Mass control method for clopidogrel splitting agent

A quality control method and a technology for splitting reagents, which are applied in the directions of measuring devices, material separation, and analysis materials, etc., can solve the problems of short service life of amino-bonded silica gel, high detection cost, and high price of sodium octane sulfonate. Long-term storage, high sensitivity, and high solution stability

Active Publication Date: 2013-07-03
HUIZHOU XINLITAI PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, compared with the C18 stationary phase, amino-bonded silica gel has a shorter service

Method used

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  • Mass control method for clopidogrel splitting agent
  • Mass control method for clopidogrel splitting agent
  • Mass control method for clopidogrel splitting agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The chromatographic conditions are:

[0034]

[0035] Preparation of sample solution: Accurately weigh 0.05g of solid sample, place it in a 100mL volumetric flask, add water to dissolve and dilute to the mark with water, acetonitrile or mobile phase, shake well, and the concentration of the obtained sample solution is 0.5mg / mL. Prepare 2 copies in parallel.

[0036]Preparation of reference solution: Accurately weigh different quality sodium camphorsulfonate reference substances, place them in 100mL volumetric flasks, add water to dissolve and dilute to the mark, and shake well. Prepare 2 copies in parallel.

[0037] Measuring method: draw reference substance solution and need testing solution appropriate amount respectively, inject high-performance liquid chromatograph, record and obtain as follows: figure 1 The chromatogram shown. Each solution was repeated twice, and the content of camphorsulfonic acid in the test sample was calculated by the peak area using the...

Embodiment 2

[0040] According to the method of Example 1, a 4.994 mg / mL sample solution was prepared. Dilute the sample solution with water in different proportions to make a solution with a concentration of 2, 1, 0.5, 0.1, 0.05, 0.01, and 0.005 mg / mL, and use the same chromatographic conditions as in Example 1 to measure from low concentration to high concentration. , each concentration was repeated 6 times, and the data shown in Table 1 were obtained. Taking the concentration (C) of camphorsulfonic acid as abscissa, taking the mean value (A) of the peak area of ​​camphorsulfonic acid as ordinate drawing to obtain such as figure 2 Standard curve shown. The results showed that the linear relationship of camphorsulfonic acid was good in the concentration range of 0.005-2.0 mg / mL. The regression equation is: y=205234x+1915.4, r=0.9998.

[0041] Table 1 camphorsulfonic acid linear range experimental data

[0042]

Embodiment 3

[0044] Prepare a 0.5 mg / mL sample solution according to the method in Example 1. Using the same chromatographic conditions as in Example 1, the determination was repeated 6 times to obtain the experimental data shown in Table 2. It can be seen from the results that the RSD value of the retention time of the main peak is 0.04%, and the RSD value of the peak area is 0.19%, indicating that the precision is good.

[0045] Table 2 camphorsulfonic acid precision experiment data

[0046] serial number

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Abstract

The invention provides a mass control method for a clopidogrel splitting agent of camphorsulfonic acid or camphorsulfonic acid salt. The method is characterized in that a C18 chromatographic column high performance liquid chromatography is used to separate the camphorsulfonic acid or the camphorsulfonic acid salt, then an ultraviolet detector is used for quantitative detection, the mobile phase of the C18 chromatographic column high performance liquid chromatography is acetonitrile-phosphate aqueous solution, the pH value of the mobile phase is 2.0-6.0, and the detection wavelength of the detector is 200-210 nm. The method provided by the invention has the advantages of wider linear range, higher sensitivity, good accuracy, strong repeatability, low detection cost and simplicity and convenience in operation, and is applicable to accurate quantification of the low-concentration camphorsulfonic acid or camphorsulfonic acid salt.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a quality control method for a clopidogrel resolution reagent (camphorsulfonic acid or camphorsulfonate). Background technique [0002] Camphorsulphonic acid (Camphorsulphonic acid, CAS No. 3144-16-9), the molecular formula is C 10 h 16 o 4 S is a sulfonic acid derivative of camphor, which can be prepared from camphor through sulfonation. Camphorsulfonic acid has a chiral carbon, and its optical isomer is an important chiral resolution agent, which can be applied to the resolution of the platelet aggregation inhibitor clopidogrel. For example, US Pat. No. 4,847,265 reports the separation of racemic clopidogrel by using L-camphorsulfonic acid to obtain salt-forming crystals of L-camphorsulfonic acid and S-clopidogrel. In addition, camphorsulfonic acid can also be used as a chiral ion pair reagent for the separation and analysis of chiral drugs. The structural formula of the optic...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/36
Inventor 谭端明汤妍怡
Owner HUIZHOU XINLITAI PHARMA
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