quality detection method of desepidine

quality detection method of desepidine

  • CN 101,042,381 B
  • Filed: 04/28/2007
  • Issued: 01/08/2014
  • Est. Priority Date: 04/28/2007
  • Status: Active Grant
First Claim
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1. the detection method of a deserpidine is characterized in that:

  • 1) detection method of the content of deserpidine and related substance, chromatographic condition and system suitability;

    with octadecylsilane chemically bonded silica, be filling agent;

    Acetonitrile-1% ammonium chloride of take is mobile phase in the ratio of 50;

    50;

    Detect wavelength 272nm;

    Number of theoretical plate calculates and should be not less than 3000 by the deserpidine peak;

    Content determination;

    the test sample precision takes deserpidine 10mg, put in the 25ml volumetric flask, add mobile phase and dissolve and be diluted to scale, shake up, precision measures in 1ml to 50ml volumetric flask, add mobile phase and be diluted to scale, shake up, obtain, as need testing solution, get the deserpidine reference substance, with method operation, product solution in contrast;

    Get 20 μ

    l injection liquid chromatographies, record chromatogram;

    With calculated by peak area, obtain deserpidine assay check result by external standard method;

    Determination of related substances method;

    get deserpidine accurately weighed, add mobile phase and make in every 1ml solution containing 80 μ

    g as need testing solution;

    Precision measures 1ml and puts in the 100ml volumetric flask, adds mobile phase and dissolves and be diluted to scale, shakes up, in contrast solution;

    According to the chromatographic condition under the assay item, get contrast solution 20 μ

    l injection liquid chromatographies, regulate detection sensitivity, make the major component peak height be about 10%~

    20% of full scale, get again each 20 μ

    l of need testing solution and contrast solution, injection liquid chromatography respectively, record to major component peak retention time 3 times of chromatogram;

    2) detection method of deserpidine enantiomter, chromatographic condition and system suitability;

    with kromasil 100-5-DMB, be filling agent;

    Take containing the methylene chloride of 1% acetic acid and hexane is mobile phase in the ratio of 38;

    62;

    Flow velocity;

    1.0ml/min, column temperature;

    30 ℃

    , detect wavelength 272nm;

    Number of theoretical plate calculates and should be not less than 3000 by the deserpidine peak;

    Determination method;

    get deserpidine 6mg and put in the 10ml measuring bottle, add the mobile phase ultrasonic dissolution, be diluted to scale, shake up, as the need testing solution precision, measure need testing solution 1.0ml, put in the 100ml measuring bottle, add mobile phase and be diluted to scale, shake up, in contrast solution;

    Precision measures contrast liquid 10 μ

    l, the injection liquid chromatography, regulate detection sensitivity, and making the major component peak height is 10%~

    20% of full scale, precision measures need testing solution and reference substance solution 10 μ

    l injection liquid chromatographies again, records to major component peak retention time 3 times of chromatogram.

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