Chitosan modified paramagnetic metal ion magnetic resonance imaging contrast agent preparation method

Chitosan modified paramagnetic metal ion magnetic resonance imaging contrast agent preparation method

  • CN 101,642,579 B
  • Filed: 08/14/2009
  • Issued: 10/23/2013
  • Est. Priority Date: 08/14/2009
  • Status: Active Grant
First Claim
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1. the preparation method of chitosan modified paramagnetic metal ion magnetic resonance imaging contrast medium is characterized in that carrying out according to the following steps:

  • (1) in reaction vessel;

    add the polyamines polycarboxylic acid solid of certain mass and the anhydrous acetic acid acid anhydride of certain volume;

    add again anhydrous pyridine as catalyst;

    logical drying nitrogen protection;

    sucking filtration behind 55~

    60 ℃

    of lower stirring reaction 24 h is used respectively anhydrous acetic acid acid anhydride, anhydrous N, N '"'"'-dimethyl formamide and absolute ether washing;

    obtain the polycarboxylic corresponding anhydride of polyamines, wherein the ratio of polyamines polycarboxylic acid and anhydrous acetic acid acid anhydride counts 1 with quality and volume ratio ;

    1~

    3;

    The polyamines polycarboxylic acid is diethylenetriamine pentaacetic acid or ethylenediaminetetraacetic acid;

    (2) at anhydrous N, add water-soluble chitosan or Narrow Molecular Weight Distribution water-soluble chitosan in N '"'"'-dimethyl formamide or the dimethyl sulfoxide, add again DMAP or triethylamine or pyridine as catalyst, add the polyamines polycarboxylic acid anhydride for preparing in the step (1) under the stirring at normal temperature, wherein the mol ratio of chitosan and polyamines polycarboxylic acid anhydride is 1 ;

    1~

    5, under room temperature, stir 36~

    72 h, add distilled water after the ice bath cooling and continue to stir 12~

    120 h, vacuum concentration adds dehydrated alcohol and separates out faint yellow solid, vacuum drying to small size;

    (3) take by weighing Sephadex G-25 type gel, dress post after the activation, in a small amount of distilled water, wherein solid and distilled water ratio count 1 with quality and volume ratio with resulting dissolution of solid in the step (2) ;

    2~

    100, upper prop, take distilled water as eluting solvent, the colour developing of 0.1% 1,2,3-indantrione monohydrate butanol solution, detect with uv analyzer, the detection wavelength is 254nm, occurs two eluting peaks in the process of eluting, and the eluting peak of part at first goes out post, it is collected final vacuum be concentrated into small size, add dehydrated alcohol after the cooling and get faint yellow precipitation, filter, vacuum drying gets the part powder;

    (4) take by weighing that resulting part powder dissolution is in distilled water in the step (3), wherein part powder and distilled water ratio count 1 with quality and volume ratio ;

    5~

    20, stir lower adding metal inorganic salt, the mol ratio of part and metal inorganic salt is 1 ;

    1~

    5, under room temperature, continue to stir 2~

    24 h, with solution for vacuum concentration, add the dehydrated alcohol precipitation after the cooling, washing and filtering obtains the pressed powder 0.3~

    3.0g of magnetic resonance imaging contrast agent after the drying;

    Wherein said metal inorganic salt is Gd 3+Salt, Mn 2+Salt, Fe 3+Salt.

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