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Preparation method of amboryl ester type sugar marker with permanent charges and application

A technology of succinate and markers, which is applied in the field of preparation of permanently charged succinate sugar markers, can solve the problems of high cost of derivatization reagents, inability to show higher sensitivity and detection intensity, and achieve mild reaction conditions and high sensitivity. Good, simple synthetic route

Inactive Publication Date: 2017-11-28
EZHOU INST OF IND TECH HUAZHONG UNIV OF SCI & TECH +1
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Chemical derivatization plays an important role in the research of proteomics and glycomics. Although the development of detection instruments is changing rapidly, without the assistance of various derivatization techniques, many peptides or sugars that exist in trace amounts cannot be detected. Not only In this way, the derivatized samples cannot show higher sensitivity and detection intensity in the detection
[0003] Samples with permanent charges can eliminate the interference of sodium ions and potassium ions during ionization and dissociation, and can

Method used

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  • Preparation method of amboryl ester type sugar marker with permanent charges and application
  • Preparation method of amboryl ester type sugar marker with permanent charges and application
  • Preparation method of amboryl ester type sugar marker with permanent charges and application

Examples

Experimental program
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Embodiment 1

[0018] a. Weigh 1g of ethyl p-aminobenzoate into a two-necked round bottom flask, add 40ml of acetone to dissolve, then add 3.6g of anhydrous potassium carbonate and 14.1g of methyl iodide, and react under nitrogen protection at 80°C and stir and reflux for 24 hours , the reaction is completed, filter the reaction solution, get the filtrate, extract with dichloromethane, dewater the organic phase with magnesium sulfate, filter the magnesium sulfate and then evaporate and concentrate, the product is separated and purified by chromatography (mobile phase dichloromethane:methanol=20 :1), obtain product A.

[0019] b. Add 10% sodium hydroxide to the resultant A in step a, just do not pass the reactant, use 95% ethanol as solvent, reflux reaction at 85°C for 6 hours, adjust the pH to weak acidity with 1M hydrochloric acid, and concentrate the reaction solution , add anhydrous acetone to dissolve, filter, take the precipitate, and dry it in vacuum to obtain product B;

[0020] c. A...

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Abstract

The invention provides a preparation method of an amboryl ester type sugar marker with permanent charges and belongs to the technical field of organic synthesis and bioinformation. The amboryl ester type sugar marker with permanent charges is prepared from benzocaine through a series of synthesis, has the advantages that the reaction conditions (45 DEG C for 40 min) are mild, detection sensitivity can be improved and deviation yield is high, the deviation yield reaches 98%, the product can be detected with HPLC (high-performance liquid chromatography and MS (mass spectrometry) (ESI-MS and MALDI-ToF-MS), and the sensitivity is high.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis and biological information, and in particular relates to a preparation method of a permanently charged succinate sugar marker. Background technique [0002] Chemical derivatization plays an important role in the research of proteomics and glycomics. Although the development of detection instruments is changing rapidly, without the assistance of various derivatization techniques, many peptides or sugars that exist in trace amounts cannot be detected. Not only In this way, the derivatized samples cannot show higher sensitivity and detection intensity in the detection. [0003] Samples with permanent charges can eliminate the interference of sodium ions and potassium ions during ionization and dissociation, and can also improve detection sensitivity. The commonly used derivatization reagent TMPP (tris(2,4,6-trimethoxyphenyl) Phosphoniumacetic acid N-hydroxysuccinimide ester ) is the applic...

Claims

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Application Information

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IPC IPC(8): C07D207/404G01N30/02G01N30/06
CPCC07D207/404G01N30/02G01N30/06
Inventor 张译芳
Owner EZHOU INST OF IND TECH HUAZHONG UNIV OF SCI & TECH
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