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A kind of isomer detection method of camphorsulfonic acid or its salt

A technology of camphorsulfonic acid and detection method, which is applied in the field of detection, can solve problems such as the detection and analysis of camphorsulfonic acid or its salt, and achieve the effects of smooth baseline, good separation and high stability

Active Publication Date: 2021-02-02
CHENGDU BRILLIANT PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Existing detection method is difficult to detect and analyze the isomer of camphorsulfonic acid or its salt, the present invention studies a kind of isomer detection method of camphorsulfonic acid or its salt

Method used

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  • A kind of isomer detection method of camphorsulfonic acid or its salt
  • A kind of isomer detection method of camphorsulfonic acid or its salt
  • A kind of isomer detection method of camphorsulfonic acid or its salt

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Experimental program
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Effect test

Embodiment 1

[0037] Take an appropriate amount of L-camphorsulfonic acid test product, accurately weighed, dissolve and dilute with methanol to a solution containing about 5 mg of L-camphorsulfonic acid per 1 ml, as the test solution; accurately pipette an appropriate amount of the test solution, and dilute with methanol A solution containing about 50 μg of levocamphorsulfonic acid per 1 ml was used as a control solution. In addition, accurately weigh an appropriate amount of the reference substance of camphorsulfonic acid racemate, dissolve it with methanol and dilute it into a solution containing about 2.5 mg each of L-camphorsulfonic acid and D-camphorsulfonic acid per 1 ml, as a system suitability solution. According to the test of high performance liquid chromatography (Chinese Pharmacopoeia 2015 edition four general rules 0512), the silica gel with quinidine derivatives bonded on the surface is used as filler (Daicel Chiralpak ZWIX (-) 250mm×4mm, 3μm or equivalent chromatographic colu...

Embodiment 2

[0039] Methodological Study on Isomers of Levocamphorsulfonic Acid

[0040] 1. Analytical method establishment

[0041] 1.1 Overview

[0042] L-camphorsulfonic acid is a chiral resolving agent used in the synthesis of voriconazole, which plays a key role in the formation of the chiral center of voriconazole. From the synthesis route of L-camphorsulfonic acid, it can be seen that the enantiomers of L-camphorsulfonic acid are more likely to remain than D-camphorsulfonic acid. In combination with the opinions issued by the Food and Drug Administration on voriconazole, the optical purity of L-camphorsulfonic acid is controlled by a specific method requirements. An HPLC method was established to control the content of enantiomers in L-camphorsulfonic acid.

[0043] 1.2 Screening and optimization

[0044] 1.2.1 Method preliminary screening

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Abstract

The invention discloses a method for detecting isomers of camphorsulfonic acid or its salts. The detection method uses high performance liquid chromatography to qualitatively or quantitatively detect the isomers of camphorsulfonic acid or its salts. The detection conditions include: Chromatographic column: ion exchange column; detection wavelength: 210~400nm; mobile phase: organic phase containing acid and diethylamine, the acid is formic acid or acetic acid, and the detection method also includes the following steps: (1) preparing the Test solution, reference substance solution; (2) need test solution, reference substance solution sample injection detection respectively; Described need test solution is the isomer solution of camphorsulfonic acid or its salt, preferably L-camphorsulfonic acid solution or / and D-camphorsulfonic acid solution, more preferably L-camphorsulfonic acid solution. Adopting the method of the invention has good separation degree and high theoretical plate number.

Description

technical field [0001] The invention relates to the field of detection methods, in particular to a method for detecting isomers of camphorsulfonic acid or its salts. Background technique [0002] Camphorsulfonic acid has prismatic crystals and is a pair of chiral optical enantiomers, which are divided into left-handed camphorsulfonic acid and right-handed camphorsulfonic acid, with melting points at 193-195°C and 197-200°C, respectively. [0003] [0004] Camphorsulfonic acid or its salt is an important organic synthesis intermediate and optical resolution agent. Due to its optical activity, it can be used for the racemization of optical isomers in industry, and it is also widely used as a pharmaceutical intermediate, such as for the production of intestinal disorder inhibitors and H1V improving agents. Left and right camphorsulfonic acid or its salts are used as important resolving agents for optically active amino acid drugs, such as using camphorsulfonic acid or its s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 周一帆童庆国罗鸣李英富苏忠海
Owner CHENGDU BRILLIANT PHARMA CO LTD
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