CN104597196B - Treat the discrimination method of ardisia japonica in the Chinese patent drug of hot heavy breathing disease - Google Patents
Treat the discrimination method of ardisia japonica in the Chinese patent drug of hot heavy breathing disease Download PDFInfo
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Abstract
The present invention relates to the discrimination method of ardisia japonica in a kind of Chinese patent drug for the treatment of hot heavy breathing disease. The preparation of need testing solution: the ethanol elution that adopts large pore resin absorption column absorption, is 35% by mass concentration; The preparation of reference substance solution: with Bergenin control sample; Adopt thin-layered chromatography: using the mixed solution of polyamide film expansion, ethyl acetate-acetic acid is solvent, and result of the test feminine gender is noiseless. The thin-layer identification method favorable reproducibility of ardisia japonica in the Chinese patent drug of the hot heavy breathing disease for the treatment of that the present invention sets up, specificity are strong, clear spot, can effectively ensure the stable of this Quality of Chinese Traditional Proprietary Medicine.
Description
Technical field
The present invention relates to a kind of discrimination method of traditional Chinese medicine ingredients, particularly relate in a kind of Chinese patent drug for the treatment of hot heavy breathing disease shortThe discrimination method of thamnolia vermicularia.
Background technology
The Chinese patent drug for the treatment of hot heavy breathing disease contains Chinese ephedra 160g, ardisia japonica 360g, root of large-flowered skullcap 210g, semen armeniacae amarae 210g, peachBenevolence 170g, earthworm 165g, fruit of Chinese magnoliavine 140g, barrenwort 240g, fruit of glossy privet 265g, Radix Glycyrrhizae 105g granulation 1000g.Preparation method is: fruit of glossy privet 265g, fruit of Chinese magnoliavine 140g add 65% alcohol heating reflux and extract secondary, each 1.5 littleTime, merging extract, it is 1.07-1.09 (60 DEG C) that recovery ethanol is concentrated into relative density; Separately get Chinese ephedra 160g, hardshipAlmond 210g, peach kernel 170g steam distillation, collect distillate for subsequent use. The dregs of a decoction and ardisia japonica 360g, root of large-flowered skullcap 210g,Earthworm 165g, barrenwort 240g, Radix Glycyrrhizae 105g gomi herbs boiling twice, each 1 hour, collecting decoctionAnd liquid after above-mentioned distillation, filtering, it is 1.02-1.06 (60 DEG C) that filtrate is concentrated into relative density, merges above-mentioned threePlant extract, spraying is dry, adds appropriate cane sugar powder, granulates, and to obtain final product. This Chinese patent drug is that one is treated clearing heat and freeing lung,The Chinese patent drug of resolving sputum and relieving asthma. For hot heavy breathing disease, disease is seen: the rough or wheezing of panting, and cough gurgling weith sputum, sweating is thirsty, tongueRed tongue Huang etc. Usage and dosage: boiling water is taken after mixing it with water, each 9g, 4 times on the one. Specification is every packed 9g.
The former traditional Chinese medicines standard of this Chinese patent drug is differentiated item without ardisia japonica, in the pharmacopeia quality standard that ardisia japonica is differentiated is applied toWhen patent medicine, there is following problem: 1. because sample is impure many, and Bergenin composition is at water layer, uses methyl alcohol to carryGet rear impure still more. 2. because Bergenin is isocoumarin class, use silica gel g thin-layer plate to launch effect and pay no attention toThink that 3. because Bergenin is without special developer, unintelligible with spot after the colour developing of pharmacopeia coloration method, poor reproducibility.
Summary of the invention
The present invention is directed to above-mentioned defect, a kind of simple to operate, favorable reproducibility, above-mentioned Chinese patent drug that stability is high are providedThe thin-layer identification method of middle ardisia japonica.
For reaching above-mentioned purpose, the discrimination method of ardisia japonica in Chinese patent drug of the present invention, this Chinese patent drug contains Chinese ephedra 160g, shortThamnolia vermicularia 360g, root of large-flowered skullcap 210g, semen armeniacae amarae 210g, peach kernel 170g, earthworm 165g, fruit of Chinese magnoliavine 140g, barrenwort240g, fruit of glossy privet 265g, Radix Glycyrrhizae 105g, preparation method is: fruit of glossy privet 265g, fruit of Chinese magnoliavine 140g add 65% ethanolHeating and refluxing extraction secondary, each 1.5 hours, merge extract, it is 1.07-1.09 that recovery ethanol is concentrated into relative density(60 DEG C); Separately get Chinese ephedra 160g, semen armeniacae amarae 210g, peach kernel 170g steam distillation, collect distillate for subsequent use. MedicineSlag and ardisia japonica 360g, root of large-flowered skullcap 210g, earthworm 165g, barrenwort 240g, the boiling of Radix Glycyrrhizae 105g gomi herbsTwice, each 1 hour, the liquid after collecting decoction and above-mentioned distillation, filtered, and filtrate is concentrated into relative density and is1.02-1.06 (60 DEG C), merges above-mentioned three kinds of extracts, and spraying is dry, adds appropriate cane sugar powder, granulation 1000g,; In this Chinese patent drug, the discrimination method of ardisia japonica composition is:
The preparation of need testing solution: the ethanol elution that adopts large pore resin absorption column absorption, is 35% by mass concentration;
The preparation of reference substance solution: with Bergenin control sample;
Adopt thin-layered chromatography: using the mixed solution of polyamide film expansion, ethyl acetate-acetic acid is solvent.
Particularly, the discrimination method of ardisia japonica in Chinese patent drug of the present invention, the preparation of described need testing solution: get described inPatent medicine 5g, porphyrize, adds ethanol 20ml, and ultrasonic extraction 30 minutes filters, filtrate evaporate to dryness, the residue 5ml that adds water makesDissolve, by large pore resin absorption column, with 35% ethanol 50ml wash-out, collect eluent, evaporate to dryness, residue adds firstAlcohol 1ml makes to dissolve, and supernatant is as need testing solution.
The preparation of described need testing solution: get Bergenin, add methyl alcohol and make the solution of every 1ml containing 1mg, as rightAccording to product solution.
Described thin-layered chromatography: draw need testing solution and the each 3 μ l of reference substance solution, put respectively in same polyamide filmUpper, taking the mixed solution of ethyl acetate-acetic acid as solvent, launch, take out, dry, put under ultraviolet lamp and inspect,In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescent spot of aobvious same color.
Further preferably, method of the present invention, in the mixed solution of wherein said ethyl acetate-acetic acid ethyl acetate withThe weight ratio of acetic acid is 2:1.
Method of the present invention, wherein the ultraviolet wavelength of preferred described ultraviolet lamp is 254nm.
In existing this Chinese patent drug extracting method, there is following problem:
1, owing to there being ten kinds of medicinal ingredients in this Chinese patent drug compound, impurity is many, interference is large, and Bergenin polarity is large,Separate with impurity is more difficult, proving to adopt general methyl alcohol extracting method to prepare need testing solution through test of many times cannot be byIt separates with impurity;
2, Bergenin is isocoumarin class, uses silica gel g thin-layer plate to launch effect undesirable, selectively not strong,Be not easy despumation;
3. because Bergenin is without special developer, unintelligible with spot after the colour developing of pharmacopeia coloration method, poor reproducibility,And it is not strong by the mode of the inspecting simplicity of colour developing;
The present invention has overcome an above-mentioned difficult problem for prior art, has the following advantages:
1, adopt the extraction of large pore resin absorption column absorption, 35% ethanol elution, refining mode, can effectively remove compoundMiddle impurity, easy to operate, favorable reproducibility;
2, thin-layer chromatography uses polyamide film to launch, high specificity, and easily despumation is disturbed;
3, selecting ethyl acetate-acetic acid (2:1) is solvent, under ultraviolet lamp (254nm), inspects. Fluorescence is aobviousColor method is easier, easy to operate.
To sum up, the invention solves ardisia japonica in Chinese patent drug differentiate in methyl alcohol extract that impurity is many, the asking of inferior separating effectTopic; By improving development system and inspecting condition, strengthen the specificity of discrimination method, and easier, quick,Easy operating. The present invention ensured better Chinese patent drug quality, make patient's drug safety obtain guarantee, effectivelyHaving ensured the stable of product quality, is containing of Bergenin in the compound preparation that impurity is many, not easily separated, interference is largeAmount is provided by a kind of method that has reference that provides.
Below in conjunction with accompanying drawing, the discrimination method of ardisia japonica in Chinese patent drug of the present invention is described further.
Brief description of the drawings
Fig. 1 is the ardisia japonica test sample of embodiment 1 and the thin-layer chromatogram of control sample;
(the ardisia japonica medicinal material 4. that ardisia japonica medicinal material 3. places of production that 1. Bergenin reference substance 2. places of production are Hebei are HubeiThe place of production is the ardisia japonica medicinal material that ardisia japonica medicinal material 6. places of production that ardisia japonica medicinal material 5. places of production in Hunan are Sichuan are Guangxi)
Fig. 2 is the ardisia japonica test sample of embodiment 2 and the thin-layer chromatogram of control sample.
(1. Bergenin reference substance; 2. lot number: 201401; 3. lot number: 201403; 4. lot number 201406; 5. batchNumbers 201407; 6. lot number 201410; 7. negative control)
Detailed description of the invention
Be below embodiment and test data etc. thereof, but content of the present invention is not limited to the scope of these embodiment.
The thin-layer chromatography of embodiment 1 ardisia japonica medicinal material is differentiated
The each 0.4g of ardisia japonica medicinal material that gets Hebei, Hubei, Hunan, Sichuan, 5 different places of production, Guangxi, porphyrize, addsEthanol 20ml, ultrasonic extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 5ml make dissolve, inhale by macroporeAttached resin column, with 35% ethanol 50ml wash-out, collects eluent, evaporate to dryness, and residue adds methyl alcohol 1ml to be made to dissolve, onClear liquid is as need testing solution. Separately get Bergenin reference substance, add methyl alcohol and make the solution of every 1ml containing 1mg, asReference substance solution, according to thin-layered chromatography (annex VI B of Chinese pharmacopoeia version in 2010) test, draws above-mentioned twoPlant the each 3 μ l of solution, put respectively on same polyamide film, taking ethyl acetate-acetic acid (2:1) as solvent, launch,Take out, dry, put under ultraviolet lamp (254nm) and inspect.
The results are shown in Figure 1, visible five different places of production ardisia japonica medicinal material test sample chromatograms with Bergenin reference substance chromatogramThe spot of aobvious same color on corresponding position, clear spot.
Embodiment 2 treats the thin-layer chromatography of ardisia japonica in the Chinese patent drug of hot heavy breathing disease and differentiates
The Chinese patent drug preparation method who treats hot heavy breathing disease is: fruit of glossy privet 265g, fruit of Chinese magnoliavine 140g add 65% ethanol and heat backStream extracts secondary, and each 1.5 hours, merge extract, it is 1.07-1.09 (60 that recovery ethanol is concentrated into relative densityDEG C); Separately get Chinese ephedra 160g, semen armeniacae amarae 210g, peach kernel 170g steam distillation, collect distillate for subsequent use. The dregs of a decoction withArdisia japonica 360g, root of large-flowered skullcap 210g, earthworm 165g, barrenwort 240g, Radix Glycyrrhizae 105g gomi herbs boiling twice,Each 1 hour, the liquid after collecting decoction and above-mentioned distillation, filtered, and it is 1.02-1.06 that filtrate is concentrated into relative density(60 DEG C), merge above-mentioned three kinds of extracts, and spraying is dry, adds appropriate cane sugar powder, granulate, and to obtain final product.
Get 5 batches of each 5g of Chinese patent drug finished product, lot number is respectively 201401,201403,201406,201407,201410.Porphyrize, adds ethanol 20ml, and ultrasonic extraction 30 minutes filters, filtrate evaporate to dryness, and the residue 5ml that adds water makes to dissolve, logicalCross large pore resin absorption column, with 35% ethanol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml to be madeDissolve, supernatant is as need testing solution. Separately get Bergenin reference substance, add methyl alcohol and make molten containing 1mg of every 1mlLiquid, product solution in contrast, according to thin-layered chromatography (annex VI B of Chinese pharmacopoeia version in 2010) test, inhalesGet the each 3 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, taking ethyl acetate-acetic acid (2:1) as launchingAgent, launches, and takes out, and dries, and puts under ultraviolet lamp (254nm) and inspects.
The results are shown in Figure 2, visible five batches of Chinese patent drug test sample chromatograms with the corresponding position of Bergenin reference substance chromatogramBe set up spot, good separating effect and the clear spot of aobvious same color.
The thin-layer identification method favorable reproducibility of ardisia japonica in the Chinese patent drug of the hot heavy breathing disease for the treatment of that the present invention sets up, specificity be strong,Clear spot, can effectively ensure the stable of this Quality of Chinese Traditional Proprietary Medicine.
Above-described embodiment is described the preferred embodiment of the present invention, not to model of the present inventionEnclose and limit, design under the prerequisite of spirit not departing from the present invention, those of ordinary skill in the art are to skill of the present inventionVarious distortion and improvement that art scheme is made, all should fall in the definite protection domain of the claims in the present invention book.
Claims (5)
1. the discrimination method of ardisia japonica in a Chinese patent drug for the treatment of hot heavy breathing disease, this Chinese patent drug contains Chinese ephedra 160g, ardisia japonica 360g, root of large-flowered skullcap 210g, semen armeniacae amarae 210g, peach kernel 170g, earthworm 165g, fruit of Chinese magnoliavine 140g, barrenwort 240g, fruit of glossy privet 265g, Radix Glycyrrhizae 105g, preparation method is: fruit of glossy privet 265g, fruit of Chinese magnoliavine 140g adds 65% alcohol heating reflux and extracts twice, each 1.5 hours, merge extract, it is 1.07-1.09 that recovery ethanol is concentrated into relative density, separately get Chinese ephedra 160g, semen armeniacae amarae 210g, peach kernel 170g steam distillation, collection distillate is for subsequent use, the dregs of a decoction and ardisia japonica 360g, root of large-flowered skullcap 210g, earthworm 165g, barrenwort 240g, twice of Radix Glycyrrhizae 105g gomi herbs boiling, each 1 hour, liquid after collecting decoction and above-mentioned distillation, filter, it is 1.02-1.06 that filtrate is concentrated into relative density, merge above-mentioned concentrated gained liquid, spraying is dry, add appropriate cane sugar powder, granulation 1000g, obtain,
In this Chinese patent drug, the discrimination method of ardisia japonica composition is:
The preparation of need testing solution: the ethanol elution that adopts large pore resin absorption column absorption, is 35% by mass concentration;
The preparation of reference substance solution: with Bergenin control sample;
Adopt thin-layered chromatography: using the mixed solution of polyamide film expansion, ethyl acetate-acetic acid is solvent, and in the mixed solution of described ethyl acetate-acetic acid, the weight ratio of ethyl acetate and acetic acid is 2:1.
2. method according to claim 1, is characterized in that, the preparation of described need testing solution: get described Chinese patent drug 5g, porphyrize, adds ethanol 20ml, ultrasonic extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 5ml make dissolve, pass through large pore resin absorption column, with 35% ethanol 50ml wash-out, collect eluent, evaporate to dryness, residue adds methyl alcohol 1ml to be made to dissolve, and supernatant is as need testing solution.
3. method according to claim 1, is characterized in that, the preparation of described reference substance solution: get Bergenin, add methyl alcohol and make the solution of every 1ml containing 1mg, product solution in contrast.
4. method according to claim 1, it is characterized in that described thin-layered chromatography: draw need testing solution and the each 3 μ l of reference substance solution, put respectively on same polyamide film, taking the mixed solution of ethyl acetate-acetic acid as solvent, launch, take out, dry, put under ultraviolet lamp and inspect, in test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescent spot of aobvious same color.
5. method according to claim 4, is characterized in that: the ultraviolet wavelength of described ultraviolet lamp is 254nm.
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