Quality controlling method of Bupleurum injection

Quality controlling method of Bupleurum injection

  • CN 101,013,110 B
  • Filed: 01/25/2007
  • Issued: 04/23/2014
  • Est. Priority Date: 01/25/2007
  • Status: Active Grant
First Claim
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1. the detection method of Bupleurum injection, comprises the steps:

  • The first step, vapor-phase chromatography is set up Bupleurum injection reference fingerprint;

    adopt nonpolar or low pole quartz capillary column, with N 2for carrier gas, flow velocity 0.8-1.5mL/min, current constant mode, split ratio is 10-20;


    Take FID as detecting device, adopt the mode of temperature programme to analyze;

    Need testing solution injecting chromatograph by least 10 batches of Bupleurum injections, records chromatogram, utilizes fingerprint similarity evaluation software to generate Bupleurum injection reference fingerprint;

    Second step, measures by the first step method finger-print that Bupleurum injection detects sample;

    The 3rd step, calculates Bupleurum injection and detects the finger-print of sample and the similarity of reference fingerprint;

    Described need testing solution is prepared by the process of following A or B;

    A, precision are drawn 10ml Bupleurum injection with heavily steaming ether equivalent extracting twice, each 10ml, and combined ether layer, adds anhydrous sodium sulfate dehydration 30 minutes, filters, and filtrate vacuum is drained, and residue is 5ml with heavily steaming ether dissolution constant volume, obtains described need testing solution;

    B, the accurate Bupleurum injection 1.0ml that draws, put in 10ml head space bottle, seals, and obtains need testing solution;

    Wherein, adopt the condition of headspace sampling mode to be;

    head space bottle temperature 80-90 ℃

    , sampling valve temperature 90-120 ℃

    , transmission line temperature 110-120 ℃


    Head space bottle equilibration time 10-25min, head space bottle pressurising time 0.1-0.5min, quantitatively ring filling time 0.1-0.5min, quantitatively encircles equilibration time 0.2-1.0min, sample injection time 0.5-2.0min;

    The mode of chromatographic column adopting temperature programme is analyzed, and the condition of temperature programme is;

    initial 35 ℃

    , keep 2min;

    1 ℃

    /min rises to 40 ℃

    , keeps 2min, and 3 ℃

    /min rises to 60 ℃

    , keeps 3min, and 7 ℃

    /min rises to 200 ℃

    , keeps 3min.

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