Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Derivatization reagent and application thereof

A technology of derivatization reagents and chemical bonds, which is applied in the field of analysis and detection, can solve the problems of few types of derivatization reagents, difficult quantitative analysis, and uneven derivatization efficiency, so as to avoid co-competitive ionization, improve the ionization efficiency of mass spectrometry, and widely The effect of developing application prospects

Active Publication Date: 2021-04-23
CHINA PHARM UNIV
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the sensitivity of mass spectrometry of existing derivatization reagents is not high enough, and the detection performance of trace analytes is not good, and the derivatization efficiency of different subtypes of molecules in a class of substances is uneven, making it difficult to quantitatively analyze
In addition, there are few types of derivatization reagents, the general synthetic route is long, the steps are cumbersome, and the yield is low

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Derivatization reagent and application thereof
  • Derivatization reagent and application thereof
  • Derivatization reagent and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0085] Example 1: Synthesis of compound 1 in formula II: N2, N2, N4, N4-tetramethyl-2,4-diamino-6-(4-phenylsulfonylpiperazine)-1,3,5- Triazine (TMTPP):

[0086] (1), the preparation of intermediate 2,4-diamino-6-(4-nitrophenyl)-1,3,5-triazine:

[0087] Add 2g of p-nitrobenzonitrile, 1.3g of dicyandiamide and 0.3g of potassium hydroxide into the three-necked flask, add 300mL of absolute ethanol, put in a magnet, place it in an oil bath at 78°C, and reflux for 3 hours. After the reaction is completed, cool to room temperature, add absolute ethanol to wash, filter, precipitate solid, evaporate and dry in the air, the obtained solid is the intermediate 2,4-diamino-6-(4-nitrophenyl)-1,3 , 5-triazine, the productive rate is 96.7%;

[0088] (2), preparation of intermediate N2, N2, N4, N4-tetramethyl-2,4-diamino-6-(4-nitrophenyl)-1,3,5-triazine:

[0089] Add 1.48g sodium hydride and 80mL N,N-dimethylformamide into the three-necked flask, then add 2g 2,4-diamino-6-(4-nitrophenyl)-1,...

Embodiment 2

[0096] Example 2, Compound 1 is used for the analysis and detection of acylcarnitine:

[0097] Take the blank control, 5-dimethylaminonaphthalene-1-sulfonylpiperazine and N2, N2, N4, N4-tetramethyl-2,4-diamino-6-(4-phenylsulfonylpiperazine) respectively -1,3,5-triazine was prepared as 9mM, and 20uL of it was taken respectively, mixed with 20uL of 500ng / mL 11 straight-chain acylcarnitine mixed standard solution, 20uL of 3mM HATU and 40uL of acetonitrile / water (1:1), Vortex for 5 minutes, mix well, heat the reaction at 47°C for 150 minutes, centrifuge at 20,000g for 10 minutes, take 20uL of the supernatant and inject it into HPLC-MS / MS for analysis;

[0098] The results show that it can be seen that the underivatized blank control, the short-chain acylcarnitine does not retain, the same concentration of N2, N2, N4, N4-tetramethyl-2,4-diamino-6-(4-benzene The mass spectrum response value of sulfonylpiperazine)-1,3,5-triazine is 3 to 4 times that of 5-dimethylaminonaphthalene-1-s...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention discloses a derivatization reagent and application thereof. The invention relates to the field of analysis and detection, and the concrete structure of the derivatization reagent is represented by general formula I shown in the description. The derivatization reagent can chemically react with a specific group of a mass spectrum difficult-to-detect molecule to generate a corresponding mass spectrum easy-to-detect derivative, so the problems of limited sensitivity, low specificity and the like of some molecules difficult to detect by mass spectrometry at the present stage are effectively solved, and the mass spectrometry detection analysis of the molecules difficult to detect is realized.

Description

technical field [0001] The invention relates to the field of analysis and detection, in particular to a class of derivatization reagents, their synthesis and use in derivatization-type mass spectrometry sensitization reagents. Background technique [0002] The history of mass spectrometry can be traced back to the end of the 19th century. The discovery of positively charged particles and the deflection of positively charged particle beams in a magnetic field laid the experimental foundation for the birth of mass spectrometry. With the advancement of technology, mass spectrometry, especially its method combined with chromatography and computer, has been widely used in organic chemistry, biochemistry, drug metabolism, clinical, toxicology, pesticide determination, environmental protection, petrochemistry, geochemistry, In the fields of food chemistry, phytochemistry, cosmic chemistry and national defense chemistry, in the research of pharmacology and biology, the existence of ...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N27/62
CPCG01N30/02G01N30/06G01N30/72G01N27/62G01N2030/067
Inventor 许风国焦宇李思奇
Owner CHINA PHARM UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com