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Method for resolution of racemization 2-chloropropionic acid by adopting capillary electrophoresis separation-diode array detection technique

A technology of capillary electrophoresis and diode array is applied in the direction of material analysis, measurement device, analysis material, etc. by electromagnetic means, which can solve the problems of high cost, easy hydrolysis of the coating, toxic and side effects, etc., and achieves simple operation, good separation, Simple to use effects

Inactive Publication Date: 2015-10-07
HUBEI BIOCHEM PHARMA TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the pesticides and pharmaceutical intermediates synthesized from 2-chloropropionic acid and its ester racemate may be in the form of competitive inhibitors due to their enantiomers with low or ineffective or toxic side effects If it works, it will not only reduce the efficacy of the medicine, but also aggravate environmental pollution, reduce the quality of agricultural products, and may also produce toxic side effects, leading to drug damage or drug resistance.
[0003] At present, the commonly used method for the resolution of chiral drugs is chromatographic separation, in which thin-layer chromatography is simple and easy to popularize, but its accuracy is poor; gas chromatography has high separation efficiency and high detection sensitivity, but the disadvantage is that the analyte must have Volatile and thermally stable, currently there are few types of chiral capillary columns, high cost, and easy hydrolysis of the coating; high performance liquid chromatography is currently the dominant chiral separation method, but chiral liquid chromatography columns are expensive, Column efficiency is low

Method used

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  • Method for resolution of racemization 2-chloropropionic acid by adopting capillary electrophoresis separation-diode array detection technique

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of buffer solution: adjust the phosphoric acid solution with a concentration of 150 mmol / L to pH 7.0 with 0.33 mol / L Tris buffer solution to obtain the final product;

[0031] (2) Preparation of electrophoresis running buffer solution: Add chiral resolving agent, organic solvent and cationic surfactant to the buffer solution prepared in step (1) respectively, and mix with ultrasonic to obtain capillary electrophoresis running buffer solution; Described chiral resolving agent is 2-HP-β-CD, and its concentration is 110 mmol / L in buffer solution; Described organic solvent is acetonitrile, and the volume fraction in buffer solution is 5%; Described cationic surface Active agent is CTAB, and its concentration in the buffer solution is 0.2 mmol / L;

[0032] (3) Standard stock solution of R / S-chloropropionic acid: prepare standard stock solutions of R-2-chloropropionic acid and S-2-chloropropionic acid with ultrapure water, the concentration is 30mmol / L, store ...

Embodiment 2

[0037] The concentration of the phosphoric acid solution in step (1) of Example 1 was replaced by 100 mmol / L, and adjusted to pH 6.0 with 0.2 mol / L Tris buffer;

[0038] The chiral resolving agent in step (2) of Example 1 was replaced by β-cyclodextrin, and its concentration in the buffer solution was 25 mmol / L; the organic solvent was replaced by methanol, and the volume fraction in the buffer solution was 3%;

[0039] Replace the concentration of R-2-chloropropionic acid and S-2-chloropropionic acid standard stock solution prepared in step (3) of Example 1 with 20mmol / L;

[0040] The remaining steps are the same as in Example 1, and the retention time of R-2-chloropropionic acid and S-2-chloropropionic acid obtained is slightly different from that of Example 1. The separation degree of the two optical isomers in this example is 2.40.

Embodiment 3

[0042] The concentration of the phosphoric acid solution in step (1) of Example 1 was replaced by 130mmol / L, and adjusted to pH 8.0 with 0.4 mol / L Tris buffer;

[0043] Replace the chiral resolving agent in step (2) of Example 1 with β-cyclodextrin, and its concentration in the buffer solution is 25 mmol / L; replace the organic solvent with absolute ethanol, the volume in the buffer solution The score is 10%;

[0044] Replace the concentration of R-2-chloropropionic acid and S-2-chloropropionic acid standard stock solution prepared in step (3) of Example 1 with 50mmol / L;

[0045] The remaining steps are the same as in Example 1, and the retention time of R-2-chloropropionic acid and S-2-chloropropionic acid is slightly different from that of Examples 1 and 2, and the degree of separation of the two optical isomers is 2.37.

[0046] Investigate enantiomeric separation retention time, peak area reproducibility, the results are as follows: 1. Standard deviation of retention t...

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Abstract

The invention discloses a method for resolution of racemization 2-chloropropionic acid by adopting a capillary electrophoresis separation-diode array detection technique. The method comprises the steps of: adding a chiral resolution agent, an organic solvent and a cation surfactant into a prepared buffer solution respectively and performing ultrasonic mixing to obtain a capillary electrophoresis operation buffer solution; using the buffer solution as an electrophoresis medium for resolution to obtain R-2-chloropropionic acid and S-2-chloropropionic acid monomers; calculating an enantiomer excessive value according to a chromatogram peak area; monitoring product quality according to the value. The method can achieve base line separation of the R-2-chloropropionic acid and S-2-chloropropionic acid monomers, and has the characteristics of good separation degree, low cost and simple and convenient operation.

Description

technical field [0001] The present invention relates to a method for splitting the racemic body of a compound, in particular to a method for splitting racemic 2-chloropropionic acid using capillary electrophoresis separation-diode array detection technology; R-2-chloropropionic acid and S-2-chloropropionic acid monomers are separated from chloropropionic acid. Background technique [0002] 2-chloropropionic acid (2-chloropropionic acid or 2-chloro-panoic acid) is an important raw material for the synthesis of pesticides, dyes and agricultural and forestry chemicals. Its application involves many sectors of the national economy and people's daily life. It is an important fine chemical products. 2-chloropropionic acid has been an important component of a large number of herbicides that have been widely used in agriculture since the 1850s. 2-chloropropionic acid is also used to produce lower alcohol esters such as anti-inflammatory, antipyretic and analgesic ibuprofen, pharm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/447G01N21/25
Inventor 周兴旺石小杉张闻艺胡红
Owner HUBEI BIOCHEM PHARMA TECH
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