Method for analyzing biological samples by using matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectra

A technology of ion cyclotron resonance and matrix-assisted laser, which is applied to the analysis of materials, the preparation of test samples, and the analysis of materials by electromagnetic means, and can solve problems that have not been reported.

Inactive Publication Date: 2011-09-07
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the past, isotope derivatization reagents have been used to label amino acids, peptides, estrogens and fatty acids,...

Method used

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  • Method for analyzing biological samples by using matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectra
  • Method for analyzing biological samples by using matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectra
  • Method for analyzing biological samples by using matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectra

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Example 1: Derivatization reaction and analysis of metabolites in urine samples

[0060] The operation steps are as follows:

[0061] Divide 1-2mL urine sample into two equal parts, add 100-200μL 2M acetic acid-sodium acetate buffer (pH5.4-5.8) and 50-100μL β-glucosidase / sulfatase to each, and digest at 37-55℃ for 3h , add 2.5-5mL of tert-butyl methyl ether (TBME) to extract twice, combine the organic layers and blow dry with nitrogen, first add 50-100μL 10-40% pyridinedichloromethane solution, and then mix with 50-100μL 10 -40% trifluoromethanesulfonic anhydride dichloromethane mixed reaction for 5-20min, the second part was added 5-100μL 10-40% deuterated pyridine dichloromethane solution, and then mixed with 50-100μL 10-40% trifluoromethane Methanesulfonic anhydride and dichloromethane were mixed and reacted for 5-20 minutes. After mixing the two reaction solutions, they were mixed with 100-200 mg / mL matrix DHB acetone solution at a volume ratio of 1:3, and analyzed...

Embodiment 2

[0069] Embodiment 2: hair sample derivatization reaction and analysis

[0070] The operation steps are as follows:

[0071] Wash the hair with distilled water, dichloromethane and isopropanol, dry at 50-60°C, cut the hair into 1-2mm, weigh 0.3-0.4mg, add 200-500μL 6M sodium hydroxide and methanol (1:1), 60 Hydrolyze at -70°C for 1-2 hours, divide into two equal parts, add dichloromethane solution to extract twice, combine the organic layer and blow dry with nitrogen, add 50-100 μL 10-40% pyridine dichloromethane solution to the first part, and then Mix and react with 50-100 μL 10-40% trifluoromethanesulfonic anhydride dichloromethane for 5-20 minutes, add 50-100 μL 10-40% deuterated pyridine dichloromethane solution to the second part, and then mix with 50-100 μL 10- 40% trifluoromethanesulfonic anhydride and dichloromethane were mixed and reacted for 5-20 minutes. The two reaction solutions were mixed and then mixed with 100-200 mg / mL matrix DHB acetone solution at a volume ...

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Abstract

The invention relates to a method for analyzing biological samples by using matrix assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectra (MALDI-FTMS), which is a method for analyzing alcohol compounds or/and alpha,beta-unsaturated ketone compounds in hair and urine samples qualitatively and quantitatively by combining a N-alkyl pyridine isotope derivatization method with the MALDI-FTMS. The method comprises the following steps of: performing sample preprocessing on a target analyte; reacting alcoholic hydroxyl or alpha,beta-unsaturated ketone on the target analyte with pyridine or deuterated pyridine; and performing MALDI-FTMS analysis on the marked sample solution directly. The analytical method is quick, efficient and sensitive.

Description

technical field [0001] The present invention relates to a biological sample matrix-assisted laser desorption ionization-Fourier transform ion cyclotron resonance mass spectrometry discovery method, and further refers to an N-alkylpyridine isotope derivatization method combined with matrix-assisted laser desorption ionization-Fourier transform ion cyclotron Resonance mass spectrometry (MALDI-FTMS) analysis is a method for qualitative or quantitative analysis of alcohol compounds and α, β-unsaturated ketone compounds in biological hair and urine samples. It is a fast, efficient and sensitive method for discovery. To further determine the relationship between the content changes of such compounds in the body and physiological functions and diseases will lay a foundation. technical background [0002] Alcohols and α, β-unsaturated ketones such as cholesterol, fatty alcohols, vitamin A, steroid hormones, etc. are important metabolites in the human body and are related to the func...

Claims

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Application Information

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IPC IPC(8): G01N27/62G01N1/28C07D213/20C07J3/00C07J7/00C07J9/00C07J1/00
Inventor 郭寅龙汪航张立张菁王昊阳刘素红
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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