Lily oral liquid and quality standard and test method of pharmaceutical preparation thereof

Lily oral liquid and quality standard and test method of pharmaceutical preparation thereof

  • CN 101,229,323 A
  • Filed: 01/21/2008
  • Published: 07/30/2008
  • Est. Priority Date: 01/21/2008
  • Status: Active Application
First Claim
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1. the method for quality control of a drug combination preparation is characterized in that this method comprises one or more in following discriminating and/or the content:

  • Differentiate;

    A, the compositions preparation 5-45 weight portion of getting it filled, add hydrochloric acid and regulate pH value to 1-5, with ether, boiling range is that 60~

    90 ℃

    petroleum ether or chloroform jolting are extracted 1-3 time, each 20-30 parts by volume, merge, evaporate to dryness, residue add methanol or ethanol 1 parts by volume makes dissolving, as need testing solution;

    Other gets the gallic acid reference substance, adds the solution that methanol or ethanol are made 0.0001-0.005g/ml, in contrast product solution;

    According to the thin layer chromatography test, draw above-mentioned each 0.001-0.006 parts by volume of two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-formic acid=3-10;

    0.5-4;

    0.1-1.5 is developing solvent, launches, and takes out, dry, spray is with 1% ferric chloride alcoholic solution;

    In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

    B, the compositions preparation 5-45 weight portion of getting it filled, add hydrochloric acid 0.5-1.5 parts by volume, ether, boiling range are 60~

    90 ℃

    petroleum ether or chloroform 15-25 parts by volume, supersound process or hot reflux or merceration extracted 25 minutes, put cold, get extracting solution, put and be concentrated into about 1 parts by volume in the water-bath, as need testing solution;

    Other gets control medicinal material 0.5-6 weight portion Radix Ophiopogonis, adds water 25-35 parts by volume, and supersound process or hot reflux or decoction were extracted 20-60 minute, filtered, and filtrate adds hydrochloric acid 1 parts by volume, below operates the preparation method of pressing need testing solution, preparation control medicinal material solution;

    Test according to thin layer chromatography, draw above-mentioned each 0.001-0.02 parts by volume of two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone=1-17;

    0.5-5.5 is developing solvent, is expanded to about 10cm place, takes out, dry, spray is with 10% sulphuric acid ethanol liquid, and it is clear to be heated to the speckle colour developing at 100 ℃

    , puts the observation 365nm ultra-violet lamp under;

    In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence principal spot of same color;

    C, the compositions preparation 5-45 weight portion of getting it filled, put in the separatory funnel, adding 10% sodium carbonate liquor, to regulate pH value be 7-10, add diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or the jolting of chloroform 20-30 parts by volume is extracted, get extracting solution, volatilize, add methanol or ethanol 1 parts by volume makes dissolving, as need testing solution;

    Other gets Rhizoma Corydalis control medicinal material 0.5-4 weight portion, adds water 25-35 parts by volume, supersound process or hot reflux or decoction 20-60 minute, filter, it is 7-10 that filtrate adds 10% sodium carbonate liquor adjust pH, and below the operation preparation method of press need testing solution prepares control medicinal material solution;

    Get tetrahydropalmatine, ginsenoside Rg again 1Reference substance adds the solution that methanol or ethanol are made 0.0001-0.005g/ml respectively, product solution in contrast;

    Test according to thin layer chromatography, draw above-mentioned each 0.005-0.01 parts by volume of four kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-chloroform-methanol-ammonia=3-12;

    1-8;

    0.3-2.2;

    0.05-1 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and observe;

    In the test sample chromatograph, with control medicinal material, the corresponding position of reference substance tetrahydropalmatine chromatograph on, show the fluorescence speckle of same color;

    Spray with 5% vanillin sulfuric acid solution-ethanol=0.5-5.5;

    3-12 colour developing, it is clear to be heated to the speckle colour developing at 105 ℃

    again;

    In the test sample chromatograph, with the reference substance ginsenoside Rg 1On the corresponding position of chromatograph, show the speckle of same color;

    D, the compositions preparation 5-35 weight portion of getting it filled add diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or the jolting of chloroform 20-30 parts by volume is extracted, and gets extracting solution, evaporate to dryness, residue is 60~

    90 ℃

    petroleum ether or chloroform dissolving with ether, boiling range, is added to 200 orders, 2g, internal diameter is on the alumina chromatographic column of 1cm, with the methanol or the ethanol elution of 15-25 parts by volume, collect eluent, evaporate to dryness, residue adds 1 parts by volume methanol or ethanol makes dissolving, as need testing solution;

    Other gets Radix Scrophulariae control medicinal material 1-3 weight portion, add water 25-35 parts by volume, supersound process or hot reflux or decoction were extracted 20-60 minute, filter, filtrate adds diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or the jolting of chloroform 20-30 parts by volume is extracted, and gets extracting solution, evaporate to dryness, residue adds methanol or ethanol 1 parts by volume makes dissolving, in contrast medical material solution;

    Get the peoniflorin reference substance again, add the solution that methanol or ethanol are made 0.0001-0.005g/ml, in contrast product solution;

    Test according to thin layer chromatography, draw above-mentioned each 0.005-0.01 parts by volume of three kinds of solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water=0.5-6.5;

    0.5-3.5;

    0.05-2.5;

    0.05-2.5 is developing solvent, be expanded to the 15cm place, take out, dry, spray is with the mixed solution of 5% vanillin sulfuric acid solution-ethanol=0.5-5.5;

    2-12, and it is clear to be heated to the speckle colour developing at 100 ℃

    ;

    In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on show an identical punctation;

    With the corresponding position of reference substance on show identical blue spot;

    E, the compositions preparation 5-35 weight portion of getting it filled add diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or the jolting of chloroform 15-25 parts by volume is extracted 2 times, and extract solvent is 20 parts by volume at every turn, merge extractive liquid,, evaporate to dryness, residue add methanol or ethanol 1 parts by volume makes dissolving, as need testing solution;

    Other gets Herba Artemisiae Scopariae control medicinal material 0.5-4 weight portion, add water 10-80 parts by volume, supersound process or hot reflux or decoction were extracted 20-60 minute, put cold, filter, add diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or chloroform and make control medicinal material solution according to the method identical with need testing solution;

    Test according to thin layer chromatography, draw above-mentioned each 0.005-0.01 parts by volume of two kinds of solution, put respectively on same silica gel g thin-layer plate, be petroleum ether-ethyl acetate=0.5-4.5 of 60~

    90 ℃

    with boiling range;

    3-12 is developing solvent, launch, take out, dry, spray is with the solution of 5% vanillin sulfuric acid solution-ethanol=0.5-5.5;

    2-12, and it is clear to be heated to the speckle colour developing at 100 ℃

    ;

    In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of a same color;

    F, the compositions preparation 5-35 weight portion of getting it filled add diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or chloroform 25-65 parts by volume, and jolting is extracted 1-2 time, and merge extractive liquid,, evaporate to dryness, residue add methanol or ethanol 1 parts by volume makes dissolving, as need testing solution;

    Other gets Radix Angelicae Sinensis, each 0.2-1.5 weight portion of Rhizoma Chuanxiong control medicinal material, control medicinal material adds methanol, ethanol or water 15-25 parts by volume respectively, supersound process or hot reflux or merceration extracted 30-60 minute, and extracting solution adds diethyl ether, boiling range is 60~

    90 ℃

    petroleum ether or chloroform 25-65 parts by volume and make control medicinal material solution according to the method identical with need testing solution;

    According to the thin layer chromatography test, draw above-mentioned two kinds of solution 0.005-0.01 parts by volume, put respectively on same silica gel g thin-layer plate, be developing solvent with normal hexane-ethyl acetate=1-12;

    0.5-5.5, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect;

    In the test sample chromatograph, with reference substance, the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

    Assay;

    Measure according to an appendix VID of Chinese Pharmacopoeia version in 2005 high-efficient liquid phase technique;

    Chromatographic condition and system suitability test;

    with octadecylsilane chemically bonded silica is filler;

    Second eyeball-0.1% phosphoric acid solution=1-25;

    75-100 is a mobile phase;

    The detection wavelength is 230nm;

    Number of theoretical plate calculates by the peoniflorin peak should be not less than 1500;

    Reference substance solution preparation;

    it is an amount of to take by weighing the peoniflorin reference substance, adds the solution that methanol is made 0.0001-0.005g/ml, promptly;

    Need testing solution preparation;

    measure drug combination preparation 5-15 weight portion, put in the separatory funnel, add water 5-15 parts by volume, shake up, extract 5 times, be respectively 20 with the water-saturated n-butanol jolting, 20,20,15,15 parts by volume merge n-butyl alcohol liquid, evaporate to dryness in the water-bath, residue adds 50% methanol makes dissolving, be transferred in the 25 parts by volume measuring bottles, and be diluted to scale, shake up;

    Measure 5 parts by volume, put in the 25 parts by volume measuring bottles, add methanol and be diluted to scale, shake up, filter, promptly;

    Algoscopy;

    Accurate respectively reference substance solution and each 0.01 parts by volume of need testing solution drawn injected chromatograph of liquid, measures, promptly;

    This drug combination preparation is the dose meter per diem, peoniflorin C 23H 28O 11Must not lack 0.015 weight portion;

    Wherein said drug combination preparation is the prescription according to the MOLUO DAN described in the pharmacopeia, adds tablet, capsule, powder, soft capsule, drop pill, honeyed pill, pill, granule, soft extract with bee honey agent, slow releasing preparation, quick releasing formulation, controlled release preparation, oral liquid or the ejection preparation that conventional adjuvant is made according to conventional method.

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