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Method for decomposing chiral mobile phase additive RP-HPLC of fudosteine enantiomer

A mobile phase additive, RP-HPLC technology, applied in the field of analytical chemistry, can solve the problems of cumbersome and time-consuming derivatization reaction, expensive CSP column, etc., and achieve the effect of quality control

Inactive Publication Date: 2008-04-16
NANJING MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

①The method is simple and fast, but the CSP column is expensive; ②The method requires chiral derivatization reagents with high optical purity, and the derivatization reaction is often cumbersome and time-consuming; ③The method is simple and cheap

Method used

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  • Method for decomposing chiral mobile phase additive RP-HPLC of fudosteine enantiomer
  • Method for decomposing chiral mobile phase additive RP-HPLC of fudosteine enantiomer
  • Method for decomposing chiral mobile phase additive RP-HPLC of fudosteine enantiomer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Instruments and Conditions 1

[0026] Shimadzu 10Avp high performance liquid chromatograph, octadecylsilane bonded silica gel as filler, L-phenylalanine solution (take L-phenylalanine 1.0g, copper sulfate 1.3g, add water 1000ml to dissolve) as Mobile phase, UV detection wavelength is 275nm, detection limit 1ug / ml, see Figure 4.

[0027] Implementation steps

[0028] Take an appropriate amount of fudosteine ​​racemate, add mobile phase solution to make a solution containing 5mg per 1ml. Take 20 μl and inject it into a liquid chromatograph, the peak order is D-(+)-enantiomer first, L-(-)-enantiomer last, and the separation degree between enantiomers is greater than 1.5. The number of theoretical plates calculated based on the L-(-)-enantiomer peak should not be less than 1000. The area ratio of the front to back peaks of the enantiomers in the recorded chromatogram should be 0.5-2. Generally, the retention time of the D-(+)-enantiomer is about 9 minutes, and the reten...

Embodiment 2

[0030] Get fudosteine ​​appropriate amount, add mobile phase solution and make the solution that contains fudosteine ​​5mg in every 1ml, as need testing solution; Under the chromatographic condition of embodiment 1, measure need testing solution 20 μ l injection liquid phase Chromatograph, the retention time of the main peak in the chromatogram of the test solution should be consistent with the retention time of the L-(-)-enantiomer peak of racemic fudosteine, see Figure 3, 5-6.

Embodiment 3

[0032] Get an appropriate amount of fudosteine ​​tablet powder, add mobile phase solution to make a solution containing 5mg of fudosteine ​​in every 1ml, as the test solution. Under the chromatographic condition of embodiment 1, measure need testing solution 20 μ l and inject liquid chromatograph, the main peak retention time in need testing solution chromatogram should be with the L-(-)-enantiomer of racemic fudosteine The peak retention time is consistent, see Figure 3, 5-7.

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Abstract

The present invention belongs to analytical chemistry field, and relates to separation and determination of Fudosteine and the enantiomer thereof (impurity). The present invention adopts RP-HPLC method, and adds a chiral metal synergist into a chromatogram flow phase system to form a tri-diastereoisomer coordination compound, because the obtained diastereoisomer coordination compound has stable structure with energy difference and capability to carry out three-dimensional selective absorption and repulsion reaction with the fixed phase, the two enantiomers can be separated from each other. The method can separate and determine Fudosteine and the enantiomer thereof (impurity), thereby making the quality of both Fudosteine and the agent containing Fudosteine controllable.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring fudosteine ​​and preparation enantiomers (impurities) by high performance liquid chromatography. Background technique [0002] Fudosteine ​​is a new type of expectorant, which belongs to a class of compounds with an expectorant effect created by SSP Pharmaceutical Co., Ltd. in 1988 with a basic skeleton of steine. Its structure contains a closed sulfhydryl group , is metabolized into active free thiol derivatives in the body to play a role. Its basic role is to inhibit the proliferation of goblet cells and regulate the normal state of mucus and mucosa in the respiratory tract. It was first launched in Japan on December 17, 2001, and is manufactured by Mitsubishi Pharmaceuticals and S.S Pharmaceuticals. The dosage form is 200 mg tablet, and the trade names are respectively: Cleanal TABLETS (Mitsubishi Pharmaceutical Co., Ltd.), SPELEAR ta...

Claims

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Application Information

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IPC IPC(8): C07C323/58C07C319/28C07B57/00
Inventor 周学敏马静袁丽华陈婷
Owner NANJING MEDICAL UNIV
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