Finger print quality detecting method by intermediates of schisandra chinensis and cordycepin powder for strengthening body resistance and dissolving stasis

Finger print quality detecting method by intermediates of schisandra chinensis and cordycepin powder for strengthening body resistance and dissolving stasis

  • CN 101,708,234 A
  • Filed: 12/18/2009
  • Published: 05/19/2010
  • Est. Priority Date: 12/18/2009
  • Status: Active Application
First Claim
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1. a supporting vital QI and dispersing blood stasis Fructus Schisandrae Chinensis, fermented Cordyceps powder intermediate finger print quality detecting method comprise:

  • (1) detection method A(1) Fructus Schisandrae Chinensis, the preparation of fermented Cordyceps powder alcohol extraction intermediate test sampleTake by weighing Fructus Schisandrae Chinensis, fermented Cordyceps powder alcohol extraction intermediate 1.00 grams, put in the 10mL volumetric flask, add 50% methanol, 5~

    8ml, supersound process 20min, add 50% methanol to scale, shake up, cross the 0.45um microporous filter membrane, get the need testing solution of subsequent filtrate as Fructus Schisandrae Chinensis, fermented Cordyceps powder alcohol extraction intermediate;

    (2) gradient elution mobile phaseWith octadecylsilane chemically bonded silica is filler, and condition of gradient elution is;

    mobile phase A is 0.05% phosphoric acid-water mutually, and B is acetonitrile mutually;

    Gradient elution;

    A phase 0-60-120min, 95-60-10%, B phase 5-40-90%, flow velocity 0.8-1.2ml/min detects wavelength 254nm, and column temperature 20-40 ℃

    , sample size 10-20ul;

    (2) detection method B(1) Fructus Schisandrae Chinensis, the preparation of fermented Cordyceps powder alcohol extraction intermediate test sampleTake by weighing Fructus Schisandrae Chinensis, fermented Cordyceps powder alcohol extraction intermediate 0.50 gram, put in the 10mL volumetric flask, add water 5~

    8ml, supersound process 20min adds water to scale, shakes up, cross the 0.45um microporous filter membrane, get the need testing solution of subsequent filtrate as Fructus Schisandrae Chinensis, fermented Cordyceps powder alcohol extraction intermediate;

    (2) gradient elution mobile phaseWith octadecylsilane chemically bonded silica is filler, and condition of gradient elution is;

    mobile phase A is water mutually, and B is acetonitrile mutually;

    Gradient elution;

    A phase 0-30min, 100-93%, B phase 0-7%, flow velocity 0.8-1.2ml/min detects wavelength 261nm, and column temperature 20-40 ℃

    , sample size 10-20ul;

    (3) foundation of standard finger-printChoose medicine compositions for strengthening healthy qi to remove blood stasis Fructus Schisandrae Chinensis, the fermented Cordyceps powder alcohol extraction intermediate of 10 batches of different batches, carry out the efficient liquid-phase chromatograph finger print atlas analysis according to above-mentioned two kinds of detection methods, the medicine of each batch obtains the finger printing under 2 different wave lengths, all peaks in the HPLC finger printing are compared, determined 8 total peaks, and be numbered by appearance time precedence;

    Wherein, among the finger printing a that under the 254nm wavelength, obtains according to detection method A, 4 total peaks (1~

    No. 4 peak) have been determined;

    Among the finger printing b that under the 261nm wavelength, obtains according to detection method B, 4 total peaks (5~

    No. 8 peaks) have been determined;

    Confirm in the total peak, No. 2 peak schisandrins, No. 3 peaks are schisantherin B, and No. 4 peaks are deoxyschizandrin, and No. 6 peaks are uridnine, and No. 7 peaks are guanosine, No. 8 peaks are adenosine;

    (4) quality control of finger printingUnder the 254nm wavelength, obtain finger printing a according to detection method A,, the HPLC finger printing and the standard finger-print of sample compared, should be with the similarity that 4 total peaks calculate less than 0.8;

    Under the 261nm wavelength, obtain finger printing b according to detection method B,, the HPLC finger printing and the standard finger-print of sample compared, should be with the similarity that 4 total peaks calculate less than 0.8.

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