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Synthesis method of alpha-cyan-4-hydroxycinnamic acids modified silicon-containing matrix

A technology of hydroxycinnamic acid and synthesis method, applied in the field of synthesis of nano-silicon materials

Inactive Publication Date: 2014-03-26
INST OF HYGIENE & ENVIRONMENTAL MEDICINE PLA ACAD OF MILITARY MEDICAL
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Problems solved by technology

[0002] Although commonly used matrix-assisted laser desorption ionization (MALDI) matrices such as CHCA, 2,5-dihydroxybenzoic acid, sinapinic acid, etc. have achieved success in the analysis of biological macromolecules, but because the matrix itself will also be ionized during the ionization process, Therefore, the strong background in the low-mass range (usually <600Da) affects the analysis of low-molecular-weight substances to a large extent. Exploring and synthesizing new matrices suitable for the detection of small-molecule targets will further expand the application range of MALDI-TOF MS. has an important role

Method used

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  • Synthesis method of alpha-cyan-4-hydroxycinnamic acids modified silicon-containing matrix
  • Synthesis method of alpha-cyan-4-hydroxycinnamic acids modified silicon-containing matrix

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Experimental program
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Effect test

Embodiment approach 1

[0023] (1) Accurately weigh 1.0 mmol of CHCA in a 100 ml three-necked flask, add 30 ml of methanol, and stir for 15 minutes under nitrogen protection at room temperature, then add 1.0 mmol of 3-APTES solution dropwise, and continue stirring for 1 hour;

[0024] (2) Add 0.5g SBA-15, stir to make the system evenly mixed, then heat up to 60°C and reflux for 12h;

[0025] (3) The reacted system was centrifuged, the supernatant was removed, the precipitate was shaken and washed 6 times with 40 ml of methanol, and vacuum-dried at 60° C. for 6 hours to obtain the product.

Embodiment approach 2

[0027] (1) Weigh 0.5g of dried SBA-15 into a 100ml three-necked flask, add 15ml of toluene, add 1.0mmol of 3-APTES dropwise, stir evenly, heat up to 80°C, and reflux for 15h under nitrogen protection;

[0028] (2) Suction filter the reacted system, wash with 40ml of toluene and isopropanol for 3 times, extract for 20min, and vacuum-dry the filter cake at 80°C for 10h to obtain amino-modified SBA-15;

[0029] (3) Weigh 1.0 mmol of CHCA into a 100 ml three-neck flask, add 30 ml of methanol, and stir under nitrogen protection at room temperature for 15 min, add the dried amino-modified SBA-15, and stir at room temperature for 3 h;

[0030] The reacted system was centrifuged to remove the supernatant, the precipitate was shaken and washed 6 times with 40 ml of methanol, and vacuum-dried at 60° C. for 6 hours to obtain the product.

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Abstract

The invention provides a synthesis method of an alpha-cyan-4-hydroxycinnamic acids (CHCA) modified silicon-containing matrix, aiming at overcoming the shortcoming that relatively high background interference of the matrix always appears in a process of detecting a micromolecule target object through MALDI (Matrix-assisted Laser Desorption Ionization). The synthesis method comprises two schemes, wherein the first scheme is characterized in that CHCA firstly reacts with 3-aminopropyltriethoxysilane (3-APTES) to produce ionic liquid, and 3-APTES is hydrolyzed and combined with SBA-15 through a silanol bond at the same time; the other scheme is characterized is that SBA-15 is firstly combined with 3-APTES to realize amination and then reacted with CHCA to form an ion complex. The novel matrix synthesized by the synthesis method is applied to MALDI-TOF MS ((Matrix-Assisted Laser Desorption / Ionization Time of Flight Mass Spectrometry), the shortcoming that relatively high background interference of the matrix always appears in the process of detecting the micromolecule target object through MALDI can be avoided, and the signal strength and signal reproducibility of a micromolecule object to be detected can also be improved; the synthesis method has a good application prospect.

Description

technical field [0001] The invention relates to a method for synthesizing a modified nano-silicon material, in particular to a method for synthesizing an SBA-15 nano-silicon matrix modified by alpha-cyano-4-hydroxycinnamic acid (CHCA). Background technique [0002] Although commonly used matrix-assisted laser desorption ionization (MALDI) matrices such as CHCA, 2,5-dihydroxybenzoic acid, sinapinic acid, etc. have achieved success in the analysis of biological macromolecules, but because the matrix itself will also be ionized during the ionization process, Therefore, the strong background in the low-mass range (usually <600Da) affects the analysis of low-molecular-weight substances to a large extent. Exploring and synthesizing new matrices suitable for the detection of small-molecule targets will further expand the application range of MALDI-TOF MS. has an important role. Contents of the invention [0003] The purpose of the present invention is to overcome the disadvan...

Claims

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Application Information

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IPC IPC(8): C01B33/021B82Y30/00
Inventor 周焕英高志贤苏璇刘飞刘忠文张亦红陈风春刘芳
Owner INST OF HYGIENE & ENVIRONMENTAL MEDICINE PLA ACAD OF MILITARY MEDICAL
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