A kind of salvianolic acid A compositions and prepare medicinal usage

A kind of salvianolic acid A compositions and prepare medicinal usage

  • CN 103,083,305 B
  • Filed: 11/20/2012
  • Issued: 04/27/2016
  • Est. Priority Date: 11/20/2012
  • Status: Active Grant
First Claim
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1. the preparation method of a salvianolic acid A compositions, it is characterized in that:

  • in wherein said compositions, salvianolic acid A content is greater than 93%, be less than 100%, and also comprise 4 other compositions by following weight proportion;

    alkannic acid 0.1% ~ 2%, rosmarinic acid 0.1% ~ 2%, salvianolic acid B 0.1% ~ 2%, salvianolic acid C 0.1% ~ 2%, described salvianolic acid A compositions adopts lower preparation method to obtain;

    Get red rooted salvia, be cut into decoction pieces or be ground into diameter 1mm ~ 5mm granule, add 3 ~ 15 times amount at every turn, 45 ~ 95 DEG C of water temperature lixiviates are got, stir with 10 ~ 50 revs/min of speed simultaneously, or add 3 ~ 15 times amount water boiling and extraction, extract 1 ~ 3 time altogether, extract 1 ~ 4 hour at every turn;

    Extracting solution is evaporated to relative density and is determined as 1.0 ~ 1.25 at 60 DEG C, adds ethanol and makes alcohol content 50% ~ 85%, leaves standstill, and filter, decompression filtrate recycling ethanol is also concentrated into without alcohol taste, obtains Radix Salviae Miltiorrhizae extract;

    OrGet red rooted salvia, be cut into decoction pieces or be ground into diameter 1mm ~ 5mm granule, add 3 ~ 15 times amount 30% ~ 60% alcohol reflux at every turn, extract 1 ~ 4 hour at every turn, extract 1 ~ 3 time altogether;

    Decompression recycling ethanol is also concentrated into without alcohol taste, obtains Radix Salviae Miltiorrhizae extract;

    Above-mentioned Radix Salviae Miltiorrhizae extract is diluted with water to every 1ml containing salvianolic acid B 1 ~ 30mg, and aqueous solution adjusting PH with base to 3.5 ~ 6.5, add with salvianolic acid B molar percentage 0.1 ~ 3% zinc chloride as catalyst, transforms 1 ~ 6 hour at 100 ~ 140 DEG C of heating temperatures;

    Conversional solution adjust pH to 2.5 ~ 4.5, leave standstill, centrifugal, supernatant is evaporated to every 1ml containing salvianolic acid A 1 ~ 10mg, be separated through HPD-100 macroporous resin column chromatography, salvianolic acid A applied sample amount is 1;

    35 ~ 1;

    70 with macroporous adsorbent resin ratio, resin column blade diameter length ratio is 1;

    4 ~ 1;

    30, use 1 ~ 8 times of cylinder hydrops respectively, 1 ~ 10 times of column volume 10% ~ 40% ethanol elution, removing impurity, use 2 ~ 10 times of column volume 20% ~ 60% ethanol elutions again, HPLC detects, collect 20% ~ 60% ethanol elution part containing salvianolic acid A, decompression recycling ethanol is also concentrated into without alcohol taste,Aqueous solution is concentrated into the solution of every 1ml containing 1-10mg salvianolic acid A, be separated by polyamide chromatography post, salvianolic acid A applied sample amount is 1;

    5 ~ 1;

    25 with polyamide ratio, resin column blade diameter length ratio is 1;

    4 ~ 1;

    25, use 1 ~ 10 times of cylinder hydrops, the remove impurity of 5 ~ 20 times of column volume 20% ~ 60% alcoholic solution eluting respectively, use 4 ~ 15 times of column volume 40% ~ 90% alcoholic solution eluting again, collect 40% ~ 90% alcoholic solution part containing salvianolic acid A, decompression recycling ethanol is also concentrated into without alcohol taste aqueous solution;

    Aqueous solution concentrates, acid adjustment pH to 2.0 ~ 4.0, by the t-butyl methyl ether of aqueous solution 1-8 times amount, and point 2 ~ 6 extractions, be separated organic layer, reclaim under reduced pressure t-butyl methyl ether, make the extract of every 1ml containing salvianolic acid A 1g ~ 10g, add 1 ~ 3 times amount silica gel, stir, volatilize;

    Stirring sample silica gel is added on the dry silicagel column of 5 ~ 20 times amount installed, silicagel column blade diameter length ratio is 1;

    4 ~ 1;

    25, with pentane-t-butyl methyl ether for eluant, gradient elution, be pentane-t-butyl methyl ether eluting 6 ~ 30 times column volume of 4;

    6 respectively by volume ratio, volume ratio is pentane-t-butyl methyl ether eluting 6 ~ 30 times column volume of 6;

    4, reclaim under reduced pressure eluant, the salvianolic acid A reclaimed after organic solvent adds 5 ~ 20 times amount water dissolutioies, microwave vacuum drying, obtains described salvianolic acid A compositions.

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