Method for purifying vincoside lactam

Method for purifying vincoside lactam

  • CN 106,518,940 A
  • Filed: 11/07/2016
  • Published: 03/22/2017
  • Est. Priority Date: 11/07/2016
  • Status: Active Application
First Claim
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1. it is a kind of purification vincoside-lactam method, it is characterised in that comprise the steps:

  • (1) prepare Fructus Camptothecae Acuminatae crude extractAfter Fructus Camptothecae Acuminatae raw material is smashed, leached 1-3 time with solvent, obtain leaching liquid;

    After leaching liquid is concentrated, plus ethanol or water and secondAlcohol, make that the mixeding liquid volume is the leaching liquid volume 1/5~

    1/20, and in the mixed liquor ethanol volumn concentrationFor 60~

    100%;

    The precipitation produced in removing mixed liquor, obtains filtrate;

    Water and ethanol dilution filtrate are used again, obtain Fructus Camptothecae Acuminatae crude extractEnter sample liquid;

    (2) vincoside-lactam is purified with simulated moving bed chromatography abbreviation SMBC1) SMBC separation conditions are as follows:

    Chromatographic column:

    3~

    10;

    Fixing phase:

    Octadecylsilane chemically bonded silica ODS, 10~

    60 μ

    m;

    Operational mode:

    Three band SMBC are set, and three bands include elution band, refined band and absorption band, a is elution band chromatographic column number, 1≤

    a≤

    2;

    B is refined band chromatographic column number, 1≤

    b≤

    4;

    C is absorption band chromatographic column number, 1≤

    c≤

    4, operational mode a-b-C is represented;

    Flowing phase composition:

    Mobile phase P of elution band is ethanol and the mixed solution or ethanol of water, the volume of ethanol in mobile phase PPercentage composition is 50~

    100%;

    Mobile phase D of refined band and absorption band is ethanol and the mixed solution of water, the volume hundred of ethanolContent is divided to be 50~

    70%;

    Flow rate of mobile phase:

    In refined band and absorption band, eluent D flow velocity QDFor 1~

    10 times of column volume per hour, enter sample liquid F streamFast QFFor 0.1QD

    1.0QD, raffinate R flow velocity QR=QD+QF

    In elution band, eluent P flow velocity QpFor 0.5QD

    2QD, extractionTake liquid E flow velocity QE=Qp

    Switching time TS

    8~

    20min;

    Simulation moving bed operation temperature:

    Room temperature;

    2) SMBC separation processes are as follows:

    SMBC separation is carried out under above-mentioned SMBC working condition, Fructus Camptothecae Acuminatae crude extract is continuously pumped into by material liquid entrance and is entered sample liquid,SMBC automatic control systems press switching time TSAlong mobile phase direction by eluent entrance, extract export, material liquid entrance andThe position of raffinate outlet is moved to next root chromatogram column simultaneously successively, removes various front impurity from raffinate R outlets, from extractionLiquid E outlets obtain vincoside-lactam extract;

    (3) post processing is carried out to extractVincoside-lactam extract is concentrated into into muddiness, stratification discards upper strata milky white liquid, lower sediment entered with distilled waterRow cleaning, until cleanout fluid is colourless;

    Wedding fruits glycoside product is obtained to lower sediment recrystallization with ethanol again.

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