied in the field of laser desorption dissociation mass spectrometry, can solve the problems of difficulty in generating low-energy electrons, increase manufacturing difficulty, and complicated operation, and achieve the effects of fast analysis speed, simple and easy control of the process, and high product purity.

Active Publication Date: 2013-07-31
HUAZHONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although electron transfer dissociation detectors (ETD / ECD) also use low-energy electrons to ionize sample molecules, the disadvantages of these methods are that it is difficult to generate low-energy electrons, or additional chemical ionization sources (CI) and reaction gases are required, and the operation is complicated and increases manufacturing difficulty

Method used

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  • Method for analyzing and dissociating lipid molecules by laser-induced electron capture mass spectrum
  • Method for analyzing and dissociating lipid molecules by laser-induced electron capture mass spectrum
  • Method for analyzing and dissociating lipid molecules by laser-induced electron capture mass spectrum

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Preparation of Nano-ZnO Matrix and Sample Target

[0042] The preparation steps are as follows:

[0043] 1. Stir and heat 15ml of zinc sulfate solution with a concentration of 1mol / L to 60°C, then dropwise add 30ml of ammonium bicarbonate solution with a concentration of 1mol / L, continue to stir for 2 hours after the dropwise addition and keep at 60°C;

[0044] 2. Centrifuge the material obtained in step 1) at 2000g (7722rpm) for 2 minutes, discard the supernatant, wash the solid with pure water until neutral, and bake at 100°C for 200 minutes;

[0045] 3. Take the dry solid obtained in step 2, put it into a muffle furnace, raise the temperature to 500°C, and calcinate for 2 hours to obtain white nano-zinc oxide matrix particles;

[0046] 4. Using an analytical balance, weigh the product obtained in step 3, suspend 1 mg of the product obtained in step 3 in 150 μl isopropanol solution, and sonicate for 10 minutes to obtain a white suspension. Using a pipette, add 1 μl o...

Embodiment 2

[0049] The nano-zinc oxide matrix and mass spectrometer sample target prepared in Example 1 were used for the analysis of free fatty acid, fatty acid methyl ester and triglyceride standard.

[0050] 1. Weigh 1 mg of the obtained nano-zinc oxide matrix material;

[0051] 2. Suspend the nano-zinc oxide obtained in step 1 in 150 μl isopropanol solution, and sonicate for 10 minutes to obtain a white suspension;

[0052] 3. Using a pipette, drop 1 μl of the white suspension onto the sample target of the mass spectrometer, and let the solvent evaporate completely;

[0053] 4. Weigh standard products such as free fatty acids, fatty acid methyl esters and triglycerides, dissolve them in n-hexane, and prepare a 10 μg / μl sample solution;

[0054] 5. Pipette 1 μl of the sample solution in step 4 and add it dropwise to the sample target obtained in step 3;

[0055] 6. In the mass spectrometry experiment, put the target with the sample added dropwise into the mass spectrometer (SYNAPT G2...

Embodiment 3

[0057] The nano-zinc oxide matrix and mass spectrometer sample target prepared in Example 1 are used for the analysis of fatty acids in vegetable oil

[0058] 1. Weigh 1 mg of the obtained nano-zinc oxide matrix material;

[0059] 2. Suspend the nano-zinc oxide obtained in step 1 in 150 μl isopropanol solution, and sonicate for 10 minutes to obtain a white suspension;

[0060] 3. Using a pipette, drop 1 μl of the white suspension onto the sample target of the mass spectrometer, and let the solvent evaporate completely;

[0061] 4. Weigh 5 mg of vegetable oil (rapeseed oil or cottonseed oil), dissolve it with n-hexane, and prepare a sample solution of 50 μg / μl;

[0062] 5. Pipette 1 μl of the sample solution in step 4 and add it dropwise to the sample target obtained in step 3;

[0063] 6. In the mass spectrometry experiment, the target with the sample added dropwise was put into a mass spectrometer (SYNAPT G2 HDMS, WATERS, USA), and the frequency of the ultraviolet laser was...

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Abstract

The invention discloses a method for analyzing and dissociating lipid molecules by laser-induced electron capture mass spectrum. The method takes nano-zinc oxide as a matrix and adopts low-energy electron generated by ultraviolet laser induction to dissociate biological sample molecules such as fatty acid, fatty acid methyl ester and triglyceride. The required nano-zinc oxide material is prepared from raw materials comprising zinc sulfate and ammonium bicarbonate by the steps of reacting at room temperature, drying, calcining and the like. The nano-zinc oxide material prepared by the method has the characteristics of uniform particles, large specific surface area, high purity, high stability and the like. The nano-zinc oxide material can effectively absorb ultraviolet light so as to induce to generate active low-energy electrons and effectively dissociate sample molecules. The obtained mass spectrum has small background interference and does not generate a series interference peaks caused by other common organic micromolecular matrix at low-mass end. The method is simple; low-energy electrons can be generated without complex instruments; the lipid micromolecules can be effectively dissociated; and sample analysis operation is simple without complex sample pretreatment.

Description

technical field [0001] The invention relates to a laser desorption dissociation mass spectrometry analysis method, in particular to a semiconductor nano-matrix and a preparation method of a mass spectrometer sample target. The principle of the present invention is based on the laser-induced electron tunneling effect of the semiconductor material ZnO (LaserActivated Electron Tunneling From Zinc Oxide), abbreviated as LAET. Background technique [0002] Mass spectrometer is a widely used analytical technology. It has high sensitivity, high accuracy and high resolution. It is a powerful tool for identifying the structure of complex organic compounds. It is widely used in chemistry, biology, medicine, environment, food, agriculture and criminal investigation. field. Since all mass spectrometers are based on the detection of gaseous charged particles, analytical dissociation of samples is one of the core technologies of mass spectrometers. [0003] In the prior art, electrospra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01J49/14G01N27/64
Inventor 钟鸿英付洁英王晓丽郑石
Owner HUAZHONG NORMAL UNIV
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