Preparation method of montmorillonite preparations

Preparation method of montmorillonite preparations

  • CN 102,406,657 B
  • Filed: 09/26/2010
  • Issued: 03/27/2013
  • Est. Priority Date: 09/26/2010
  • Status: Active Grant
First Claim
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1. the preparation method of a montmorillonite preparation is characterized in that preparing montmorillonite preparation with the Montmorillonitum crude drug that meets following technical standard:

  • Natural bentonite is got through washing refining being processed into by Montmorillonitum system, is hydrated aluminium silicate salt;

    [character] Montmorillonitum crude drug is canescence or for yellow fine powder, adds the abnormal smells from the patient that water has clay after moistening, and color burn;

    Almost insoluble in water, diluted acid or alkali hydroxide test solution;

    [discriminating] (1) gets the Montmorillonitum crude drug and each 0.5g of calcium fluoride puts in the same platinum crucible, and it is moistening to add sulphuric acid 1ml, covers crucible with the surface plate that adds 1 in water, if necessary slowly heating, and the adularescent colloid generates on the water droplet surface;

    (2) it is an amount of to get the Montmorillonitum crude drug, x-ray powder diffraction is measured, the X ray diffracting spectrum of Montmorillonitum should be consistent with the Montmorillonitum collection of illustrative plates of international X-ray pounder diff action archives, and other impurity peaks intensity must not be higher than the characteristic peak at about 0.45nm place of Montmorillonitum in the collection of illustrative plates;

    (3) solution under the aluminium sesquioxide assay item should show the identification of aluminum salt;

    [inspection] acid-base value is got Montmorillonitum crude drug 0.20g, adds water 20ml, puts on the boiling water bath and heats after 2-3 minute, lets cool, and filters, and gets filtrate and measures by 2005 editions two appendix VI H of Chinese Pharmacopoeia, and pH value should be 5.0-9.0;

    Chloride is got Montmorillonitum crude drug 0.20g, adds 1 in water 25ml and nitric acid, boils 5 minutes, filter, get filtrate and check according to two appendix VIIIA of Chinese Pharmacopoeia version in 2005, with concentration be the contrast liquor ratio made of 0.025% standard chloride solution 5.0ml, must not be denseer;

    Carbonate is got Montmorillonitum crude drug 0.2g, puts in the test tube, adds water 2ml and makes it suspendible, the acetum 2ml that adds 2mol/L, rapidly with the close plug of stopper with the glass bend pipe, slowly heating, escaping gas is imported in the calcium hydroxide test solution, must not the adularescent precipitation produce;

    Solute is got Montmorillonitum crude drug 2.0g in the water, adds water 50mL, boils 5 minutes, and adds water and be adjusted to 50mL, lets cool, and after filtering with filter paper, with the microporous membrane filtration of 0.45 μ

    m, the filtrate water bath method is dried to constant weight at 105 ℃

    , leaves over residue and must not cross 14mg again;

    Loss on drying is got the Montmorillonitum crude drug, is dried to constant weight at 105 ℃

    , subtracts weight loss between 5-10%;

    Granularity is measured according to 2010 editions attached IX E three therapeutic methods of traditional Chinese medicine of Chinese Pharmacopoeia, and mean diameter or meso-position radius must not be greater than 15 μ

    m, and particle diameter is not less than 90% less than the accumulative total percentage rate of the granule of 35 μ

    m, and specific surface area must not be less than 8000cm2/cm 3Heavy metal is got Montmorillonitum crude drug 4.0g, adds acetate buffer 4ml and the water 46ml of pH3.5, boils, let cool, add water and make into 50ml, filter, get filtrate 25ml, check according to 2005 editions appendix VIII of Chinese Pharmacopoeia H first method, contain heavy metal and must not cross 10/1000000ths;

    Arsenic salt is got Montmorillonitum crude drug 1.0g, adds hydrochloric acid 5ml and water 23ml, checks that according to Chinese Pharmacopoeia version appendix in 2005 VIII J first method arsenic salt must not cross 2/1000000ths;

    Swelling degree is got Montmorillonitum crude drug 1.0g in the 100ml band plug graduated cylinder that adds 40ml, adds water to 75ml scale place again.The jam-pack stopper shakes up 3 minutes, and sample is fully scattered, and adds the 1mol hydrochloric acid solution of 25ml, and jolting 5 minutes was left standstill 24 hours, read the scale value at precipitate interface, was swelling degree;

    Swelling degree should be 10-25ml;

    Absorption affinity is measured with the cation exchange capacity method, and cation exchange capacity should be at 70-150mmol/100g;

    Microorganism is limited the quantity of and is got the Montmorillonitum crude drug, according to the test of 2005 editions two appendix XI J of Chinese Pharmacopoeia microbial limit detection method, and should be up to specification;

    [assay] Montmorillonitum crude drug is pressed dry product and is calculated, and contains silicon dioxide and should be 55%-65%, contains aluminium sesquioxide and should be 12%-25%;

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