Method for detecting related substances in aniracetam raw material or aniracetam preparation

A technology of related substances and detection methods, which is applied in the field of detection of related substances of aniracetam raw materials or preparations, can solve problems such as poor stability, unseparated impurities, tailing, etc., and achieve high sensitivity, shortened time, and accurate results reliable effect

Active Publication Date: 2012-03-07
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the determination method for related substances of aniracetam raw materials and preparations has been recorded in the national standard, the quality standard number is [WS1-(X-027)-2001Z], which uses methanol-water (60:40) as the mobile phase , the main peak retention time is 4.0min, and tailing, suggesting that there may be impurities behind the main peak that have not been separated; then reduce the proportion of methanol in the organic phase in the mobile phase, and the separation between the main peak and its front and rear impurity peaks is improved, but the total analysis time is as long as 2h
At the same time, the sample has poor stability in methanol-water, and related substances increase by 0.25% within 4h

Method used

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  • Method for detecting related substances in aniracetam raw material or aniracetam preparation
  • Method for detecting related substances in aniracetam raw material or aniracetam preparation
  • Method for detecting related substances in aniracetam raw material or aniracetam preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Instruments and conditions: Agilent 1200 liquid chromatography system, DAD detector, chromatographic column: AgilentC18 (250×4.6mm, 5μm); detection wavelength: 254nm; water as mobile phase A, acetonitrile as mobile phase B, according to Table 1 Gradient elution.

[0027] Table 1 Concentration gradient of mobile phase

[0028]

[0029]

[0030] experiment procedure:

[0031] 1. System suitability test: Take about 10 mg of aniracetam raw material, put it in a 10 ml measuring bottle, add 1 ml of 3% hydrogen peroxide, heat in an oven at 60°C for 30 minutes, dilute to the mark with acetonitrile-water (1:1), Shake well, as a system suitability test solution, accurately measure 10 μl into the liquid chromatograph, record the chromatogram, see the attached HPLC chart figure 1 .

[0032] Depend on figure 1 It can be seen that the retention time of the main peak of aniracetam is 8.5 minutes, and the separation degrees of the two adjacent impurity peaks are 2.9 and 6.2, ...

Embodiment 2

[0045] Instruments and conditions: Agilent 1200 liquid chromatography system, DAD detector, chromatographic column: Welch Materials C8 (150×4.6mm, 5μm); detection wavelength: 254nm; water as mobile phase A, acetonitrile as mobile phase B, according to the table 2 for gradient elution.

[0046] Table 2 Concentration gradient of mobile phase

[0047]

[0048] Experimental procedure: take about 10 mg of aniracetam raw material, put it in a 10 ml measuring bottle, add 1 ml of 3% hydrogen peroxide, heat in a 60°C oven for 30 minutes, dilute to the mark with acetonitrile-water (8:2), shake well, and use as For the system suitability test solution, 10 μl was accurately measured and injected into a liquid chromatograph, and measured according to the detection method of the present invention.

[0049] It can be seen from the test results that the detection method of the present invention can well separate aniracetam from its most difficult oxidative degradation product, and the pea...

Embodiment 3

[0051]Instruments and conditions: Agilent 1200 liquid chromatography system, DAD detector, chromatographic column: Welch Materials C18 (250×4.6mm, 5μm); detection wavelength: 254nm; water as mobile phase A, acetonitrile as mobile phase B, according to the table 3 for gradient elution.

[0052] Table 3 Concentration Gradient of Mobile Phase

[0053]

[0054]

[0055] Experimental procedure: Take about 10 mg of aniracetam raw material, put it in a 10 ml measuring bottle, add 1 ml of 3% hydrogen peroxide, heat in a 60°C oven for 30 minutes, dilute to the mark with acetonitrile-water (9.5:0.5), shake well, and use as For the system suitability test solution, 10 μl was accurately measured and injected into a liquid chromatograph, and measured according to the detection method of the present invention.

[0056] From the test results, it can be seen that the detection method of the present invention can well separate aniracetam from its most difficult oxidative degradation pro...

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Abstract

The invention relates to a method for detecting related substances in an aniracetam raw material or an aniracetam preparation. The method for detecting related substances in an aniracetam raw material or an aniracetam preparation is characterized in that in detection, a high performance liquid chromatography is adopted; detection wavelength is 254 nanometers; a solvent is 50 to 95% of an acetonitrile aqueous solution; a chromatographic column is filled with octylsilane chemically bonded silica gel or octadecylsilane chemically bonded silica gel; a mobile phase comprises water and acetonitrile; and a gradient mobile phase elution technology is adopted. The method for detecting related substances in an aniracetam raw material or an aniracetam preparation has the advantages that a sample dissolution speed is fast; analysis time is short; mobile phase preparation processes are simple; an analysis method is stable; and sensitivity is high.

Description

technical field [0001] The invention relates to a method for detecting related substances of aniracetam raw materials or preparations. Background technique [0002] Aniracetam is a drug for improving brain function, which selectively acts on the central nervous system through the blood-brain barrier. Animal experiments have proved that aniracetam can promote the memory reproduction process of discrimination learning in normal rats, can resist memory loss caused by hypoxia, and can effectively improve memory impairment caused by certain reasons. [0003] At present, the determination method for related substances of aniracetam raw materials and preparations has been recorded in the national standard, the quality standard number is [WS1-(X-027)-2001Z], which uses methanol-water (60:40) as the mobile phase , the retention time of the main peak is 4.0min, and it tails, suggesting that there may be impurities behind the main peak that have not been separated; then the proportion...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/34
Inventor 赵志全刘阿利孙建合
Owner LUNAN PHARMA GROUP CORPORATION
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