A kind of preparation method of Salinomycin Sodium fine work

A kind of preparation method of Salinomycin Sodium fine work

  • CN 104,447,789 B
  • Filed: 12/15/2014
  • Issued: 09/14/2018
  • Est. Priority Date: 12/15/2014
  • Status: Active Grant
First Claim
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1. a kind of preparation method of Salinomycin Sodium fine work, which is characterized in that steps are as follows:

  • (1) pH is adjusted:

    By salinomycin zymotic fluid sodium hydroxide tune pH value to 6.5-8.0, salinomycin is made to be generated as sodium salt;

    (2) it filters:

    The zymotic fluid that plate-frame filtering step (1) is handled well, the salinomycin zymotic fluid chemical titer are 75000-Moisture in zymotic fluid is removed, obtains the filter cake containing Salinomycin Sodium by 80000u/mL;

    (3) it extracts:

    By 5-8m3Methanol is added into pot for solvent extraction for the ratio of methanol/ton Salinomycin Sodium filter cake, then puts into filter cake, stirsIt mixes 30-60 minutes, filters, collect methanol extract liquid;

    Isometric methanol solution is added into pot for solvent extraction, extracts 20-40 againMinute, filtering is collected methanol extract, is mixed with first time methanol extract, is concentrated for lower step;

    The third leaching:

    With sameIt is primary that the methanol solution of volume extracts filter cake again, and 300u/mL should be less than by detecting salinomycin content in filter cake, stopped extraction, obtainedLeaching liquor be used for lower batch of product production;

    (4) it concentrates:

    By the leaching liquor extracted twice before step (3) in 55-65 DEG C of temperature, vacuum degree is not less than 0.03MPaUnder be concentrated into the 1/5 of original volume, stop concentration;

    (5) it crystallizes:

    Under stirring at normal temperature state, by purified water/concentrate volume ratio 1;

    Purifying is added into concentrate for 2 ratioWater, you can obtain the crystallization of Salinomycin Sodium, centrifugation separates Salinomycin Sodium from liquid to get Salinomycin Sodium crude product;

    (6) it refines:

    Under room temperature, the crude product acetone solution that step (5) is obtained, crude product:

    Acetone=1;

    3-4 (w/v, kilogram/It rises);

    Activated carbon is added into lysate in the ratio of 3% kg/liter of quality percent by volume again, then stirs 15-30 minutes,Filtrate is obtained by filtration, then concentrates the filtrate to 2 times of amount volumes of crude product weight;

    Under stirring, by purified water/concentrated liquidProduct ratio 1;

    10 ratio is added purified water and obtains crystal solution, and decrease temperature crystalline centrifuges, and centrifugation 20-50 rises methanol leaching every timeThe Salinomycin Sodium washed on bowl inner wall crystallizes to get Salinomycin Sodium wet product;

    (7) it dries:

    Salinomycin Sodium wet product is positioned over 60-70 DEG C, dries 6-8 hours in the baking oven of vacuum degree >

    =0.06MPa, i.e.,Obtain Salinomycin Sodium fine work.

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