Method for detecting indigowoad root in Pudilan Xiaoyan tablets

Method for detecting indigowoad root in Pudilan Xiaoyan tablets

  • CN 105,628,838 A
  • Filed: 12/24/2015
  • Published: 06/01/2016
  • Est. Priority Date: 12/24/2015
  • Status: Active Application
First Claim
Patent Images

1. the detection method of Radix Isatidis in the blue Pianomide in Pu ground, it is characterized in that:

  • described detection method is with (R, S)-goitrin is reference substance, adopt high performance liquid chromatography to (R contained by Radix Isatidis in the blue Pianomide in Pu ground, the content of S)-goitrin detects, comprise the following stepsStep one, setting high performance liquid chromatography detection chromatographic conditionChromatographic column;

    octadecylsilane chemically bonded silica post;

    Mobile phase;

    mobile phase A is methanol, Mobile phase B is volume fraction 0.02% phosphoric acid solution, and mobile phase ratio is 7;

    93;

    Flow velocity;

    1.0ml/min;

    Detection wavelength;

    245nm;

    Column temperature;

    30 DEG C;

    Theoretical cam curve calculates by (R, S)-goitrin peak, is not less than 7000;

    Step 2, preparation reference substance solutionWeigh (R, S)-goitrin reference substance 10.08mg, it is placed in 50ml volumetric flask, add methanol solution that volume fraction is 30% to scale, mixing, draws mixed liquor 2ml, is placed in 10ml volumetric flask, add volume fraction be the methanol solution of 30% to scale, standby as reference substance solution;

    Step 3, prepare need testing solutionTake blue 20, the Pianomide sample in Pu ground, remove film-coat, be ground to the powder that granularity is 60 order�



    80 orders, weighed 1.5g, is placed in 50ml conical flask, adds the methanol solution 50ml that volume fraction is 30%, weigh, supersound process 30min, put to room temperature, it is re-weighed, supplies weight with the methanol solution that volume fraction is 30%, mixing, filter, discarding just filtrate, take subsequent filtrate 0.45um microporous filter membrane and filter, gained filtrate is as need testing solution;

    Step 4, (R, S)-goitrin content linear relationship detectTake (R prepared by described step 2, S)-goitrin reference substance solution 2 �



    l, 4 �



    l, 6 �



    l, 8 �



    l and 10 �



    l, it is injected separately in high performance liquid chromatograph and is measured, record (R, S)-goitrin peak area, obtain (R, S)-goitrin content linear with (R, S)-goitrin peak area within the scope of 0.08064mg�



    0.4032mg;

    Step 5, Detection of StabilityDraw need testing solution 10 �



    l prepared by described step 3, inject in high performance liquid chromatograph, measure respectively at 0h, 2h, 4h, 8h, 12h sample introduction, it is thus achieved that (R, S)-goitrin content;

    Step 6, precision detectDraw need testing solution 10 �



    l prepared by described step 3, inject in high performance liquid chromatograph, repeat sample introduction 5 times, record (R, S)-goitrin peak area value;

    Step 7, repeatability detectMethod according to described step 3, weighs the blue Pianomide sample powder 5 parts in Pu ground, prepares 5 parts of need testing solutions, draw each 10 �



    l of described 5 parts of need testing solutions respectively, be injected separately in high performance liquid chromatograph, it is thus achieved that (R, S)-goitrin content;

    Step 8, the response rate detectWeighing the blue Pianomide sample powder 5 parts in described Pu ground, every part of 0.5007g�



    0.5036g, being separately added into concentration is 0.4976mg/ml (R, S)-goitrin reference substance solution 1ml�



    1.8ml, mixing, takes mixed liquor 10 �



    l and injects in high performance liquid chromatograph, calculate the response rate.

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