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A method for analyzing and separating 2,4-dicyano-3-isobutylglutaramide by high performance liquid chromatography

A technology of isobutylglutaramide and high performance liquid chromatography, applied in the field of analytical chemistry, to achieve the effect of quality control

Active Publication Date: 2022-04-08
WUHAN WUYAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no relevant report on the analysis and separation of 2,4-dicyano-3-isobutylglutaramide

Method used

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  • A method for analyzing and separating 2,4-dicyano-3-isobutylglutaramide by high performance liquid chromatography
  • A method for analyzing and separating 2,4-dicyano-3-isobutylglutaramide by high performance liquid chromatography
  • A method for analyzing and separating 2,4-dicyano-3-isobutylglutaramide by high performance liquid chromatography

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Embodiment 1

[0031] This embodiment provides a method for analyzing and separating 2,4-dicyano-3-isobutylglutaramide by high performance liquid chromatography, comprising the following steps:

[0032] (1) Chromatographic conditions: high performance liquid chromatography: Diana: UltiMate3000; column: SB-CN (250mm×4.6mm); mobile phase: acetonitrile: water = 40:60, adjust the pH to 6; flow rate: 1.0ml / min; Detection wavelength: 205nm; Column temperature: 25°C;

[0033] (2) Take the sample containing 2,4-dicyano-3-isobutylglutaramide, dissolve the sample with mobile phase, and prepare the concentration of 2,4-dicyano-3-isobutylglutaramide 2.5mg / ml sample solution;

[0034] (3) Get 10 μ l of the obtained sample solution of step (2) and inject it into a high-performance liquid chromatograph to complete the analysis and separation of 2,4-dicyano-3-isobutylglutaramide (results are shown in the appendix figure 1 ).

Embodiment 2

[0036] Instruments and Conditions

[0037] High-performance liquid chromatography: Dianne: UltiMate3000;

[0038] Chromatographic column: SB-CN (250mm×4.6mm);

[0039] Mobile phase: methanol: water = 40:60, adjust the pH to 6;

[0040] Flow rate: 1.0ml / min;

[0041] Detection wavelength: 205nm;

[0042] Column temperature: 25°C;

[0043] Injection volume: 10 μl.

[0044] Experimental procedure

[0045] (1) Weigh 50mg of 2,4-dicyano-3-isobutylglutaramide, place it in a 20ml volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as a sample solution;

[0046] (2) Take the sample solution, carry out high-performance liquid chromatography analysis according to the above conditions, and record the chromatogram. see attached results figure 2 , figure 2 Peak No. 1 is 2,4-dicyano-3-isobutylglutaramide, and peak No. 2 is impurity. It can be seen that 2,4-dicyano-3-isobutylglutaramide and impurities are well separated. And the main peak ...

Embodiment 3

[0048] Instruments and Conditions

[0049] High-performance liquid chromatography: Dianne: UltiMate3000;

[0050] Chromatographic column: SB-CN (250mm×4.6mm);

[0051] Mobile phase: acetonitrile: water = 30:70, adjust the pH to 6;

[0052] Flow rate: 1.0ml / min;

[0053] Detection wavelength: 205nm;

[0054] Column temperature: 35°C;

[0055] Injection volume: 10 μl.

[0056] Experimental procedure

[0057] (1) Weigh 50mg of 2,4-dicyano-3-isobutylglutaramide, put it in a 20ml volumetric flask, add mobile phase to dissolve and dilute to the mark, shake well, and use it as the sample solution.

[0058] (2) Take the sample solution, carry out high-performance liquid chromatography analysis according to the above conditions, and record the chromatogram. see attached results image 3 , image 3 Peak No. 1 is an impurity peak, peak No. 2 is cyanoacetamide, peak No. 3 is 2,4-dicyano-3-isobutylglutaramide, and peak No. 4 is an impurity peak. It can be seen that under this con...

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Abstract

The invention discloses a method for analyzing and separating pregabalin intermediate 2,4-dicyano-3-isobutylglutaramide by HPLC, belonging to the field of analytical chemistry. Adopting the method of the present invention can effectively separate 2,4-dicyano-3-isobutylglutaramide and related substances introduced during its synthesis process, thereby controlling 2,4-dicyano-3-isobutylglutaramide The mass of butyl glutaramide, the accurate determination of the content of 2,4-dicyano-3-isobutyl glutaramide, the indication of the stability of 2,4-dicyano-3-isobutyl glutaramide. The method established by the invention has strong specificity, high accuracy and simple operation.

Description

technical field [0001] The invention belongs to the field of analytical chemistry, and relates to a high-performance liquid phase analysis and separation method, in particular to a high-performance liquid chromatography (HPLC) method for analyzing and separating 2,4-dicyano-3-isobutylglutaramide. Background technique [0002] Pregabalin, chemically known as (S)-3-(aminomethyl)-5-methylhexanoic acid, is a morphine analog used to treat epilepsy and nerve pain, and is also used for anxiety, social phobia, arthritis . 2,4-dicyano-3-isobutylglutaramide is an intermediate of pregabalin and an important indicator for controlling the quality of pregabalin. Its structural formula is [0003] [0004] Using cyanoacetamide and isovaleraldehyde as raw materials, 2,4-dicyano-3-isobutylglutaramide obtained by suction filtration after reaction and crystallization under certain conditions will introduce related substances, whether it is in pregabalin Both raw materials and preparation...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/54
CPCG01N30/02G01N30/06G01N30/54G01N2030/027G01N2030/062
Inventor 赵涛涛徐煜涵张伟王成冯路平张琦谢国范吴鸣
Owner WUHAN WUYAO PHARMA
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