Preparation method of high-purity refined salinomycin sodium salt

Preparation method of high-purity refined salinomycin sodium salt

  • CN 104,447,789 A
  • Filed: 12/15/2014
  • Published: 03/25/2015
  • Est. Priority Date: 12/15/2014
  • Status: Active Application
First Claim
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1. a preparation method for high purity Salinomycin Sodium fine work, is characterised in that, step is as follows:

  • (1) adjust pH;

    by Salinomycin. fermented liquid with sodium hydroxide adjust pH to 6.5-8.0, make Salinomycin. be generated as sodium salt;

    (2) filter;

    the fermented liquid that Plate Filtration step (1) is handled well, by the moisture removing in fermented liquid, obtain the filter cake containing Salinomycin Sodium;

    (3) lixiviate;

    by 4-8m 3the ratio of methyl alcohol/ton Salinomycin Sodium filter cake adds methyl alcohol in pot for solvent extraction, then drops into filter cake, stirs 30-60 minute, filters, and collects methanol extract;

    In pot for solvent extraction, add isopyknic methanol solution, again lixiviate 20-40 minute, filter, collect methanol extract, mix with first time methanol extract, concentrate for lower step;

    Third time lixiviate;

    with the methanol solution of same volume again lixiviate filter cake once, detecting Salinomycin. content in filter cake should lower than 300u/mL, and stop lixiviate, the vat liquor obtained is for the production of lower batch of product;

    (4) concentrated;

    the vat liquor front for step (3) twice lixiviate obtained is temperature 55-65 DEG C, and vacuum tightness is concentrated into 1/5 of original volume under being not less than 0.03MPa, stop concentrated;

    (5) crystallization;

    under stirring at normal temperature state, adds purified water in the ratio of purified water/concentrated solution volume ratio 1;

    2, can obtain the crystallization of Salinomycin Sodium in concentrated solution, is centrifugally separated from liquid by Salinomycin Sodium, obtains Salinomycin Sodium crude product;

    (6) refining;

    under normal temperature, by the crude product acetone solution that step (5) obtains, crude product;

    acetone=1;

    3-4 (w/v, kg/liter);

    The ratio of pressing 1-3% (w/v, kg/liter) again adds gac in lysate, then stirs 15-30 minute, filters and obtains filtrate, then filtrate is concentrated into 2 times amount volumes of crude product weight;

    Under whipped state, add purified water in the ratio of purified water/concentrated solution volume ratio 1;

    10 and obtain crystal solution, decrease temperature crystalline, centrifugation, obtain Salinomycin Sodium wet product;

    (7) dry;

    by Salinomycin. wet product bake drying, obtain Salinomycin Sodium fine work.

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