CN103175938B - Detecting method of drug for treating cough - Google Patents
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Abstract
The invention discloses a quality control method of a drug for treating cough. The quality control method comprises the following steps of: respectively indentifying borneol, immature fruits of terminalia chebula, ephedra, root barks of white mulberry and radix scutellariae in the drug by using thin layer chromatography, and measuring the content of ephedrine hydrochloride in the drug by using liquid chromatography. The quality control method established by the invention has the advantages that a crude drug indentifying method is mature and feasible, strong in specificity, negative and free of interference; a content measuring method is easy to operate, high in precision and good in repeatability; and by using the quality control method disclosed by the invention, the quality of the drug can be precisely and stably controlled so that the requirement for stable industrial production of the drug is met.
Description
Technical field
The present invention relates to a kind of Chinese medicine that is used for the treatment of cough, particularly relate to the method for quality control of this medicine.
Background technology
The cough class medication of Chinese white olive for relieving cough ball system, the cough with profuse sputum who causes for wind-cold affecting lung, chest diaphragm is full vexed, and shortness of breath is breathed heavily, dryness of the mouth and throat.
The existing operative norm of Chinese white olive for relieving cough ball is included in the tenth of the Sanitation Ministry medicine standard Traditional Chinese medicine historical preparation.In this quality standard, formulated following content.
1) get this product, put micro-Microscopic observation: cellulose contains calcium oxalate prismatic crystal in parenchyma cell around, forms crystal fiber.Calcium oxalate cluster crystal is distributed in mesophyll cell, diameter 2-10um.Amylum body oval, diameter 35-48um, omphalion point-like, herringbone shape or horse-hof shape, be positioned at compared with small end, and laminated striation is fine and closely woven.Pollen granule is faint yellow, is class spherical, diameter 28-40um, tool 3 hole dumbbell shapeds.Irregular flaky crystal is colourless, has straight texture.Endocarp organizes apical view to be class polygon, boundary fuzzy, and cell is starlike, visible topped planocellular close grain.Needle-like calcium oxalate crystal is more, be dispersed in everywhere, or bunchy is present in oval mucilage cell, and needle is very thin, long 20-144um.Faint yellow or the brown color of lithocyte, similar round or class are square, and wall is thicker, and laminated striation is obvious, and the inhomogeneous lignify of wall of crystal cell thickens, and includes calcium oxalate prismatic crystal or prism.Fiber is faint yellow, fusiformis, and wall thickness, hole ditch is thin.
2) get this product 6g, chopping, adds zeyssatite 6g, grinds well, and adds methenyl choloride 40ml.Ultrasonic processing 10 minutes, filters, and filtrate is waved to 2ml, as need testing solution.Separately get borneol reference substance, add methenyl choloride and make every 1ml containing the solution of 0.2mg, in contrast product solution.According to thin-layered chromatography (appendix VI B) test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica G thin layer plate, benzene-the ethyl acetate (17:1) of take is developping agent, launches, and takes out, dry, spray is with 5% phosphomolybdic acid ethanol solution, 105 ℃ of heating several minutes.In test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical blue spot.
Above-mentioned quality standard exists more serious defect: first, this standard is not carried out the quantitative measurement of active constituent content for main medicine; Secondly, more than 50% composition medicine does not all carry out chemistry discriminating.
Chinese medicine preparation steady quality, controlled and have that to produce repeatability be the premise that medicine has pharmacology and clinical effectiveness repeatability, can traditional Chinese medicine quality controlled and whether traditional Chinese medicine quality standard is scientific, is the important restriction factor that affects industrialization of Chinese medicine.Quality controllability is the important indicator that medicine is evaluated, and quality standard is the imbody of drug quality controllability.
Summary of the invention
The method of quality control that the object of this invention is to provide a kind of above-mentioned treatment cough medicine, to guarantee that the drug quality of producing stablizes controlled.
The method of quality control for the treatment of cough medicine provided by the invention is suitable for the medicine being prepared from by following bulk drug: FRUCTUS TERMINALIAE IMMATURUS, Chinese ephedra, stir-fry semen armeniacae amarae, gypsum, stir-fry perilla seed, the tuber of pinellia processed, fritillaria thunbergii, the root bark of white mulberry processed, perilla leaf, the root of large-flowered skullcap, Radix Glycyrrhizae, tussilago, borneol.Described method of quality control comprises discrimination method and content assaying method.
Wherein, described discrimination method comprises following discriminating:
1) get described medicine 6g, add zeyssatite 3g, grind well, add methenyl choloride 40ml, ultrasonic processing 10 minutes, filters, and filtrate is waved to 2ml, as need testing solution; Separately get borneol reference substance, add methenyl choloride and make every 1ml containing the solution of 0.1mg, in contrast product solution; According to thin-layered chromatography, test, draw each 2 μ l of above-mentioned two kinds of solution, put on same silica gel g thin-layer plate respectively, take toluene: ethyl acetate=17:1 as developping agent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical blue spot;
2) get described medicine 6g, add zeyssatite 3g, grind well, add ethyl acetate 30ml, heating water bath refluxing extraction 1 hour, filters, and filtrate is reclaimed solvent to dry, and residue adds 1ml ethyl acetate to be made to dissolve, as need testing solution; Separately get FRUCTUS TERMINALIAE IMMATURUS control medicinal material 0.5g, add ethyl acetate 20ml, ultrasonic processing 20 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds ethyl acetate 1ml to be made to dissolve, in contrast medicinal material solution; According to thin-layered chromatography, test, draw each 5 μ l of above-mentioned test sample liquid and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take toluene: ethyl acetate: formic acid=5:4:1 is developping agent, launch, take out, dry, spray is with ammonia silver nitrate test solution processed, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;
3) get described medicine 5g, add zeyssatite 3g, grind well, add methyl alcohol 20ml, ultrasonic processing 30 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution; Separately get Chinese ephedra control medicinal material 1g, be made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw above-mentioned test sample liquid 10 μ l, control medicinal material 2 μ l, put respectively on same silica gel g thin-layer plate, take methenyl choloride: methyl alcohol: strong aqua=20:5:0.5 is developping agent, launch, take out, dry, spray, with ninhydrin solution, is heated to spot colour developing at 105 ℃ clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical punctation;
4) get described medicine 5g, add zeyssatite 3g, grind well, add absolute ethyl alcohol 50ml, ultrasonic processing 30 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds ethyl acetate 2ml to be made to dissolve, as need testing solution; Separately get root bark of white mulberry control medicinal material 1g, add absolute ethyl alcohol 30ml, be made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw above-mentioned need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, take 60-90 ℃ of sherwood oil: toluene: methenyl choloride=20:5:4 is developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;
5) get described medicine 6g, add zeyssatite 3g, grind well, add ethyl acetate: the mixed solution 30ml of methyl alcohol=3:1, add hot reflux 30 minutes, let cool, filter, filtrate is reclaimed solvent to dry, and residue adds methyl alcohol 5ml to be made to dissolve, and gets supernatant as need testing solution; Separately get root of large-flowered skullcap control medicinal material 1g, be made in the same way of control medicinal material solution; According to thin-layered chromatography, test, draw each 5 μ l of above-mentioned two kinds of solution, put on same polyamide film respectively, take toluene: ethyl acetate: methyl alcohol: formic acid=10:3:1:2 is developping agent, presaturation 30 minutes, launch, take out, dry, spray is with 5% ferric trichloride ethanolic solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
Described content assaying method comprises the mensuration of Determination of ephedrine hydrochloride.
The present invention is specifically with the content of ephedrine hydrochloride described in following high effective liquid chromatography for measuring:
1) chromatographic condition and system suitability: take octadecylsilane chemically bonded silica as filling agent, take acetonitrile: the 0.1% phosphoric acid solution=5:95 that contains 0.1% triethylamine is mobile phase; Detect wavelength 210nm; Number of theoretical plate calculates and is not less than 2000 by ephedrine hydrochloride peak;
2) preparation of reference substance solution: the ephedrine hydrochloride reference substance of the phosphorus pentoxide drying under reduced pressure of learning from else's experience is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml containing the reference substance solution of 42 μ g;
3) preparation of need testing solution: the described medicine 1g that gets porphyrize, accurately weighed, put in tool plug conical flask, add 1% hydrochloric acid 50ml, power 250W, the ultrasonic processing of frequency 33kHz 30 minutes, extract moves in centrifuge tube centrifugal 10 minutes, getting supernatant puts in separating funnel, precipitation is used 1% salt acid elution 2 times again, each 5ml, washing lotion is incorporated in same separating funnel, with ammoniacal liquor, regulate pH value to 9-10, adding methenyl choloride jolting extracts 3 times, each 20ml, centrifugal elimination emulsion layer, merge methenyl choloride liquid, low temperature is flung to methenyl choloride, residue dissolves with methyl alcohol, be transferred in 10ml measuring bottle, add methyl alcohol to scale, shake up, filter, get subsequent filtrate, obtain,
4) draw respectively each 10 μ l of reference substance solution and need testing solution, injection liquid chromatography, measures and get final product.
The present invention has set up the method for quality control for the treatment of cough medicine, in the method for setting up, the discrimination method mature and feasible of medicinal material, specificity is strong, negative noiseless, content assaying method processing ease, precision is high, favorable reproducibility, is used method of quality control of the present invention can accurately, stably control the drug quality of Chinese white olive for relieving cough ball, to adapt to the industrialization steady production of medicine.
Embodiment
Embodiment 1: the thin layer of borneol is differentiated.
Get Chinese white olive for relieving cough ball 6g, add zeyssatite 3g, grind well, add methenyl choloride 40ml, ultrasonic processing 10 minutes, filters, and filtrate is waved to 2ml, as need testing solution.Separately get borneol reference substance, add methenyl choloride and make every 1ml containing the solution of 0.1mg, in contrast product solution.According to thin-layered chromatography (appendix VI B of < < Chinese Pharmacopoeia > > version in 2005), test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, toluene-the ethyl acetate (17:1) of take is developping agent, launch, take out, dry, spray, with 5% phosphomolybdic acid ethanol solution, is heated to spot colour developing at 105 ℃ clear.In test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical blue spot.
Embodiment 2: the thin layer of FRUCTUS TERMINALIAE IMMATURUS is differentiated.
Get Chinese white olive for relieving cough ball 6g, add zeyssatite 3g, grind well, add ethyl acetate 30ml, heating water bath refluxing extraction 1 hour, filters, and filtrate is reclaimed solvent to dry, and residue adds 1ml ethyl acetate to be made to dissolve, as need testing solution.Separately get FRUCTUS TERMINALIAE IMMATURUS control medicinal material 0.5g, add ethyl acetate 20ml, ultrasonic processing 20 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds ethyl acetate 1ml to be made to dissolve, in contrast medicinal material solution.According to thin-layered chromatography (appendix VI B of < < Chinese Pharmacopoeia > > version in 2005), test, draw each 5 μ l of above-mentioned test sample liquid and control medicinal material solution, put respectively on same silica gel g thin-layer plate, toluene-ethyl acetate-the formic acid (5:4:1) of take is developping agent, launch, take out, dry, spray, with ammonia silver nitrate test solution processed, is heated to spot colour developing at 105 ℃ clear.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.The method chromatogram is satisfactory for result, and FRUCTUS TERMINALIAE IMMATURUS negative sample is noiseless.Through three batch sample checkings, chromatogram reappearance is good.
Embodiment 3: the thin layer of Chinese ephedra is differentiated.
Get Chinese white olive for relieving cough ball 5g, add zeyssatite 3g, grind well, add methyl alcohol 20ml, ultrasonic processing 30 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution.Separately get Chinese ephedra control medicinal material 1g, be made in the same way of control medicinal material solution.According to thin-layered chromatography (appendix VI B of < < Chinese Pharmacopoeia > > version in 2005), test, draw above-mentioned test sample liquid 10 μ l, control medicinal material 2 μ l, put on same silica gel g thin-layer plate respectively, the methenyl choloride-methyl alcohol-strong aqua (20:5:0.5) of take is developping agent, launches, take out, dry, spray, with ninhydrin solution, is heated to spot colour developing at 105 ℃ clear.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical punctation.This method experimental result chromatogram is satisfactory for result, and Chinese ephedra negative sample is noiseless.Through three batch sample checkings, chromatogram reappearance is good.
Embodiment 4: the thin layer of the root bark of white mulberry is differentiated.
Get Chinese white olive for relieving cough ball 5g, add zeyssatite 3g, grind well, add absolute ethyl alcohol 50ml, ultrasonic processing 30 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds ethyl acetate 2ml to be made to dissolve, as need testing solution.Separately get root bark of white mulberry control medicinal material 1g, add absolute ethyl alcohol 30ml, be made in the same way of control medicinal material solution.According to thin-layered chromatography (appendix VI B of < < Chinese Pharmacopoeia > > version in 2005), test, draw above-mentioned need testing solution 10 μ l, control medicinal material solution 2 μ l, put on same silica gel g thin-layer plate respectively, sherwood oil (the 60-90 ℃)-toluene-methenyl choloride (20:5:4) of take is developping agent, launches, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.This method test chromatogram is satisfactory for result, and root bark of white mulberry negative sample is noiseless.Through three batch sample checkings, chromatogram reappearance is good.
Embodiment 5: the thin layer of the root of large-flowered skullcap is differentiated.
Get Chinese white olive for relieving cough ball 6g, add zeyssatite 3g, grind well, add the mixed solution 30ml of ethyl acetate-methyl alcohol (3:1), add hot reflux 30 minutes, let cool, filter, filtrate is reclaimed solvent to dry, and residue adds methyl alcohol 5ml to be made to dissolve, and gets supernatant as need testing solution.Separately get root of large-flowered skullcap control medicinal material 1g, be made in the same way of control medicinal material solution.According to thin-layered chromatography (appendix VI B of < < Chinese Pharmacopoeia > > version in 2005), test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, toluene-ethyl acetate-methyl alcohol-the formic acid (10:3:1:2) of take is developping agent, presaturation 30 minutes, launches, and takes out, dry, spray is with 5% ferric trichloride ethanolic solution.In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.The method chromatogram is satisfactory for result, and root of large-flowered skullcap negative sample is noiseless.Through three batch sample checkings, chromatogram reappearance is good.
Embodiment 6: the mensuration of Determination of ephedrine hydrochloride.
Chinese white olive for relieving cough ball is comprised of FRUCTUS TERMINALIAE IMMATURUS, Chinese ephedra, semen armeniacae amarae etc., and it is cold that its epheday intermedia has Pulvis Diaphoreticus, freeings lung and relieving asthma, and the effect of inducing diuresis for removing edema plays an important role in preparation.Chinese ephedra Ephedrine content is higher, and bibliographical information is more, and method is more ripe, therefore select Determination of ephedrine hydrochloride as method of quality control.
1, instrument and reagent.
U.S. Agilent company high performance liquid chromatograph, Agilent 1100 series chromatographic work stations; KQ5200DE ultrasonic cleaner (Kunshan ultrasonic instrument factory); BS223S per mille electronic balance, CP225D 100,000/electronic balance (German Sai Duolisi); Hydro-extractor LXJ-ⅡB(Anting Scientific Instrument Factory, Shanghai); Acetonitrile is chromatographically pure (Brudick & Jackson), and it is pure that other reagent are analysis; Ephedrine hydrochloride reference substance (Nat'l Pharmaceutical & Biological Products Control Institute, lot number 171241-200506).
Chinese white olive for relieving cough ball (Katyuan, Shanxi pharmaceutical factory, lot number 080919,080920,080921).
2, chromatographic condition.
Chromatographic column: kromasil-C
18(4.6mm * 250mm, 5 μ m); Mobile phase: acetonitrile-0.1% phosphoric acid (including 0.1% triethylamine) solution (5:95); Detect wavelength 210nm, flow velocity 0.8ml/min.Number of theoretical plate calculates and should be not less than 2000 by ephedrine hydrochloride peak.
3, the preparation of reference substance solution.
The ephedrine hydrochloride reference substance of phosphorus pentoxide drying under reduced pressure of learning from else's experience is appropriate, accurately weighed, adds methyl alcohol and makes every 1ml containing the solution of 42.72 μ g, obtains.
4, the preparation of need testing solution.
Get Chinese white olive for relieving cough ball, porphyrize, get about 1g, accurately weighed, put in tool plug conical flask, add 1% watery hydrochloric acid 50ml, ultrasonic processing (power 250W, frequency 33kHz) 30 minutes, extract moves in centrifuge tube, centrifugal (rotating speed is that per minute 4500 turns) 10 minutes, get supernatant, put in separating funnel, precipitation is again with 1% watery hydrochloric acid washing 2 times, each 5ml, washing lotion is incorporated in same separating funnel, with ammoniacal liquor, regulate pH value to 9-10, adding methenyl choloride jolting extracts 3 times, each 20ml, centrifugal elimination emulsion layer if desired, merge methenyl choloride liquid, low temperature is flung to methenyl choloride, residue dissolves with methyl alcohol, be transferred in 10ml measuring bottle, add methyl alcohol to scale, shake up, filter, get subsequent filtrate, obtain.
5, the mensuration of Determination of ephedrine hydrochloride.
Precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and injection liquid chromatography, measures, and obtains.The every g of preparation contains Chinese ephedra with ephedrine hydrochloride (C
10h
15nOHCl) meter, must not be less than 0.220mg.
6, negative sample test.
In Chinese white olive for relieving cough pill prescription ratio, the negative control sample of Chinese ephedra is removed in the preparation of simulation process method for making.Precision takes negative control sample 1.0g, by need testing solution preparation method, makes negative need testing solution.Under definite chromatographic condition, record respectively the chromatogram of ephedrine reference substance, test sample and negative control product, collection of illustrative plates result shows: in the corresponding section with ephedrine retention time, in negative control product chromatogram, without chromatographic peak, occur, under definite condition determination, in preparation prescription, other flavour of a drug are noiseless to the mensuration of ephedrine.
7, the investigation of linear relationship.
Accurate absorption concentration is ephedrine reference substance solution 2 μ l, 4 μ l, 6 μ l, 8 μ l and the 10 μ l injecting chromatographs of 42.72 μ g/ml respectively, under definite chromatographic condition, record peak area, take peak area integrated value as ordinate, ephedrine sample size (μ g) is horizontal ordinate, obtaining regression equation is y=2600.2x-4.49, r=0.9998; Proof ephedrine, within the scope of 0.085-0.4272 μ g, is good linear relationship, in Table 1 between sample size and peak area.
8, precision test.
Prepare need testing solution, the accurate need testing solution 10 μ l that draw, repeat sample introduction 6 times, and the RSD of results peaks area value is 0.903%, the results are shown in Table 2.
9, stability test.
Get with a need testing solution in the airtight placement of room temperature, within 0,3,6,9,12 and 24 hour after preparation, measure respectively its peak area, investigate the variation of ephedrine peak area.Result shows, need testing solution was measured in 24 hours, had good stability, and the results are shown in Table 3.
10, replica test.
Get 6 parts of same batch samples, each about 1g, accurately weighed, by need testing solution preparation method, extract respectively, assay, calculates.Result average content is 0.237mg/g, and RSD is 0.99%, the results are shown in Table 4.
11, average recovery test.
Get respectively 6 parts of each 0.5g of sample of known content, accurately weighed, precision is added a certain amount of ephedrine reference substance respectively, and by need testing solution, preparation method extracts, and assay the results are shown in Table 5.
According to above test findings, the ephedrine recovery 95.94%, RSD is 1.10%; Be less than 3%, the recovery is qualified, shows that the accuracy of institute's construction method is better, and the method can be for the assay of Chinese white olive for relieving cough ball small honey pill Ephedrine.
Claims (1)
- One kind treat cough medicine detection method, described treatment cough medicine is the medicine being prepared from by following bulk drug: FRUCTUS TERMINALIAE IMMATURUS, Chinese ephedra, stir-fry semen armeniacae amarae, gypsum, stir-fry perilla seed, the tuber of pinellia processed, fritillaria thunbergii, the root bark of white mulberry processed, perilla leaf, the root of large-flowered skullcap, Radix Glycyrrhizae, tussilago, borneol, and the discrimination method in described detection method comprises following discriminating:1) get described medicine 6g, add zeyssatite 3g, grind well, add methenyl choloride 40ml, ultrasonic processing 10 minutes, filters, and filtrate is waved to 2ml, as need testing solution; Separately get borneol reference substance, add methenyl choloride and make every 1ml containing the solution of 0.1mg, in contrast product solution; According to thin-layered chromatography, test, draw each 2 μ l of above-mentioned two kinds of solution, put on same silica gel g thin-layer plate respectively, take toluene: ethyl acetate=17:1 as developping agent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious identical blue spot;2) get described medicine 6g, add zeyssatite 3g, grind well, add ethyl acetate 30ml, heating water bath refluxing extraction 1 hour, filters, and filtrate is reclaimed solvent to dry, and residue adds 1ml ethyl acetate to be made to dissolve, as need testing solution; Separately get FRUCTUS TERMINALIAE IMMATURUS control medicinal material 0.5g, add ethyl acetate 20ml, ultrasonic processing 20 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds ethyl acetate 1ml to be made to dissolve, in contrast medicinal material solution; According to thin-layered chromatography, test, draw each 5 μ l of above-mentioned test sample liquid and control medicinal material solution, put on same silica gel g thin-layer plate respectively, take toluene: ethyl acetate: formic acid=5:4:1 is developping agent, launch, take out, dry, spray is with ammonia silver nitrate test solution processed, at 105 ℃, be heated to spot colour developing clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;3) get described medicine 5g, add zeyssatite 3g, grind well, add methyl alcohol 20ml, ultrasonic processing 30 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution; Separately get Chinese ephedra control medicinal material 1g, be made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw above-mentioned test sample liquid 10 μ l, control medicinal material 2 μ l, put respectively on same silica gel g thin-layer plate, take methenyl choloride: methyl alcohol: strong aqua=20:5:0.5 is developping agent, launch, take out, dry, spray, with ninhydrin solution, is heated to spot colour developing at 105 ℃ clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious identical punctation;4) get described medicine 6g, add zeyssatite 3g, grind well, add ethyl acetate: the mixed solution 30ml of methyl alcohol=3:1, add hot reflux 30 minutes, let cool, filter, filtrate is reclaimed solvent to dry, and residue adds methyl alcohol 5ml to be made to dissolve, and gets supernatant as need testing solution; Separately get root of large-flowered skullcap control medicinal material 1g, be made in the same way of control medicinal material solution; According to thin-layered chromatography, test, draw each 5 μ l of above-mentioned two kinds of solution, put on same polyamide film respectively, take toluene: ethyl acetate: methyl alcohol: formic acid=10:3:1:2 is developping agent, presaturation 30 minutes, launch, take out, dry, spray is with 5% ferric trichloride ethanolic solution, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color;It is characterized in that the discrimination method in described detection method also comprises following discriminating:5) get described medicine 5g, add zeyssatite 3g, grind well, add absolute ethyl alcohol 50ml, ultrasonic processing 30 minutes, filters, and filtrate is reclaimed solvent to dry, and residue adds ethyl acetate 2ml to be made to dissolve, as need testing solution; Separately get root bark of white mulberry control medicinal material 1g, add absolute ethyl alcohol 30ml, be made in the same way of control medicinal material solution; According to thin-layered chromatography test, draw above-mentioned need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively on same silica gel g thin-layer plate, take 60-90 ℃ of sherwood oil: toluene: methenyl choloride=20:5:4 is developping agent, launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 105 ℃ clear, in test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the spot of aobvious same color.
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