Method for preparing hydroxysafflor yellow A

Method for preparing hydroxysafflor yellow A

  • CN 102,127,124 B
  • Filed: 12/27/2010
  • Issued: 04/22/2015
  • Est. Priority Date: 12/27/2010
  • Status: Active Grant
First Claim
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1. a preparation method for hydroxyl radical carthamin yellow carthamus A, is characterized in that following these steps to carry out:

  • A, extraction;

    the dried floral getting safflower, add the deionized water of 15-20 times of weight, and 30-60 minute are soaked in temperature 80 DEG C of water-baths, and by water refluxing extraction 2 times, united extraction liquid, is evaporated to 50% of extracting liquid volume, obtains extracting solution;

    B, separation;

    extracting solution is added mass ratio 3-10% absorptive clarificant chitosan or 101 fruit juice clarifiers or the removal of impurities of ZTC II natural clarifying agent, upper macroporous adsorbent resin, when effluent liquid Molish reaction is negative, be that 20-50% ethanol carries out wash-out by concentration, obtain safflower crude extract, wherein macroporous adsorbent resin is D-4020 or AB-8 or D-141 or D-201 or HPD500 model;

    Or extracting solution is directly gone up macroporous adsorbent resin, when effluent liquid Molish reaction is negative, be that 20-50% ethanol carries out wash-out by concentration, obtain safflower crude extract, wherein macroporous adsorbent resin is D-4020 or AB-8 or D-141 or D-201 or HPD500 model;

    C, high-speed countercurrent chromatography are separated;

    adopt high-speed counter-current chromatograph, chromatographic instrument is separated the solvent that solvent systems is formed by two-phase or three phase components, that propyl carbinol or Pentyl alcohol and hydrochloric acid form two-phase respectively, or propyl carbinol or Pentyl alcohol and methyl alcohol or ethanol and hydrochloric acid composition three-phase, wherein each volume components is than being 1-3;

    0-2;

    0.5-2, and hydrochloric acid is 0.05-0.2mol/L;

    D, solvent systems is configured in separating funnel, stratification after shake well, get upper strata phase solution as stationary phase, lower floor'"'"'s phase solution is as moving phase, crude extract is dissolved in the mixing solutions of upper strata phase and lower floor'"'"'s phase, make to be full of stationary phase in high-speed counter-current chromatograph pillar, then its main frame is made to rotate, again moving phase is pumped into post, the mixing solutions that crude extract is dissolved in the upper and lower is entered again by sampling valve, retention time is 100-200 minute, the high-speed counter-current chromatograph flow rates used is 1-3ml/min, speed range is 700-1000 revolution, according to the detected result receiving target composition hydroxyl radical carthamin yellow carthamus A of detector spectrogram or high performance liquid chromatography,E, purifying deacidify;

    the sample hydroxyl radical carthamin yellow carthamus A obtained by high-speed counter-current carries out column chromatography, the blade diameter length ratio of pillar is 1;

    50-100, ultrapure water is with the flow velocity wash-out of 0-3ml/min, collect orange-yellow colour band stream part, concentrate drying under temperature 30-80 DEG C of condition, can obtain hydroxyl radical carthamin yellow carthamus A dry powder, the filler wherein in column chromatography selects sephadex lh-20 or LH-60 or G-25 model.

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