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N-(1-naphthyl) ethylenediamine dinitrate and preparation method and application thereof

A technology of naphthaleneethylenediamine nitrate and naphthaleneethylenediamine hydrochloride, which is applied in the fields of organic synthesis and mass spectrometry detection, and can solve the problems of long time consumption, poor repeated use effect, and decline in analysis effect

Active Publication Date: 2013-12-11
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When desorption / ionization occurs on the porous silicon surface, the surface of the silicon crystal must first be etched to produce a nanostructured surface. Although peptides and antiviral drugs can be directly analyzed on such a surface, the repeated use of this surface is not effective. OK, so repeated treatments on the same nanostructured surface are required to get a reusable surface
In addition, it takes a long time to chemically modify the surface of porous silicon, and the analysis effect will be greatly reduced when the modified porous silicon is reused.

Method used

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  • N-(1-naphthyl) ethylenediamine dinitrate and preparation method and application thereof
  • N-(1-naphthyl) ethylenediamine dinitrate and preparation method and application thereof
  • N-(1-naphthyl) ethylenediamine dinitrate and preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0031] The preparation of embodiment 1, naphthalene ethylenediamine nitrate

[0032] At room temperature, 33.50mg of naphthaleneethylenediamine hydrochloride and 44.71mg of AgNO 3 (Naphthylethylenediamine hydrochloride and AgNO 3 The molar ratio is 1:2) to 1.200ml of ethanol / water with a volume ratio of 30:70, so that the two are mixed uniformly by ultrasound and reacted; during the reaction, white AgCl precipitates will be produced; when the white AgCl When the precipitation no longer increases, it indicates that the reaction is complete, the supernatant liquid of the upper layer is the ethanol / water solution of naphthalene ethylenediamine nitrate, and the precipitate of the lower layer is AgCl. After separating and filtering out the precipitate AgCl, the ethanol / water solution of naphthaleneethylenediamine nitrate in the upper layer is passed through 732 type strongly acidic cation exchange resin, and the effluent is pure ethanol / water solution of naphthaleneethylenediamine...

Embodiment 2

[0036] Embodiment 2, the molecular weight of sucrose is measured as matrix with the naphthalene ethylenediamine nitrate prepared in embodiment 1

[0037](1) Dissolving 3.41 mg of sucrose with 1.000 ml of methanol / water solution with a volume ratio of 50:50 to obtain methanol / water solution of sucrose, the molar concentration of the solution is 10 mmol / L;

[0038] (2) directly use the ethanol / water solution of the naphthalene ethylenediamine nitrate prepared by embodiment 1, the molar concentration of this solution is 100mmol / L;

[0039] (3) get mixed solution after each 10 μ L of the ethanol / water solution of the sucrose solution prepared in step (1) and the ethanol / water solution of step (2) naphthalene ethylenediamine nitrate, and obtain mixed solution, the mol ratio of naphthalene ethylenediamine nitrate and sucrose in the mixed solution The ratio is 10:1; then draw 1 μL of the above mixed solution to apply the sample, and inject the sample after the solvent in the mixed so...

Embodiment 3

[0042] Embodiment 3, with the naphthalene ethylenediamine nitrate prepared in embodiment 1 as the molecular weight of substrate measurement Gly-Ala

[0043] (1) Dissolving 2.48 mg of Gly-Ala with 1.697 ml of ethanol / water solution with a volume ratio of 30:70 to obtain a molar concentration of Gly-Ala solution of 10 mmol / L;

[0044] (2) directly use the ethanol / water solution of the naphthalene ethylenediamine nitrate prepared by embodiment 1, the molar concentration of this solution is 100mmol / L;

[0045] (3) get the solution of Gly-Ala prepared by step (1) and the ethanol / water solution of step (2) naphthalene ethylenediamine nitrate and mix each 10 μ L to obtain the mixed solution, and in this mixed solution, naphthalene ethylenediamine nitrate and Gly- The molar ratio of Ala is 10:1; then draw 1 μL of the above mixed solution to apply the sample, and inject the sample after the solvent in the mixed solution is completely evaporated in the air. It was analyzed by MALDI-TOF...

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Abstract

The invention provides N-(1-naphthyl) ethylenediamine dinitrate, and a preparation method and application thereof. The structural formula of the N-(1-naphthyl) ethylenediamine dinitrate is shown as a formula (I) described in the specification; the preparation method of the N-(1-naphthyl) ethylenediamine dinitrate comprises the following step of: reacting N-(1-naphthyl) ethylenediamine dihydrochloride and silver nitrate to obtain the N-(1-naphthyl) ethylenediamine dinitrate; and the invention further provides the application of the N-(1-naphthyl) ethylenediamine dinitrate to determining the molecular weight of compounds in MALDI-TOF MS (Matrix-Assisted Laser Desorption / Ionization Time of Flight Mass Spectrometry).

Description

technical field [0001] The invention relates to naphthaleneethylenediamine nitrate and a preparation method and application thereof, belonging to the fields of organic synthesis and mass spectrometry detection. Background technique [0002] Since Karas et al. and Tanaka et al. reported in 1988 that matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) technology can be used for effective mass spectrometry analysis of biological macromolecules, MALDI-TOF MS technology has been favored by researchers from various countries. of favor. However, since the commonly used matrices of MALDI-TOF MS technology are small molecular organic compounds, such as α-cyano-4-hydroxycinnamic acid (CCA), 2,5-dihydroxybenzoic acid (DHB), sinapinic acid (SA), 3-Hydroxy-2-pyridinecarboxylic acid (3-HPA), anthracenol (DI) and 3-aminoquinoline (3-AQ), etc. In the analysis process, because the above-mentioned matrix molecules are prone to fragmentation and associ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/58C07C209/00G01N27/64G01N21/31G01N21/33
Inventor 聂宗秀陈芮徐文军熊彩侨
Owner INST OF CHEM CHINESE ACAD OF SCI
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