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

Separation method of sulfonic acid combination

A technology of sulfonic acid conjugate and separation method, applied in the field of preparation of sulfonic acid conjugate, can solve the problem of lack of an effective method for rapid separation of sulfonic acid conjugate monomer, and achieve wide applicability, simple and efficient operation, and simple operation. Effect

Active Publication Date: 2013-09-18
ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
View PDF2 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is still a lack of effective methods for the rapid separation of sulfonic acid conjugate monomers, so it is necessary to develop a practical, rapid, and highly selective separation of target sulfonic acid conjugates.

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
  • Separation method of sulfonic acid combination
  • Separation method of sulfonic acid combination
  • Separation method of sulfonic acid combination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1, the preparation of pregnenol ketone sulfonic acid conjugate, as follows:

[0024]

[0025] 1) Preparation of isolated samples by biotransformation method: Pregnenolone was dissolved in methanol to form a 5mg / ml stock solution, 20ml was taken out and phosphate buffer salt of pH 7.4 was added, after stirring, rat liver cytoplasm ( RLC), adding sulfonic acid group donor PAPS, the final concentration of bufagenin in the system is 0.10mg / ml, the final concentration of protein is 0.5mg / ml, the final concentration of PAPS is 0.2mM, and incubated in a constant temperature water bath at 37°C for 2h. After the substrate conversion rate reached 50% as detected by HPLC, the reaction solution was transferred to a -80°C refrigerator for cooling. Take 100ml of the reaction solution and put it directly on the flash chromatography column. The filler of the flash chromatographic column is a mixed filler, wherein the silica gel is bonded with phenyl groups, the particle ...

Embodiment 2

[0027] Embodiment 2, the preparation of esterbufaxin sulfonic acid conjugates, as follows:

[0028]

[0029] Bufagenin was dissolved in dimethyl sulfoxide (DMSO) to make a 5 mg / ml stock solution, 20 ml was taken out and phosphate buffer salt of pH 7.4 was added, after stirring, human recombinant monoenzyme rhSULT2A1 was added in turn, and sulfonium The acid group donor PAPS, the final concentration of bufagenin in the system is 0.10mg / ml, the final concentration of protein is 0.25mg / ml, the final concentration of PAPS is 0.2mM, and the mixture is stirred and incubated in a constant temperature water bath at 37°C for 2h. After the substrate conversion rate reached 50% as detected by HPLC, the reaction solution was transferred to a -80°C refrigerator for cooling. Take 100ml of the reaction solution and put it directly on the flash chromatography column. The filler of the flash chromatographic column is a mixed filler, wherein the silica gel is bonded with phenyl groups, the ...

Embodiment 3

[0030] Example 3, Preparation of daphnetin sulfonated metabolites

[0031]

[0032] Daphnetin was dissolved in methanol to make a 5mg / ml stock solution, 30ml was taken out and added to phosphate buffer salt with pH 7.4, after stirring, it was added to rat intestine S9 (RIS9) in turn, and PAPS, a sulfonic acid group donor, was added to the system The final concentration of daphnetin was 0.10 mg / ml, the final concentration of protein was 0.5 mg / ml, the final concentration of PAPS was 0.2 mM, and the mixture was stirred and incubated in a constant temperature water bath at 37°C for 1 hour. After the substrate conversion rate reached 50% as detected by HPLC, the reaction solution was transferred to a -80°C refrigerator for cooling. Take 100ml of the reaction solution and put it directly on the flash chromatography column. The filler of the flash chromatographic column is a mixed filler, in which silica gel is bonded with phenyl groups, the particle size is 40 μm, and the dosage ...

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

PropertyMeasurementUnit
Particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention discloses a separation method of a sulfonic acid combination. The separation method of the sulfonic acid combination comprises the following step of: separating the acidity dependence of a hydroxy compound as well as a sulfonic acid combination thereof rapidly by taking a mixture of a substrate of the hydroxy compound (containing phenolic hydroxyl group and alcoholic hydroxyl group) after chemical derivation or biological conversion as raw materials in virtue of chromatographic columns filled by composite materials, and meanwhile through utilizing eluents with different pH values. The separation method of the sulfonic acid combination provided by the invention has wide application in preparing the sulfonic acid combination, and is suitable for the purification and preparation of all sulfonic acid combinations which contain phenolic (alcohol) hydroxyl group, but not contain acidity groups.

Description

technical field [0001] The invention belongs to the technical field of medicine, and particularly provides a preparation method of a sulfonic acid conjugate. Background technique [0002] Drug metabolism is the most important way for the body to defend against the invasion of foreign substances, and is considered to be an important biochemical barrier for the body to resist foreign harmful substances. Sulfonate-binding metabolism is an important type II-binding metabolic reaction in the body. It is involved in the biotransformation of endogenous small molecules (such as steroids, catecholamines, arachidic acids, etc.) and exogenous substances (such as drugs) play an important role (Naunyn Schmiedebergs Arch Pharmacol 2004; 369:55-68; Toxicol Sci 2006; 90:5-22.). After most drugs undergo sulfonic acid conjugation reactions, the resulting sulfonated conjugates have higher solubility than the substrates, so they are easier to excrete from the body, thereby reducing drug effica...

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): B01D15/10C07B45/02C07B63/00C12P33/00C12P33/20C12P17/06
Inventor 杨凌宁静葛广波朱亮亮
Owner ZHANGJIAGANG IND TECH RES INST CO LTD DALIAN INST OF CHEM PHYSICS CHINESE ACADEMY OF SCI
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