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Brivaracetam isomer detection method

A detection method and technology for isomers, applied in the field of medicine

Inactive Publication Date: 2019-06-25
成都美域高制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] In view of the fact that the existing preparation methods of buvaracetam all produce isomers, but there is no detection method for the content of isomers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Embodiment 1 high-performance liquid chromatography is measured Bu Waracetam enantiomer content

[0053] 1. Main technical parameters of high performance liquid chromatography

[0054] a. High performance liquid chromatography;

[0055] b. A chiral chromatographic column with amylose-tris(3,5-xylylcarbamate) as the stationary phase covalently bonded to the surface of silica gel;

[0056] c, mobile phase: normal hexane: ethanol: trifluoroacetic acid=85:15:0.1, flow velocity is 1.0ml / min;

[0057] d. The detection wavelength is 210nm, and the column temperature is 30°C.

[0058] 2. Detection

[0059] (1) Prepare the solution

[0060]a. The test solution: Accurately weigh 49.45mg of brivaracetam sample (batch number 20180501, provided by Chengdu Weibang Pharmaceutical Co., Ltd.), place it in a 50ml volumetric flask, dilute to the mark with the mobile phase, and use it as the test solution .

[0061] b. Control solution: Accurately measure 1.0ml of the test solution i...

Embodiment 2

[0085] Embodiment 2 high-performance liquid chromatography is measured Bu Waracetam enantiomer content

[0086] 1. Main technical parameters of high performance liquid chromatography

[0087] a. High performance liquid chromatography;

[0088] b. A chiral chromatographic column with amylose-tris(3,5-xylylcarbamate) as the stationary phase covalently bonded to the surface of silica gel;

[0089] c, mobile phase: normal hexane: ethanol: trifluoroacetic acid=85:15:0.1, flow velocity is 1.0ml / min;

[0090] d. The detection wavelength is 210nm, and the column temperature is 30°C.

[0091] 2. Detection

[0092] (1) Prepare the solution

[0093] a. The test solution: Accurately weigh 49.54mg of brivaracetam sample (batch number 20180801, provided by Chengdu Weibang Pharmaceutical Co., Ltd.), place it in a 50ml volumetric flask, dilute to the mark with the mobile phase, and use it as the test solution .

[0094] b. Control solution: Accurately measure 1.0ml of the test solution ...

experiment example 1

[0119] Experimental Example 1 System Applicability Investigation

[0120] Solution preparation: Accurately weigh the appropriate amount of Buvaracetam reference substance (batch number 20171201) and Brivaracetam isomer reference substance, and prepare it with mobile phase (the volume ratio of n-hexane:ethanol:trifluoroacetic acid is 85:15:0.1) Prepare a system suitability solution with a concentration of brivaracetam of 1.0 mg / ml and each isomer of 0.01 mg / ml. Take 20 μl of the test solution, inject it into the liquid chromatograph, inject the sample 6 times, investigate the relative standard deviation of retention time and peak area, the results are shown in Table 7.

[0121] Table 7 Summary of system suitability solution test results

[0122]

[0123] Conclusion: the test solution was injected continuously for 6 times, and the RSD of the peak area of ​​brivaracetam was 0.6%, not more than 2%, which met the requirements; the RSDs of each isomer were 1.95%, 2.73%, and 2.34...

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Abstract

The invention provides a brivaracetam isomer detection method. According to the detection method, high performance liquid chromatography is adopted. The operation process of the method includes the following steps of: (1) solution preparation; (2) detection; and (3) chromatogram analysis. According to the brivaracetam isomer detection method of the invention, specific chromatographic conditions are selected, and therefore, brivaracetam and the optical isomer impurities thereof can be separated out and detected simply and quickly, and therefore, the quality of basistatin and the preparations thereof can be controlled. With the method adopted, isomer content can be measured, and the development of a synthesis process can be guided, and the formulation of the quality standards of bulk pharmaceutical chemicals can be facilitated.

Description

technical field [0001] The invention relates to a method for detecting buvaracetam isomers, belonging to the technical field of medicine. Background technique [0002] Brivaracetam is the third-generation antiepileptic drug newly developed by Belgian drugmaker UCB, with the chemical name (S)-2-(R)-3-propylpyrrolidin-1-ylbutyramide. It is a new type of synaptophysin 2A (SV2A) high-affinity ligand, and it also has a certain inhibitory effect on voltage-dependent sodium ion channels. In 2005, brivaracetam was approved by the FDA and the European Union for the treatment of rare symptomatic myoclonic seizures. Currently, a number of phase III clinical trials including adjuvant treatment for partial seizures of epilepsy are underway. Generalized seizures have a better curative effect. [0003] The chemical structural formula of Brivaracetam is as follows: [0004] [0005] At present, the preparation process of brivaracetam almost all needs to use chiral chromatographic colu...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
Inventor 王继英陈睿宇戢颖瑶随裕敏
Owner 成都美域高制药有限公司
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