CN1954871A - Yanhouqing preparation for treating throat disease and its preparation method and quality control method - Google Patents

Abstract

A Chinese medicine in the form of dripping pill, dispersing tablet, or micropill for treating thirst, painful throat, hoar seness, cough, etc is prepared from 8 Chinese- medicinal materials including Japanese peristrophe herb, coral ardisia root, thinleaf adina root, etc. Its preparing process and quality control method are also disclosed.

Description

The clear preparation of throat and the method for making and the quality control method of treatment laryngopharyngeal diseases

Technical field

The present invention is a kind of clear preparation of throat and method for making and quality control method for the treatment of laryngopharyngeal diseases, belongs to technical field of Chinese medicine.

Technical background

Throat is the first line of defence of human respiratory.In recent years; because the harm of atmospheric pollution and tobacco poisoning; the influence of occupational factor; drink; factors such as the stimulation of dust; laryngopharyngeal diseases is in rising trend; especially in dry winter; air pollution; dust particle rolls up; very easily bring out pharyngolaryngitis, cause people's hoarseness; aphonia; dry pharynx is puckery; itching throat; pharyngalgia; expectoration is not well; the pharynx foreign body sensation is often with the tcs response of " uttering a sound or a word; noise made in coughing or vomiting "; the sensation that these be can't get rid of; as untimely diagnosis and treatment; prevention, easily repeatedly, very obstinate; troublesome throughout one's life probably; even can cause the generation of other disease, happiness in all one's life shortcoming therefore and to some extent makes us suffering untold misery.Throat health is becoming the topic of new millennium medical expert and consumers in general's common concern.Though because what big defect chronic pharyngolaryngitis is not, become the difficult problem of modern medicine really, generally be difficult to return to one's perfect health.For this reason, expert call: vigilant chronic pharyngitis harm, seek the healthy fashion that specific throat medication and natural throat health product are just becoming the new millennium people.So clinical treatment must promptly and accurately be selected appropriate drug preparation and Therapeutic Method.The clear sheet of throat is made up of Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, Mentholum eight flavor medicines.Monarch drug in Herba Peristrophes wind and heat dispersing, the removing toxic substances and promoting subsidence of swelling side of being, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae resolving heat and reducing pathogenic fire, subduing swelling and detoxicating, blood circulation and promoting silt, expelling phlegm for arresting cough are ministerial drug altogether; Radix Tinosporae, Radix Platycodonis are opened lung qi dispersing gas, the evacuation of pus of eliminating the phlegm, and are adjuvant drug in the side, Herba Menthae, Mentholum wind-dispelling heat-dissipating, and the clear sharp head is messenger drug.This side's dispelling wind to relieve the exterior syndrome, heat-clearing and toxic substances removing, clearing throat are used for pharyngalgia, dry pharynx, hoarseness, or symptoms such as fever and aversion to wind, cough are arranged.The clear sheet of throat is determined curative effect clinically, welcome by extensive patients.But also found some problems in secular clinical practice, fallen behind such as dosage form that dose is big, onset is slow, and product quality is not ideal enough, and the dosage form kind is abundant inadequately, is suitable for crowd's narrow range, takes inconvenience etc.In view of such circumstances, optimize technology, improve dosage form, the control method that improves the quality becomes bastard feverfew throat clearing granule urgent problem.

Summary of the invention

The objective of the invention is to: a kind of clear preparation of throat for the treatment of laryngopharyngeal diseases and preparation method thereof and method of quality control are provided; The present invention is directed to prior art, dosage forms such as the drop pill that provides, dispersible tablet have not only solved granule and taken inconvenience and the relatively poor problem of mouthfeel, and disintegrative are good, the bioavailability height; Preparation method provided by the present invention can effectively prepare needs preparation, guarantee that the preparation production technique obtain is scientific and reasonable; The method of quality control that is provided, the means, technical method of the index that detects, detection etc. can be provided to relevant production, testing agency, so that better control the quality of said preparation, guarantee the safety of medication, can better instruct production, make controlling of production process rationally strict more, make consumer's energy full appreciation product quality.

The present invention constitutes like this: calculate according to weight, it mainly is by Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, the preparation that Mentholum 2.5g is made, comprise: injection comprises: injection, the powder pin, freeze-dried powder, gel, tablet, dispersible tablet, capsule, soft capsule, microcapsule, granule, pill, micropill, powder, drop pill, slow releasing preparation, controlled release preparation, gel, oral liquid, soft extract, all acceptable dosage forms on the pharmaceutics such as extractum and membrane.Say accurately: described preparation is drop pill, soft capsule, dispersible tablet.

The method for making of the clear preparation of throat of described treatment laryngopharyngeal diseases: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, merge with above-mentioned aqueous solution, it when being evaporated to 60 ℃ of relative densities 1.10～1.12 clear paste, adding ethanol makes and contains alcohol amount and reach 60%, left standstill 24 hours, filtrate is concentrated, dry at decompression recycling ethanol below 80 ℃, adds Mentholum, spray into above-mentioned volatile oil, make different preparations.Drop pill in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 1～3 add substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 70 ℃～90 ℃ of system temperature, coolant is 5 ℃～30 ℃ a dimethicone, and dripping speed is 20～40d/min, drips distance at 2～12cm, collect drop pill and remove the dimethicone on surface, promptly.Drop pill in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 1.5 adding substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 85 ℃ of system temperature, coolant is 10 ℃～20 ℃ a dimethicone, and dripping speed is 30d/min, drips distance at 4～8cm, collect drop pill and remove the dimethicone on surface, promptly.Soft capsule in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filtering, merge with above-mentioned aqueous solution, is 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, adding ethanol makes and contains alcohol amount and reach 60%, left standstill 24 hours, and filtered, filtrate concentrates at decompression recycling ethanol below 80 ℃, dry, add Mentholum, mix homogeneously is ground into fine powder, sprays into above-mentioned volatile oil again, mixing, airtight 2 hours, press extract powder again: substrate=1: 1.5 adds soybean oil, the mixed-matrix of soybean lecithin, heating and melting, mixing gets soft capsule content; The preparation of glue: with gelatin: glycerol: water=1: 0.7: 1.0, getting gelatin adds an amount of distilled water and makes its imbibition, in addition the water of glycerol and remainder is put and be heated to 70～80 ℃ in the glue pot, mix homogeneously adds expansible gelatin and stirs, and makes it to dissolve into uniform glue, in 60 ℃ of insulations 2～3 hours, leave standstill, remove the come-up foam, filter standby with cloth bag.Soft capsule content and glue are pressed into soft capsule in encapsulating machine, put in the drum drying machine and finalize the design, whole ball, drying, promptly.Dispersible tablet in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, and the aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, and merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, mix homogeneously is ground into fine powder, add 10% microcrystalline Cellulose, 7% crospolyvinylpyrrolidone, mixing adds ethanol, the system soft material, granulate drying, 40 mesh sieve granulate, tabletting behind the mixing, other gets Mentholum, adds ethanol and makes dissolving in right amount, sprays into, spray into above-mentioned volatile oil again, mixing, airtight 2 hours, promptly.

The quality control method of the clear preparation of throat of described treatment laryngopharyngeal diseases, its discrimination method comprise following all or part of content:

A. the thin layer chromatography of Radix Gei japonici is differentiated in the preparation

It is an amount of to get this product powder, adds methanol extraction, and extracting solution evaporate to dryness, residue add water makes dissolving, adds the ethyl acetate jolting and extracts, and acetic acid ethyl fluid evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other the Radix Myricae rubrae control medicinal material of fetching water is an amount of, adds ethyl acetate extraction, and extracting solution evaporate to dryness, residue add methanol makes dissolving, in contrast medical material solution; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution respectively, puts on same silica gel g thin-layer plate, and with chloroform-acetone=4～6: 0.3～0.7 is developing solvent, launch, take out, dry, put under the uviol lamp and inspect, or spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

B. one or both thin layer chromatography discriminating in Radix Ardisiae Crenatae medical material, the Bergeninum in the preparation

It is an amount of to get this product powder, adds the methanol supersound extraction, and extracting solution concentrates, as need testing solution; Get the Radix Ardisiae Crenatae control medicinal material, shine medical material solution in pairs with legal system; Other gets the Bergeninum reference substance, adds methanol and makes reference substance solution; According to the thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution respectively, puts on same silica gel g thin-layer plate, with chloroform-ethyl acetate-ethanol=4～6: be developing solvent at 3～5: 2～4, launches, and takes out, dry, spray is to contain the developer that mixes of ferric chloride and the potassium ferricyanide; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

C. the thin layer chromatography of Radix Platycodonis is differentiated in the preparation

It is an amount of to get this product powder, adds the mixed solution of ethanol solution of sulfuric acid and water, and reflux is put cold, add the chloroform jolting and extract, chloroform liquid adds water washing, discards water liquid, chloroform liquid anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other gets the Radix Platycodonis control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate, and with chloroform-ether=4～5: 5～6 be developing solvent, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.

D. one or both thin layer chromatography discriminating in Herba Menthae medical material, the Mentholum in the preparation

It is an amount of to get this product powder, adds the petroleum ether jolting and extracts, and extracting solution is as need testing solution; Other gets the Herba Menthae medical material, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether and make reference substance solution; Test according to thin layer chromatography, it is an amount of to draw above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=8～10: be developing solvent at 1.5～2.5: 0.8～1.2, launch, take out, dry, spray is with the vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

Say that accurately discrimination method comprises following all or part of content:

A. the thin layer chromatography of Radix Gei japonici is differentiated in the preparation

It is an amount of to get this product powder, adds the methanol supersound extraction, and extracting solution evaporate to dryness, residue add water makes dissolving, adds the ethyl acetate jolting and extracts, and acetic acid ethyl fluid evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other the Radix Myricae rubrae control medicinal material of fetching water is an amount of, adds the ethyl acetate supersound extraction, and extracting solution evaporate to dryness, residue add methanol makes dissolving, in contrast medical material solution; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution respectively, put on same silica gel g thin-layer plate, be developing solvent with chloroform-acetone=5: 0.5, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

B. one or both thin layer chromatography discriminating in Radix Ardisiae Crenatae medical material, the Bergeninum in the preparation

It is an amount of to get this product powder, adds the methanol supersound extraction, and extracting solution concentrates, as need testing solution; Get the Radix Ardisiae Crenatae control medicinal material, shine medical material solution in pairs with legal system; Other gets the Bergeninum reference substance, adds methanol and makes reference substance solution; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, and be developing solvent with chloroform-ethyl acetate-ethanol=5: 4: 3, launch, take out, dry, spray to contain the developer that mixes of ferric chloride and the potassium ferricyanide; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

C. the thin layer chromatography of Radix Platycodonis is differentiated in the preparation

It is an amount of to get this product powder, add the mixed solution of 7% ethanol solution of sulfuric acid-water=1: 3, reflux is put cold, adding the chloroform jolting extracts, chloroform liquid adds water washing, discards water liquid, chloroform liquid anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other gets the Radix Platycodonis control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-ether=4: 6, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.

D. one or both thin layer chromatography discriminating in Herba Menthae medical material, the Mentholum in the preparation

It is an amount of to get this product powder, adds the petroleum ether jolting and extracts, and extracting solution is as need testing solution; Other gets the Herba Menthae medical material, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether and make reference substance solution; According to the thin layer chromatography test, it is an amount of to draw above-mentioned three kinds of solution, puts respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=9: 2: 1 was developing solvent, launched, and took out, dry, spray is with the vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

In the quality control method of the clear preparation of throat of described treatment laryngopharyngeal diseases, its content assaying method comprises following all or part of content:

A. the high performance liquid chromatography assay of Bergeninum in the preparation

It is an amount of to get this product powder, accurate claims surely, puts in the tool plug conical flask, and the accurate methanol that adds claims decide weight, and supersound process is put coldly, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes reference substance solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, with methanol-water=15～21: 85～79 is mobile phase; The detection wavelength is 270～280nm; Accurate respectively absorption reference substance solution and need testing solution are an amount of, inject chromatograph of liquid, measure; Calculate with one point external standard method or standard curve method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 1.5mg every day;

B. the gas chromatography assay of Mentholum in the preparation

It is an amount of to get this product powder, and accurate the title decides, and puts in the tool plug conical flask, the accurate dehydrated alcohol that adds, supersound process is placed to room temperature, claim again to decide weight, supply the weight that subtracts mistake, shake up with dehydrated alcohol, centrifugal, it is an amount of that precision is measured supernatant, and the accurate again inner mark solution that adds is an amount of, adds dehydrated alcohol and is settled to debita spissitudo, shake up, as need testing solution; It is an amount of that naphthalene decided in accurate title, adds anhydrous alcohol solution and make inner mark solution; Other gets the Mentholum reference substance, and accurate the title decides, and the accurate inner mark solution that adds is an amount of, adds dehydrated alcohol and makes reference substance solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 8～12%; Column temperature is 110～150 ℃; Draw an amount of inject gas chromatograph of reference substance solution, calculate than positive divisor; The absorption need testing solution is an amount of, and inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 15mg every day.

Say that accurately content assaying method comprises following all or part of content:

A. the high performance liquid chromatography assay of Bergeninum in the preparation

Get this product, porphyrize is got about 0.2g, accurate claims surely, puts in the tool plug conical flask, and the accurate methanol 25ml that adds claims decide weight, and supersound process 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes the solution that every 1ml contains 0.05mg, in contrast product solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, be mobile phase with methanol-water=18: 82; The detection wavelength is 275nm; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; Calculate with one point external standard method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 3.Omg every day;

B. the gas chromatography assay of Mentholum in the preparation

It is an amount of to get this product, and porphyrize is got 1g, and accurate the title decides, put in the tool plug conical flask, the accurate dehydrated alcohol 20ml that adds claims to decide weight, ice-bath ultrasonic was handled 30 minutes, was placed to room temperature, claimed to decide weight again, supply the weight that subtracts mistake with dehydrated alcohol, shake up, centrifugal, precision is measured supernatant 5ml, puts in the 10ml measuring bottle, the accurate inner mark solution 2ml that adds, add dehydrated alcohol to scale, shake up, as need testing solution; Get naphthalene 150mg, the accurate title, decide, and puts in the 100ml measuring bottle, adds anhydrous alcohol solution and be diluted to scale, as inner mark solution; Other gets Mentholum reference substance 10mg, and accurate the title decides, and puts in the 10ml measuring bottle, and the accurate inner mark solution 2ml that adds adds dehydrated alcohol to scale, shakes up, in contrast product solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 10%; With Chromosorb W (AW-DMCS) (60-80 order) is carrier, and column temperature is 140 ℃; Draw reference substance solution 1 μ l, inject gas chromatograph calculates than positive divisor; Draw need testing solution 1 μ l, inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 20mg every day.

Compare with technology with existing dosage form, the invention solves dosage form and be suitable for crowd's narrow range, take inconvenience, the unfavorable problem of medicine stability.Its preparation formulation taking convenience, bioavailability height, good stability, easy to carry, good mouthfeel, absorption be fast, it is wide to be suitable for the crowd; The preparation method that is provided can effectively prepare needs preparation, guarantee that the preparation variety effect obtain is remarkable, production technology is scientific and reasonable, has overcome the problem that existing product exists; The method of quality control that is provided can more fully be controlled the quality of said preparation; Reached purpose of the present invention.

The applicant finds in development process, is the assurance product quality, the screening of adjuvant, process conditions, and the screening of all conditions of method of quality control is most important.The applicant has carried out a series of experiments, with method and parameter of the supplementary product kind of the preparation technology that selects pharmaceutical preparation provided by the invention, use and consumption and ratio, quality control etc.; To guarantee science, reasonability, the feasibility of invention.

Experimental example 1: Study on extraction

1. volatile oil extraction conditions screening

(1) factor selective volatilization oil extraction effect is subjected to the influence of factors such as amount of water, extraction time.Therefore choose amount of water and extraction time as factor, the varying level of high spot reviews factor is to the influence of volatile oil extraction effect.

(2) to determine to select oil mass be evaluation index to index, and assay method is as follows:

Take by weighing respectively three parts of Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g respectively, decoct with water, collect volatile oil simultaneously, receive oil mass every 1 hour record.

(3) test: test arrangement and the results are shown in following table.

Volatile oil extracts investigates table as a result

Extraction time (h) oil pump capacity (ml) amount of water (doubly)	1	2	3	4	5	6	7	8
									8 10 12	0.2 0.6 0.8	0.8 1.0 1.3	1.5 1.6 1.6	1.8 2.1 2.1	2.2 2.6 2.6	2.6 3.2 3.2	2.6 3.2 3.2	2.6 3.2 3.2

As seen from the above table, amount of water is put forward oil mass for 10 times and 12 times and is more or less the same, and extracts after 6 hours volatile oil and carries substantially to the greatest extent, from saving time and the angle of the energy, selects to add 10 times of water extraction 6 hours.And carry out demonstration test according to these process conditions.

2. the screening of water boiling and extraction condition

(1) factor is selected: the decocting for Chinese herbal medicine extraction effect is subjected to the influence of factors such as amount of water, extraction time, extraction time.Though prior art is investigated extraction time, extraction time, amount of water is not done any research as key factor, and the varying level of the applicant's high spot reviews factor is to decocting the influence of extraction effect.Take all factors into consideration the selection factor level in conjunction with aspects such as production cost, the energy.

(2) index is determined:

1. select the extractum recovery rate as evaluation index.Extractum is the material base of solid preparation performance curative effect, and its yield height directly influences preparation process, is reasonable, effective control device so be chosen as the extraction index.

2. Bergeninum content: extractum yield height can not reflect fully that active ingredient extracts situation, so select in the prescription the contained main component Bergeninum of Radix Ardisiae Crenatae content as the decoction screening index simultaneously; With reference to relevant document, adopt reversed phase high efficiency liquid phase method to measure Bergeninum content.

(3) decoct test: take by weighing respectively three parts of Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g respectively, add 10 times of water extraction volatile oil respectively, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, filtrate and above-mentioned aqueous solution merge, being evaporated to relative density is the clear paste of 1.10～1.12 (60 ℃), adds ethanol and makes and contain alcohol amount and reach 60%, leaves standstill 24 hours, filter, filtrate decompression concentrates, drying, and it is heavy to claim to decide cream, calculate paste-forming rate, result of the test sees the following form.

Amount of water is investigated table as a result

Tested number	Amount of water (doubly)	Extractum recovery rate (%)	Bergeninum content (mg/g)
				1 2 3	6 8 10	3.31 4.48 4.52	12.28 17.68 17.52

As seen from the above table: extractum recovery rate and Bergeninum content were higher when amount of water was 10 times and 8 times amount, and not significantly difference between the two, guaranteeing under the sufficient prerequisite of extracts active ingredients,, determining that extracting amount of water is 8 times of amounts in order to save cost and to shorten man-hour.

(4) confirmatory experiment carries out confirmatory experiment by above extraction process condition, the experimental result tabulation:

Decoct amount of water confirmatory experiment result

Scheme	Tested number	Extractum recovery rate (%)	Bergeninum content (mg/g)
				Decoct each 8 times of amounts 1 time	1 2 3	4.68 4.35 5.02	17.45 18.02 17.23

Remarks: investigation amount 500g

As seen decoct the optimum organization condition by the result of confirmatory experiment and extract that extractum yield and the fluctuation of Bergeninum content are little as a result, as seen this extraction process condition is reasonable, feasible and stable.

In sum, Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae add 10 times of water extraction volatile oil in the side, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, filtrate and distillate are evaporated to the clear paste that relative density is 1.10～1.12 (60 ℃) after merging, add ethanol and make and contain alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate decompression concentrates, drying.

Experimental example 2 reclaims ethanol research

For the ease of production operation control with avoid loss of effective components, take decompression recycling ethanol, and concentrating under reduced pressure, cream, standby.The condition of alcohol extraction medicinal liquid concentrating under reduced pressure is: temperature is 60 ℃, and vacuum is 0.08～0.1Mpa.

Experimental example 3 separates, concentrates and drying process research

Separating technology research: for the ease of production operation control, extracting solution adopts 200 order filter clothes to filter.

Concentration technology research: concentrate and adopt the triple effect concentration tank to concentrate, extracting solution is concentrated into the thick paste that relative density is 1.10～1.12 (60 ℃); Recovery ethanol concentrates, and the relative density of concentrated solution is that the concentrated condition of 1.25～1.30 (70 ℃) is: temperature is 84 ℃ of effects, two 80 ℃ of effects, 70 ℃ of triple effects, and vacuum is an effect-0.025Mpa, two effect-0.045Mpa, triple effect-0.065Mpa.

Drying process research: the vacuum drying condition is: 60～70 ℃, and-0.08Mpa.

Experimental example 4: Study on Forming

4.1 dispersible tablet Study on Forming

Dispersible tablet meet water rapidly disintegrate form the water dispersion tablet of uniform sticky suspension, it is poor to have solved former dosage form disintegrative, stripping is shortcoming slowly, and the dispersible tablet that the applicant makes is fully disintegrate in the 3min in 19 ℃～21 ℃ water, and suspension ability is good, bioavailability is high, be uniformly dispersed.

Check disintegration: adopting changes the basket method, and the lift disintegration tester is got 6, observes the situation by screen cloth, and percent of pass height then disintegrative is good, more pleasant bulk absorption.

Group	Microcrystalline Cellulose %	Crospolyvinylpyrrolidone %	Disintegration time s
				1 2 3 4 5 6 7 8 9	10 10 10 15 15 15 18 18 18	3 5 7 3 5 7 3 5 7	110 95 72 105 136 89 213 114 101

The result shows that optimum process condition is for adding 10% microcrystalline Cellulose, 7% crospolyvinylpyrrolidone, and mixing adds ethanol, the system soft material.

4.2 soft capsule Study on Forming

4.2.1 the adsorbing base rate is investigated

Medicated powder: substrate suspension situation

1: 1.0 inhomogeneous suspension

1: 1.5 even suspension

1: 2.0 even suspension

4.2.2 adjuvant is to the influence of composition:

Group Bergeninum (mg/g)

Medicated powder 0.51

Add after the substrate 0.49

The result shows that optimum process condition is for pressing medicated powder: substrate=1: 1.5, Bergeninum content did not have significant change after medicated powder added substrate.

4.3 drop pill Study on Forming

4.3.1 the initial option of substrate

Drop pill requires preparation to bring into play curative effect rapidly, and medicine contains volatile ingredient in addition, so select fusing point low, the PEG4000 with fine dispersion power and big cohesiveness satisfies the requirement of clinical treatment and active ingredient character as substrate.Preliminary study shows that when making substrate with PEG4000, the hardness of drop pill, flowability are all good, the results are shown in following table.

Substrate screening experiment result

Matrix species	Hardness	Roundness	Hangover
				PEG4000 PEG6000	+++ +++	+++ +	Do not hold in the palm a little holder tail of tail

Annotate: +++show fine; ++ show better; + show general

4.3.2 medicine and substrate composition

Mix the back situation with substrate and drip the system complexity with medicine, establish the proportioning of medicine and substrate.See the following form.The result shows that the ratio of medicine and Macrogol 4000 is at 1: 1.5 o'clock, and medicine and substrate amalgamation are better, and hardness, roundness suit, and is easy to the system of dripping.

The proportioning test result of medicine and substrate

The proportioning of medicine and substrate	Hardness	Roundness	Hangover
				1∶1 1∶1.2 1∶1.5 1∶2 1∶3	+ ++ +++ +++ +++	- - +++ ++ +	Obviously do not trail and or not

Annotate: +++show fine; ++ show better; + show general;-differential

4.3.3 coolant is selected

Earlier with medicine: the ratio of Macrogol 4000=1: 1.5, from methyl-silicone oil, liquid Paraffin, soybean oil, Oleum Arachidis hypogaeae semen, rapeseed oil, select suitable condensing agent.Decrease speed, molding situation with drop pill are index, with the investigation result of each index by good to poorly using " +++" successively, " ++ ", "+", "-" expression the results are shown in following table.

The selection experimental result of coolant

Condensing agent	Decrease speed	The molding situation
			Dimethicone liquid Paraffin soybean oil rapeseed oil	+++ - ++ ++	+++ ++ - +

Annotate: +++show fine; ++ show better; + show general

As seen from the above table, coolant selection dimethicone is good.

4.3.4 dripping the system temperature selects

The too high meeting of polyethylene glycols heating temperature color and luster occurs and deepens to be difficult for solidifying.Drip the system temperature as can be known when 80 ℃ of left and right sides by prerun test, it is very slow to drip speed, and molding is bad.Select to drip the system temperature about 85 ℃, a speed is moderate, and molding is good.By preferred medicine and substrate composition, extractum and substrate to be put in the water-bath heat, fusion adds in the drop pill machine, and the different temperatures insulation is spent so that pill shaped circle is whole, and the state of oozing is an index, the results are shown in following table.

Drip the selection experimental result of system temperature

Drip the system temperature (℃)	Roundness	Ooze state
			70 80 85 90	- + +++ +	Can not drip more easily ooze too fast

Annotate: +++show fine; ++ show better; + show general;-differential

4.3.5 coolant temperature is investigated

By preferred medicine and substrate composition, mix homogeneously is heated to 80-90 ℃, treat whole fusions after, get in right amount, splash into respectively in the dimethyl-silicon oil coolant of different temperatures, observe drop pill molding situation, the results are shown in following table.

Coolant temperature is selected

Coolant temperature	Drip distance	Drip speed	The material temperature	Drop pill molding situation
					10 ℃ of 20 ℃ of gradients coolings	6cm 6cm 6cm	30～40d/min 30～40d/min 30～40d/min	85℃ 85℃ 85℃	Roundness is good, and the forming roundness is good, and the forming roundness is good, forming

Annotate: the gradient cooling means is: top is 10～20 ℃, and the bottom is 5～10 ℃.

Last table shows that under above-mentioned three kinds of chilling temperatures, the mouldability of this product is all good, is easy operation, is 10～20 ℃ so select coolant temperature.

4.3.6. resitting an exam, ball examines

By above optimum condition, select the dropper of different bores, drip and make ball, with the whole degree of pill shaped circle, hardness, hangover the results are shown in following table for index.

Ball is resit an exam and is examined experimental result

Bore (inside/outside mm/mm)	Ball heavy (mg)	Roundness	Hardness	Hangover
					3.0/4.0 4.0/5.0 5.0/6.0	40 60 70	+++ +++ -	+ +++ +	Do not ask tail not hold in the palm tail holder tail

Annotate: +++show fine; ++ show better; + show general;-differential

The above results shows, the water dropper bore is that appearance index such as the drop pill roundness of the water dropper of 4.0/5.0 (inside/outside mm/mm) system of dripping and hardness are better, so selection water dropper bore is 4.0/5.0 (inside/outside mm/mm).

4.3.7 dripping speed investigates

By above optimum condition, select the different speed of dripping, drip and make ball, with the whole degree of pill shaped circle, hardness, trailing is index, the results are shown in following table.

Drip speed and investigate experimental result

Drip speed (d/min)	Roundness	Hardness	Hangover
				20 30 40	+++ +++ -	+ +++ +++	The hangover of not trailing

Annotate: +++show fine; ++ show better; + show general;-differential

So can determine that by last table dripping speed is 30d/min.

4.3.8 drip apart from investigating

By above optimum condition, select the different distances of dripping, drip and make ball, with the whole degree of pill shaped circle, hardness, hangover the results are shown in following table for index.

Drip apart from investigating experimental result

Drip apart from (cm)	Weight differential	The drop pill outward appearance
			2 4 8 12	------ 6％ 8％ 17％	The drop pill adhesion, roundness difference drop pill outward appearance rounding, smooth surface drop pill outward appearance rounding, smooth surface drop pill outward appearance rounding, smooth surface

Last table shows, when dripping apart from the time at 4～8cm, and drop pill outward appearance rounding, smooth surface, weight differential is little, is 4～8cm so select to drip a distance.

Experimental example 5: the research of antiinflammatory action

5.1 the influence of xylol induced mice otitis

Get 50 of mices, the male and female dual-purpose, body weight 18～22g is divided at random: matched group, the clear sheet group of throat, preparation group of the present invention, 10 every group.Clear sheet group of throat and formulation components of the present invention are not pressed the dosage gastric infusion in the table 4, matched group is given isopyknic normal saline, 1h after the administration, every Mus auris dextra is coated with the dimethylbenzene with 0.3ml, cause scorching back 4 hours, take off the auricle of ears same position, weigh with the 8mm card punch, with two ear weight differences is the swelling index, the results are shown in following table.

Group	Dosage (g/kg)	Left and right sides ear weight difference (mg)
			The clear sheet group of matched group throat drop pill group of the present invention dispersible tablet group of the present invention soft capsule group of the present invention	- 6 6 6 6	24.4±1.5 18.0±2.3 17.1±1.2 17.4±3.0 17.2±0.8

5.2 influence to ankle swelling in rat

Get 50 of rats, male and female dual-purpose, body weight 180～220g are divided at random: matched group, the clear sheet group of throat, preparation group of the present invention, 10 every group.Clear sheet group of throat and formulation components of the present invention are not pressed the dosage gastric infusion in the table 5, every day 1 time, 3d continuously.1h after the last administration, right back sufficient plantar subcutaneous injection 1% carrageenin solution 0.1ml/ only causes inflammation rat, and before the Yu Zhiyan and cause scorching back 1,2,5,8h, measure the girth of the right back ankle joint of rat respectively with inelastic tape, and the difference of the girth of consequently scorching front and back ankle joint the results are shown in following table as the swelling degree.

Group	Dosage (g/kg)	Ankle swelling in rat degree (mm)
					1h	2h	5h
		The clear sheet group of matched group throat drop pill group of the present invention dispersible tablet group of the present invention soft capsule group of the present invention	- 6 6 6 6	3.56±1.87 1.82±0.54 1.70±0.18 1.71±0.54 1.69±0.66				9.75±4.21 6.48±0.51 6.20±1.22 6.19±2.03 6.23±1.88	12.98±1.46 7.86±2.05 7.77±2.29 7.75±0.98 7.79±3.04

More than two experimental results show that preparation of the present invention can obviously alleviate mice ear due to the dimethylbenzene and the ankle swelling in rat due to the carrageenin, action intensity is not less than the clear sheet of throat of same dose.

The thin layer chromatography discrimination method of Radix Gei japonici research in experimental example 6 drop pills

Feature for outstanding Radix Gei japonici, selected the characteristic component speckle in the Radix Gei japonici medical material to contrast as it, but owing to there are composition, for example liposoluble constituent in Herba Peristrophes, the Radix Ardisiae Crenatae like the close or polar phase of characteristic component structure in more and the Radix Gei japonici medical material in the preparation.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving multiple unfolding condition, part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Radix Gei japonici research in the drop pill

Condition	The result
		Benzinum (30～60 ℃)-ethanol=15: 4 silica gel H lamellae chloroform-acetone-glacial acetic acid=10: 1: 1 silica gel 6F254 lamellae n-hexane-ethyl acetate=9: 1 silica gel g thin-layer plate chloroform-acetone=5: 0.5 silica GF254 lamellae toluene-methyl alcohol=5: 1 silica gel 6F254 lamellae chloroform-acetone=6: 0.3 silica gel g thin-layer plate chloroform-acetone=4: 0.7 silica gel g thin-layer plate chloroform-acetone=5: 0.5 silica gel g thin-layer plates	Separating unintelligible feminine gender has the Rf value of interference feminine gender on the low side to have the interference separation poor separation clear, Rf value is low slightly, negative noiseless separation is clear, Rf value is high slightly, negative noiseless separation is the most clear, Rf value is moderate, and is negative noiseless

Through screening, determined optimum condition: with the silica gel g thin-layer plate immobile phase, chloroform-acetone=be developing solvent at 5: 0.5, with this understanding, the Rf value of Radix Gei japonici medical material feature speckle is moderate, and it is the most clear to separate with other speckle, negative noiseless.

The thin layer chromatography discrimination method of Radix Ardisiae Crenatae medical material, Bergeninum research in experimental example 7 dispersible tablets

For the feature of outstanding Radix Ardisiae Crenatae, selected Bergeninum as its characteristic component, but owing to had composition, for example saponin component in Radix Platycodonis, the Radix Tinosporae like the more or polar phase close in the preparation with the Bergeninum structure.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving multiple unfolding condition, part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Radix Ardisiae Crenatae medical material, Bergeninum research in the dispersible tablet

Condition	The result
		Benzinum (30～60 ℃)-ethanol=8: 1 silica gel g thin-layer plate chloroform-acetone-methyl alcohol=10: 1: 1 silica GF254 lamellae n-hexane-ethyl acetate=9: 1 silica GF254 lamellae chloroform-acetone=5: 1 silica gel g thin-layer plate chloroform-ethyl acetate-ethanol=8: 3: 4 silica gel g thin-layer plate chloroform-ethyl acetate-ethanol=6: 3: 4 silica gel g thin-layer plate chloroform-ethyl acetate-ethanol=4: 5: 2 silica gel g thin-layer plate chloroform-ethyl acetate-ethanol=5: 4: 3 silica gel g thin-layer plates	Separating unintelligible feminine gender has the Rf value of interference feminine gender on the low side to have the interference separation poor separation clear, Rf value is low slightly, negative noiseless separation is clear, Rf value is high slightly, negative noiseless separation is the most clear, Rf value is moderate, and is negative noiseless

Through screening, determined optimum condition: with the silica gel g thin-layer plate immobile phase, chloroform-ethyl acetate-ethanol=be developing solvent at 5: 4: 3, with this understanding, the Rf value of Bergeninum feature speckle is moderate, and it is the most clear to separate with other speckle, negative noiseless.

The thin layer chromatography discrimination method of Radix Platycodonis research in experimental example 8 pellets

For the feature of outstanding Radix Platycodonis, selected the characteristic component speckle of Radix Platycodonis medical material to be contrast, but owing to had composition, for example saponin component in Radix Tinosporae, the Herba Peristrophes like the more or polar phase close in the preparation with the Bergeninum structure.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, experiment sieving multiple unfolding condition, part unfolding condition and result are as follows:

The thin layer chromatography discrimination method of Radix Platycodonis research in the pellet

Condition	The result
		Chloroform-ethanol=9: 1 silica gel H lamellae chloroform-acetone-methyl alcohol=15: 3: 1 silica GF254 lamellae n-hexane-ethyl acetate=7: 1 silica GF254 lamellae chloroform-acetone=5: 1 silica gel g thin-layer plate chloroform-ethyl acetate-ethanol=8: 3: 4 silica gel g thin-layer plate chloroform-ether=3: 7 silica gel g thin-layer plate chloroform-ether=5: 5 silica gel g thin-layer plate chloroform-ether=4: 6 silica gel g thin-layer plates	The higher feminine gender of Rf value has the unintelligible feminine gender of interference separation to have interference separation poor separation poor separation clear, Rf value is low slightly, negative noiseless separation is the most clear, Rf value is moderate, and is negative noiseless

Through screening, determined optimum condition: with the silica gel g thin-layer plate immobile phase, chloroform-ether=be developing solvent at 4: 6, with this understanding, the Rf value of Radix Platycodonis medical material characteristic component speckle is moderate, and it is the most clear to separate with other speckle, negative noiseless.

Herba Menthae medical material, the research of Mentholum thin layer chromatography discrimination method in experimental example 9 microcapsules

Feature for outstanding Herba Menthae, selected Mentholum as its characteristic component, but owing to there are composition, for example the volatile oil composition in the medical materials such as Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, Radix Tinosporae like the more or polar phase close in the preparation with the Mentholum structure.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of thin layer chromatography effect quality is the composition of unfolding condition, particularly developing solvent.Therefore, the test silica gel g thin-layer plate is an immobile phase, has screened multiple developing solvent, and part developing solvent and result are as follows:

Herba Menthae medical material, the research of Mentholum thin layer chromatography discrimination method in the microcapsule

Condition	The result
		Benzene-chloroform=9: 1 silica gel g thin-layer plate chloroform-acetone-methyl alcohol=10: 1: 1 n-hexane-ethyl acetate=9: 1 chloroform-acetone=5: 1 chloroform-ethyl acetate-ethanol=8: 3: 4 cyclohexane-ethyl acetate-chloroform=8: 1.5: 1.2 cyclohexane-ethyl acetate-chloroform=10: 2.5: 0.8 cyclohexane-ethyl acetate-chloroform=9: 2: 1	Separating unintelligible feminine gender has the Rf value of interference feminine gender on the low side to have the interference separation poor separation clear, Rf value is low slightly, negative noiseless separation is clear, Rf value is high slightly, negative noiseless separation is the most clear, Rf value is moderate, and is negative noiseless

Through screening, determined optimum condition: with the silica gel g thin-layer plate immobile phase, cyclohexane extraction-ethyl acetate-chloroform=be developing solvent at 9: 2: 1, with this understanding, the Rf value of Mentholum feature speckle is moderate, and it is the most clear to separate with other speckle, negative noiseless.

The high performance liquid chromatography assay of Bergeninum research in experimental example 10 drop pills

1 instrument and reagent

1.1 key instrument

High performance liquid chromatograph 1100Series Agilent

The general all purpose instrument company limited of analysing in ultraviolet spectrophotometer TU-1800SPC Beijing

Electronic analytical balance BP211D SARTORIUS

Ultrasonic washing unit KQ250B Kunshan Ultrasonic Instruments Co., Ltd.

1.2 reagent

Methanol analytical pure Beijing Chemical Plant

Acetonitrile chromatographically pure CALEDON

The pure Beijing of phosphoric acid top grade chemical reagents corporation

The pure water WAHAHA

It is an amount of that the 2 selection precisions that detect wavelength take by weighing the Bergeninum reference substance, adds methanol and make the solution that every 1ml contains 50 μ g, in the interscan of 200～400nm wave-length coverage.The result shows that Bergeninum has absorption maximum at the 275nm place, therefore selects 275nm as the detection wavelength of measuring Bergeninum content in the featherleaf rodgersflower and pyrola herb contained tablet for treating mammary disease.

3 chromatographic conditions

Chromatographic column: Diamonsil (diamond) C ₁₈(250 * 4.6mm, 5 μ m);

Mobile phase: methanol-water (18: 82);

Detect wavelength: 275nm;

Flow velocity: 1ml/min;

Test and Selection Bergeninum as its index components, but owing to have for example saponin component in Radix Platycodonis, the Radix Tinosporae of composition like the more or polar phase close in the preparation with the Bergeninum structure.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of high performance liquid chromatography effect quality is the composition of elution requirement, particularly mobile phase.Therefore, experiment sieving multiple mobile phase, part mobile phase and result are as follows:

The investigation of chromatographic condition

The mobile phase condition	The result
		Methanol-water=50: 50 acetonitrile-water=60: 20 acetonitrile-0.05mol/L sodium dihydrogen phosphate=10: 90 methanol-water=30: 70 methanol-water=21: 79 methanol-water=15: 85 methanol-water=18: 82	The incomplete separation of the long separation of the incomplete appearance time of the incomplete separation of separation is clear, negative noiseless retention time is long slightly, it is clear to separate, negative noiseless retention time is moderate, it is the most clear to separate, negative noiseless

Through screening, determined with the octadecylsilane chemically bonded silica to be immobile phase, methanol-water=18: 82 be a mobile phase, and with this understanding, the Bergeninum retention time is moderate, and the peak is capable sharp-pointed, symmetry, it is the most clear to separate with adjacent peak, and feminine gender is noiseless.

4 algoscopys

Get this product, porphyrize is got about 0.2g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, supersound process (power 250W, frequency 33KHz) 60 minutes, take out, put to room temperature, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, as need testing solution; It is an amount of to get the Bergeninum reference substance, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 0.05mg, in contrast product solution; Accurate respectively each the 10 μ l of above-mentioned two kinds of solution that draw inject chromatograph of liquid, measure, promptly.

The investigation precision of 5 linear relationships is measured Bergeninum reference substance solution (0.5136mg/ml) 0.4ml, 0.8ml, 1.2ml, 1.6ml, 2.0ml, split in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, be mixed with the reference substance solution of 0.020544mg/ml, 0.041088mg/ml, 0.061632mg/ml, 0.082176mg/ml, 0.10272mg/ml, the therefrom accurate respectively 10 μ l that draw inject chromatograph of liquid, according to high effective liquid chromatography for measuring.With the peak area is abscissa, and Bergeninum sample size (μ g) is figure for vertical coordinate, the drawing standard curve.The result is as follows:

The Bergeninum linear relationship

Numbering	Peak area	Bergeninum (μ g)
			1 2 3 4 5	262.23 530.14 801.55 1073.15 1320.08	0.20544 0.41088 0.61632 0.82176 1.02720

Regression equation: Y=0.000772X+0.000325

Correlation coefficient: γ=0.9999

The result shows that Bergeninum linear relationship between 0.20544 μ g～1.0270 μ g is good.

Through calculating, the Bergeninum standard curve is one to cross the straight line of initial point, therefore selects one point external standard method to measure the content of Bergeninum in the throat clearing dropping pill.

The test of 6 precision is accurate draws with a Bergeninum reference substance solution 10 μ l, injects chromatograph of liquid, and replication 5 times is investigated reference substance solution precision, and measurement result is as follows:

The precision test

Test number (TN)	1	2	3	4	5	Meansigma methods	RSD(％)
								Peak area	680.70	685.23	681.16	688.94	675.38	682.28	0.74

The result shows that reference substance solution precision is good.

7 need testing solution stability tests are accurate to be drawn with a need testing solution 10 μ l, injects chromatograph of liquid, measures at 0,2,4,8,24 hour sample introduction respectively, and measurement result is as follows:

Need testing solution stability test result

Testing time (h)	0	2	4	8	24	Meansigma methods	RSD(％)
								Content (mg/ grain)	0.3812	0.3774	0.3805	0.3826	0.3769	0.3797	0.65

The result shows that need testing solution is good at 24 hours internal stabilities.

8 replica tests are got same lot number this product, and porphyrize is got about 0.2g (totally 5 parts), and accurate the title decides, and press operation under chromatographic condition and the algoscopy item.The result is as follows:

Replica test

Numbering	1	2	3	4	5	Meansigma methods	RSD(％)
								Content (mg/ grain)	0.3783	0.3821	0.3856	0.3746	0.3805	0.3802	1.08

The result shows that repeatability is good.

The application of sample absorption method is adopted in the test of 9 average recoveries, gets this product under the weight differential item, and porphyrize is got about 0.1g, and accurate the title decides, and puts in the tool plug conical flask; Precision is measured Bergeninum (0.6092mg/ml) 0.8mg, 1.0ml, 1.2ml (each 2 parts) split in the above-mentioned tool plug conical flask, and precision adds methanol to 25ml, close plug, claim to decide weight, supersound process (power 250W, frequency 33KHz) 60 minutes, take out, put, claim to decide weight to room temperature, supply the weight that subtracts mistake with methanol, shake up, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, press operation under chromatographic condition and the algoscopy item, measure, promptly.Measurement result is as follows:

The test of Bergeninum average recovery

Numbering	Weighing (g)	Bergeninum amount (mg) in the test sample	Bergeninum addition (mg)	Measured value (mg)	The response rate (%)
						1 2 3 4 5 6	0.10525 0.11073 0.10594 0.11215 0.10958 0.10737	0.6415 0.6749 0.6457 0.6836 0.6679 0.6544	0.48736 0.48736 0.60920 0.60920 0.73104 0.73104	1.1205 1.1497 1.2480 1.2803 1.3853 1.3783	98.28 97.42 98.87 97.95 98.13 99.02

Average recovery rate=98.27%, RSD=0.60%.

10 sample sizes are measured and are pressed chromatographic condition and the operation down of algoscopy item, measure ten batch samples, and the result is as follows:

The content of Bergeninum in the throat clearing dropping pill

Lot number	Bergeninum on average contains (mg/ grain)
		1 2 3 4 5 6 7 8 9 10	0.3774 0.3851 0.3695 0.3901 0.3887 0.3795 0.3824 0.3885 0.3793 0.3815

The gas chromatography assay of Mentholum research in experimental example 11 dispersible tablets

1 instrument and reagent

1.1 key instrument

Gas chromatograph day island proper Tianjin company

Electronic analytical balance BP211D SARTORIUS

Ultrasonic washing unit KQ250B Kunshan Ultrasonic Instruments Co., Ltd.

1.2 reagent

Ethanol analytical pure Beijing Chemical Plant

The pure water WAHAHA

2 chromatographic conditions

Glass column (3.2mm * 2.1m); With PEG-20M is immobile phase; Coating concentration is 10%; Column temperature is 140 ℃; Fid detector; Nitrogen (50ml/min), hydrogen (50ml/min), air (500ml/min).

Test and Selection Mentholum as its index components, but owing to have composition, for example the volatile oil composition in the medical materials such as Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, Radix Tinosporae like the more or polar phase close in the preparation with the Mentholum structure.Have only the interference of getting rid of these compositions, could obtain ideal chromatograph effect.The key factor of gas phase color method effect quality is factors such as the kind, coating concentration, post of elution requirement, particularly immobile phase.Therefore, test is screened above factor related levels, and partial condition and result are as follows:

The investigation of chromatographic condition

The mobile phase condition	The result
		PEG-20M is an immobile phase; Coating concentration is 5%; Column temperature is that 200 ℃ of PEG-20M are immobile phase; Coating concentration is 5%; Column temperature is that 110 ℃ of SE-54 are immobile phase; Coating concentration is 20%; Column temperature is that 130 ℃ of SE-54 are immobile phase; Coating concentration is 10%; Column temperature is that 140 ℃ of PEG-20M are immobile phase; Coating concentration is 12%; Column temperature is that 150 ℃ of PEG-20M are immobile phase; Coating concentration is 8%; Column temperature is that 110 ℃ of PEG-20M are immobile phase; Coating concentration is 10%; Column temperature is 140 ℃	Not exclusively the incomplete separation of separation is more clear to separate the incomplete separation of incomplete separation, negative noiseless separation is more clear, negative noiseless retention time is moderate, it is the most clear to separate, negative noiseless

Through screening, determined optimum condition: be immobile phase with PEG-20M, coating concentration is 10%, and column temperature is 140 ℃; With this understanding, the Mentholum retention time is moderate, and the peak is capable sharp-pointed, symmetry, and it is the most clear to separate with adjacent peak, negative noiseless.

3 algoscopys

It is an amount of to get this product, and porphyrize is got 1g, and accurate the title decides, put in the tool plug conical flask, the accurate dehydrated alcohol 20ml that adds claims to decide weight, ice-bath ultrasonic was handled 30 minutes, was placed to room temperature, claimed to decide weight again, supply the weight that subtracts mistake with dehydrated alcohol, shake up, centrifugal, precision is measured supernatant 5ml, puts in the 10ml measuring bottle, the accurate inner mark solution 2ml that adds, add dehydrated alcohol to scale, shake up, as need testing solution; Get naphthalene 150mg, the accurate title, decide, and puts in the 100ml measuring bottle, adds anhydrous alcohol solution and be diluted to scale, as inner mark solution; Other gets Mentholum reference substance 10mg, and accurate the title decides, and puts in the 10ml measuring bottle, and the accurate inner mark solution 2ml that adds adds dehydrated alcohol to scale, shakes up, in contrast product solution; Draw reference substance solution 1 μ l, inject gas chromatograph calculates than positive divisor; Draw need testing solution 1 μ l, inject gas chromatograph is measured.

The investigation of 4 linear relationships

Get the reference substance solution of variable concentrations, sample introduction 1 μ l does linear regression with sample size and peak area respectively.The result shows that Mentholum sample size linear relationship between 0.314 μ g～3.143 μ g is good, correlation coefficient γ＞0.9999.

The test of 5 precision

Test shows that the accurate reference substance solution 10 μ l that draw inject chromatograph of liquid, calculate than positive divisor replication 5 times.RSD=0.91% shows that instrument precision is good as a result.

6 need testing solution stability tests are accurate to be drawn with a need testing solution 10 μ l, injects chromatograph of liquid, measures at 0,2,4,8,24 hour sample introduction respectively, calculates than positive divisor.RSD=0.97% shows that need testing solution is good at 24 hours internal stabilities as a result.

7 replica tests are got same lot number this product, and porphyrize is got about 1g, accurate claim surely, press under chromatographic condition and the algoscopy item and operate, and prepare and measure 5 duplicate samples, Mentholum content in the calculation sample.RSD=2.15% shows that repeatability is good as a result.

The application of sample absorption method is adopted in 8 average recoveries tests; get this product; porphyrize, get about 0.5g (totally 6 parts), accurate claim fixed; split in the tool plug conical flask; the accurate Mentholum reference substance solution that adds, make in the sample Mentholum actual content suitable, press respectively again under chromatographic condition and the algoscopy item and operate; mensuration, the calculating Mentholum response rate with addition.Average recovery rate=98.7% as a result, RSD=1.26%.The result shows that the method response rate is good.

9 sample sizes are measured and are pressed chromatographic condition and the operation down of algoscopy item, measure ten batch samples, and the result is as follows:

The content of Mentholum in the throat Yiqing dispersing tablets

Lot number	Mentholum average content (mg/ sheet)
		1 2 3 4 5 6 7 8 9 10	5.5 5.6 5.6 5.5 5.4 5.5 5.6 5.4 5.3 5.5

Concrete embodiment

Embodiments of the invention 1: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 1.5 adding substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 85 ℃ of system temperature, coolant is 15 ℃ a dimethicone, and dripping speed is 30d/min, drips distance at 6cm, collect drop pill and remove the dimethicone on surface, promptly get drop pill, oral, one time 2～4, one hour 1 time, 5～6 times on the one.

Embodiments of the invention 2: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 1.5 adding substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 85 ℃ of system temperature, coolant is 10 ℃ ℃ a dimethicone, and dripping speed is 30d/min, drips distance at 4cm, collect drop pill and remove the dimethicone on surface, promptly get drop pill.

Embodiments of the invention 3: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 1.5 adding substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 85 ℃ of system temperature, coolant is 20 ℃ a dimethicone, and dripping speed is 30d/min, drips distance at 8cm, collect drop pill and remove the dimethicone on surface, promptly get drop pill.

Embodiments of the invention 4: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 1 adding substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 70 ℃ of system temperature, coolant is 5 ℃ a dimethicone, and dripping speed is 20d/min, drips distance at 2cm, collect drop pill and remove the dimethicone on surface, promptly get drop pill.

Embodiments of the invention 5: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, press extract powder: substrate=1: 3 adding substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing is transferred to the drop pill machine, drip 90 ℃ of system temperature, coolant is 30 ℃ a dimethicone, and dripping speed is 40d/min, drips distance at 12cm, collect drop pill and remove the dimethicone on surface, promptly

Embodiments of the invention 6: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filtering, merge with above-mentioned aqueous solution, is 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, adding ethanol makes and contains alcohol amount and reach 60%, left standstill 24 hours, and filtered, filtrate concentrates at decompression recycling ethanol below 80 ℃, dry, add Mentholum, mix homogeneously is ground into fine powder, sprays into above-mentioned volatile oil again, mixing, airtight 2 hours, press extract powder again: substrate=1: 1.5 adds soybean oil, the mixed-matrix of soybean lecithin, heating and melting, mixing gets soft capsule content; The preparation of glue: with gelatin: glycerol: water=1: 0.7: 1.0, getting gelatin adds an amount of distilled water and makes its imbibition, in addition the water of glycerol and remainder is put and be heated to 70～80 ℃ in the glue pot, mix homogeneously adds expansible gelatin and stirs, and makes it to dissolve into uniform glue, in 60 ℃ of insulations 2～3 hours, leave standstill, remove the come-up foam, filter standby with cloth bag.Soft capsule content and glue are pressed into soft capsule in encapsulating machine, put in the drum drying machine and finalize the design, whole ball, drying promptly gets soft capsule.

Embodiments of the invention 7: Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, Mentholum 2.5g

Get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, and the aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, and merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, mix homogeneously is ground into fine powder, add 10% microcrystalline Cellulose, 7% crospolyvinylpyrrolidone, mixing adds ethanol, the system soft material, granulate drying, 40 mesh sieve granulate, tabletting behind the mixing, other gets Mentholum, adds ethanol and makes dissolving in right amount, sprays into, spray into above-mentioned volatile oil again, mixing airtight 2 hours, promptly gets dispersible tablet.

The thin layer chromatography of Radix Gei japonici is differentiated in embodiment 8 drop pills

Get this product powder 3.0g, add methanol 50ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, adds the ethyl acetate jolting and extracts 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets negative sample (hydropenia Radix Myricae rubrae), makes negative sample solution with method.The Radix Myricae rubrae control medicinal material 2g that fetches water again adds ethyl acetate 50ml, and supersound process 60 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.According to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone (5: 0.5) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to speckle colour developing clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The thin layer chromatography of Radix Gei japonici is differentiated in embodiment 9 dispersible tablets

Get this product powder 2.0g, add methanol 50ml, supersound process 30 minutes filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, adds the ethyl acetate jolting and extracts 2 times, each 20ml, combined ethyl acetate liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.The Radix Myricae rubrae control medicinal material 2g that fetches water again adds ethyl acetate 50ml, and supersound process 60 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.According to thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-acetone (4: 0.7), launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The thin layer chromatography of Radix Gei japonici is differentiated in embodiment 10 pellets

Get this product powder 2.0g, add methanol 30ml, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add water 15ml makes dissolving, adds ethyl acetate 20ml jolting and extracts, and acetic acid ethyl fluid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.The Radix Myricae rubrae control medicinal material 2g that fetches water again adds ethyl acetate 50ml, and supersound process 60 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-acetone (6: 0.3), launch, take out, dry, put under the uviol lamp and inspect; Spray with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing again.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The thin layer chromatography of Radix Ardisiae Crenatae medical material, Bergeninum is differentiated in embodiment 11 dispersible tablets

Get this product powder 2g, add methanol 20ml supersound extraction, extracting solution is concentrated into about 1ml, as need testing solution; Get Radix Ardisiae Crenatae control medicinal material 0.5g, shine medical material solution in pairs with legal system; Other gets the Bergeninum reference substance, adds methanol and makes the reference substance solution that every ml contains 0.5mg; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-ethanol=5: 4: 3 was developing solvent, launched, and took out, dry, spray is with the mixed solution of 1% liquor ferri trichloridi-1% potassium ferricyanide solution (1: 1); In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The thin layer chromatography of Bergeninum is differentiated in embodiment 12 pellets

Get this product powder 2g, add methanol 30ml supersound extraction, extracting solution is concentrated into about 1ml, as need testing solution; Other gets the Bergeninum reference substance, adds methanol and makes the reference substance solution that every ml contains 1mg; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-ethanol=4: 5: 2 was developing solvent, launched, and took out, dry, spray is with the mixed solution of 1% liquor ferri trichloridi-1% potassium ferricyanide solution (1: 2); In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.

The thin layer chromatography of Radix Ardisiae Crenatae medical material, Bergeninum is differentiated in embodiment 13 microcapsules

Get this product powder 1g, add methanol 25ml supersound extraction, extracting solution is concentrated into about 1ml, as need testing solution; Get Radix Ardisiae Crenatae control medicinal material 1g, shine medical material solution in pairs with legal system; Other gets the Bergeninum reference substance, adds methanol and makes the reference substance solution that every ml contains 1mg; According to the thin layer chromatography test, draw each 3 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-ethanol=6: 3: 4 was developing solvent, launched, and took out, dry, spray is with the mixed solution of 1% liquor ferri trichloridi-1% potassium ferricyanide solution (2: 1); In the test sample chromatograph, with reference substance and the corresponding position of control medicinal material chromatograph on, show the speckle of same color.

The thin layer chromatography of Radix Platycodonis is differentiated in embodiment 14 dispersible tablets

Get this product powder 3g, add the mixed solution 30ml of 7% ethanol solution of sulfuric acid-water=1: 3, reflux 3 hours, put coldly, add the chloroform jolting and extract 2 times, each 20ml, merge chloroform liquid, add water 30ml washing, discard water liquid, chloroform liquid anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets the Radix Platycodonis control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 3 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-ether=4: 6, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.

The thin layer chromatography of Radix Platycodonis is differentiated in embodiment 15 drop pills

Get this product powder 2g, add the mixed solution 25ml of 10% ethanol solution of sulfuric acid-water=1: 4, reflux 2 hours, put coldly, add the chloroform jolting and extract 2 times, each 20ml, merge chloroform liquid, add water 30ml washing, discard water liquid, chloroform liquid anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets the Radix Platycodonis control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 3 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-ether=5: 5, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color.

The high performance liquid chromatography assay of Bergeninum in embodiment 16 drop pills

Get this product, porphyrize is got about 0.2g, accurate claims surely, puts in the tool plug conical flask, and the accurate methanol 25ml that adds claims decide weight, and supersound process 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes the solution that every 1ml contains 0.05mg, in contrast product solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, be mobile phase with methanol-water=18: 82; The detection wavelength is 275nm; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; Calculate with one point external standard method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 3.0mg every day;

The high performance liquid chromatography assay of Bergeninum in embodiment 17 dispersible tablets

Get this product powder 0.5g, accurate claim surely, put in the tool plug conical flask, the accurate methanol 30ml that adds claims decide weight, and supersound process 15 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes the solution that every 1ml contains 0.1mg, in contrast product solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, be mobile phase with methanol-water=15: 85; The detection wavelength is 270nm; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; Calculate with one point external standard method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 2.0mg every day;

The high performance liquid chromatography assay of Bergeninum in embodiment 18 microcapsules

Get this product powder 0.5g, accurate claim surely, put in the tool plug conical flask, the accurate methanol 30ml that adds claims decide weight, and supersound process 15 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes the solution that every 1ml contains 0.1mg, in contrast product solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, be mobile phase with methanol-water=21: 79; The detection wavelength is 280nm; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; Calculate with one point external standard method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 2.0mg every day;

The gas chromatography assay of Mentholum in embodiment 19 pellets

It is an amount of to get this product, and porphyrize is got 1g, and accurate the title decides, put in the tool plug conical flask, the accurate dehydrated alcohol 20ml that adds claims to decide weight, ice-bath ultrasonic was handled 30 minutes, was placed to room temperature, claimed to decide weight again, supply the weight that subtracts mistake with dehydrated alcohol, shake up, centrifugal, precision is measured supernatant 5ml, puts in the 10ml measuring bottle, the accurate inner mark solution 2ml that adds, add dehydrated alcohol to scale, shake up, as need testing solution; Get naphthalene 150mg, the accurate title, decide, and puts in the 100ml measuring bottle, adds anhydrous alcohol solution and be diluted to scale, as inner mark solution; Other gets Mentholum reference substance 10mg, and accurate the title decides, and puts in the 10ml measuring bottle, and the accurate inner mark solution 2ml that adds adds dehydrated alcohol to scale, shakes up, in contrast product solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 10%; With Chromosorb W (AW-DMCS) (60-80 order) is carrier, and column temperature is 140 ℃; Draw reference substance solution 1 μ l, inject gas chromatograph calculates than positive divisor; Draw need testing solution 1 μ l, inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 20mg every day.

The gas chromatography assay of Mentholum in embodiment 20 dispersible tablets

It is an amount of to get this product, and porphyrize is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate dehydrated alcohol 25ml that adds claims to decide weight, ice-bath ultrasonic was handled 30 minutes, was placed to room temperature, claimed to decide weight again, supply the weight that subtracts mistake with dehydrated alcohol, shake up, centrifugal, precision is measured supernatant 5ml, puts in the 10ml measuring bottle, the accurate inner mark solution 2ml that adds, add dehydrated alcohol to scale, shake up, as need testing solution; Get naphthalene 100mg, the accurate title, decide, and puts in the 100ml measuring bottle, adds anhydrous alcohol solution and be diluted to scale, as inner mark solution; Other gets Mentholum reference substance 10mg, and accurate the title decides, and puts in the 10ml measuring bottle, and the accurate inner mark solution 2ml that adds adds dehydrated alcohol to scale, shakes up, in contrast product solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 8%; With Chromosorb W (AW-DMCS) (60-80 order) is carrier, and column temperature is 110 ℃; Draw reference substance solution 1 μ l, inject gas chromatograph calculates than positive divisor; Draw need testing solution 1 μ l, inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 10mg every day.

The gas chromatography assay of Mentholum in embodiment 21 pellets

It is an amount of to get this product, and porphyrize is got 0.5g, and accurate the title decides, put in the tool plug conical flask, the accurate dehydrated alcohol 25ml that adds claims to decide weight, ice-bath ultrasonic was handled 30 minutes, was placed to room temperature, claimed to decide weight again, supply the weight that subtracts mistake with dehydrated alcohol, shake up, centrifugal, precision is measured supernatant 5ml, puts in the 10ml measuring bottle, the accurate inner mark solution 2ml that adds, add dehydrated alcohol to scale, shake up, as need testing solution; Get naphthalene 100mg, the accurate title, decide, and puts in the 100ml measuring bottle, adds anhydrous alcohol solution and be diluted to scale, as inner mark solution; Other gets Mentholum reference substance 10mg, and accurate the title decides, and puts in the 10ml measuring bottle, and the accurate inner mark solution 2ml that adds adds dehydrated alcohol to scale, shakes up, in contrast product solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 12%; With Chromosorb W (AW-DMCS) (60-80 order) is carrier, and column temperature is 150 ℃; Draw reference substance solution 1 μ l, inject gas chromatograph calculates than positive divisor; Draw need testing solution 1 μ l, inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 20mg every day.

The thin layer chromatography of Herba Menthae medical material, Mentholum is differentiated in embodiment 22 microcapsules

Get this product powder 2g, add petroleum ether (30～60 ℃) 10ml jolting and extract, filter, filtrate is as need testing solution; Other gets Herba Menthae medical material 0.5g, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether (30～60 ℃) and make the reference substance solution that every ml contains 2mg; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=9: 2: 1 was developing solvent, launched, and took out, dry, spray is with 1% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

The thin layer chromatography of Herba Menthae medical material, Mentholum is differentiated in embodiment 23 pellets

Get this product powder 2g, add petroleum ether (60～90 ℃) 10ml jolting and extracted 10 minutes, centrifugal, supernatant is as need testing solution; Other gets Herba Menthae medical material 0.5g, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether (60～90 ℃) and make the reference substance solution that every ml contains 2mg; According to the thin layer chromatography test, draw each 3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=8: 1.5: 1.2 was developing solvent, launched, and took out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

The thin layer chromatography of Herba Menthae medical material, Mentholum is differentiated in embodiment 24 pellets

Get this product powder 2g, add petroleum ether (60～90 ℃) 10ml jolting and extracted 10 minutes, centrifugal, supernatant concentration is as need testing solution; Other gets Herba Menthae medical material 1g, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether (60～90 ℃) and make the reference substance solution that every ml contains 4mg; According to the thin layer chromatography test, draw each 5 μ 1 of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=10: 2.5: 0.8 was developing solvent, launched, and took out, dry, spray is with 2% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

Claims (11)

1, a kind of clear preparation of throat for the treatment of laryngopharyngeal diseases, it is characterized in that: calculate according to weight, it mainly is by Herba Peristrophes 105.5g, Radix Ardisiae Crenatae 63g, Radix Gei japonici 79g, root of Herba Gonostegiae hirtae 79g, Radix Tinosporae 31.5g, Radix Platycodonis 63g, Herba Menthae 79g, the preparation that Mentholum 2.5g is made, comprise: injection comprises: injection, the powder pin, freeze-dried powder, gel, tablet, dispersible tablet, capsule, soft capsule, microcapsule, granule, pill, micropill, powder, drop pill, slow releasing preparation, controlled release preparation, gel, oral liquid, soft extract, all acceptable dosage forms on the pharmaceutics such as extractum and membrane.

2, according to the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 1, it is characterized in that: described preparation is drop pill, soft capsule, dispersible tablet.

3, method for making according to the clear preparation of throat of claim 1 or 2 described treatment laryngopharyngeal diseasess, it is characterized in that: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, merging with above-mentioned aqueous solution, is 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, adds ethanol and makes and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, spray into above-mentioned volatile oil, make different preparations.

4, preparation method according to the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 3, it is characterized in that: the drop pill in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filtering, merge with above-mentioned aqueous solution, is 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, adding ethanol makes and contains alcohol amount and reach 60%, left standstill 24 hours, and filtered, filtrate concentrates at decompression recycling ethanol below 80 ℃, dry, add Mentholum, mix homogeneously is ground into fine powder, presses extract powder: substrate=1: 1～3 add substrate PEG4000, spray into above-mentioned volatile oil behind the heating and melting, mixing, transfer to the drop pill machine, drip 70 ℃～90 ℃ of system temperature, coolant is 5 ℃～30 ℃ a dimethicone, dripping speed is 20～40d/min, drip apart from 2～12cm, collect drop pill and remove the dimethicone on surface, promptly.

5, preparation method according to the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 4, it is characterized in that: the drop pill in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filtering, merge with above-mentioned aqueous solution, is 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, adding ethanol makes and contains alcohol amount and reach 60%, left standstill 24 hours, and filtered, filtrate concentrates at decompression recycling ethanol below 80 ℃, dry, add Mentholum, mix homogeneously is ground into fine powder, presses extract powder: substrate=add substrate PEG4000 at 1: 1.5 sprays into above-mentioned volatile oil behind the heating and melting, mixing, transfer to the drop pill machine, drip 85 ℃ of system temperature, coolant is 10 ℃～20 ℃ a dimethicone, dripping speed is 30d/min, drip apart from 4～8cm, collect drop pill and remove the dimethicone on surface, promptly.

6, method for making according to the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 3, it is characterized in that: the soft capsule in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, medicinal residues decoct with water 1.5 hours, filter, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, spray into above-mentioned volatile oil again, mixing airtight 2 hours, is pressed extract powder: substrate=1: 1.5 again, add soybean oil, the mixed-matrix of soybean lecithin, heating and melting, mixing gets soft capsule content; The preparation of glue: with gelatin: glycerol: water=1: 0.7: 1.0, getting gelatin adds an amount of distilled water and makes its imbibition, in addition the water of glycerol and remainder is put and be heated to 70～80 ℃ in the glue pot, mix homogeneously adds expansible gelatin and stirs, and makes it to dissolve into uniform glue, in 60 ℃ of insulations 2～3 hours, leave standstill, remove the come-up foam, filter standby with cloth bag.Soft capsule content and glue are pressed into soft capsule in encapsulating machine, put in the drum drying machine and finalize the design, whole ball, drying, promptly.

7, method for making according to the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 3, it is characterized in that: the dispersible tablet in the described preparation prepares like this: get Herba Peristrophes, Radix Ardisiae Crenatae, Radix Gei japonici, root of Herba Gonostegiae hirtae, Radix Tinosporae, Radix Platycodonis, Herba Menthae, vapor distillation extracts volatile oil, aqueous solution after distillation device is in addition collected, and medicinal residues decoct with water 1.5 hours, filters, merge with above-mentioned aqueous solution, be 1.10～1.12 clear paste when being evaporated to 60 ℃ of relative densities, add ethanol and make and contain the alcohol amount and reach 60%, left standstill 24 hours, filter, filtrate concentrates at decompression recycling ethanol below 80 ℃, drying adds Mentholum, and mix homogeneously is ground into fine powder, add 10% microcrystalline Cellulose, 7% crospolyvinylpyrrolidone, mixing adds ethanol, the system soft material, granulate, drying, 40 mesh sieve granulate, tabletting behind the mixing, spray into above-mentioned volatile oil again, mixing, airtight 2 hours, promptly.

8, according to the quality control method of the clear preparation of throat of any described treatment laryngopharyngeal diseases in the claim 1～7, it is characterized in that: discrimination method comprises following all or part of content:

A. the thin layer chromatography of Radix Gei japonici is differentiated in the preparation

It is an amount of to get this product powder, adds methanol extraction, and extracting solution evaporate to dryness, residue add water makes dissolving, adds the ethyl acetate jolting and extracts, and acetic acid ethyl fluid evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other the Radix Myricae rubrae control medicinal material of fetching water is an amount of, adds ethyl acetate extraction, and extracting solution evaporate to dryness, residue add methanol makes dissolving, in contrast medical material solution; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution respectively, puts on same silica gel g thin-layer plate, and with chloroform-acetone=4～6: 0.3～0.7 is developing solvent, launch, take out, dry, put under the uviol lamp and inspect, or spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

B. one or both thin layer chromatography discriminating in Radix Ardisiae Crenatae medical material, the Bergeninum in the preparation

It is an amount of to get this product powder, adds the methanol supersound extraction, and extracting solution concentrates, as need testing solution; Get the Radix Ardisiae Crenatae control medicinal material, shine medical material solution in pairs with legal system; Other gets the Bergeninum reference substance, adds methanol and makes reference substance solution; According to the thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution respectively, puts on same silica gel g thin-layer plate, with chloroform-ethyl acetate-ethanol=4～6: be developing solvent at 3～5: 2～4, launches, and takes out, dry, spray is to contain the developer that mixes of ferric chloride and the potassium ferricyanide; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

C. the thin layer chromatography of Radix Platycodonis is differentiated in the preparation

It is an amount of to get this product powder, adds the mixed solution of ethanol solution of sulfuric acid and water, and reflux is put cold, add the chloroform jolting and extract, chloroform liquid adds water washing, discards water liquid, chloroform liquid anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other gets the Radix Platycodonis control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate, and with chloroform-ether=4～5: 5～6 be developing solvent, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;

D. the thin layer chromatography of Herba Menthae medical material, Mentholum is differentiated in the preparation

It is an amount of to get this product powder, adds the petroleum ether jolting and extracts, and extracting solution is as need testing solution; Other gets the Herba Menthae medical material, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether and make reference substance solution; Test according to thin layer chromatography, it is an amount of to draw above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=8～10: be developing solvent at 1.5～2.5: 0.8～1.2, launch, take out, dry, spray is with the vanillin sulfuric acid solution, and it is clear to be heated to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

9, according to the quality control method of the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 8, it is characterized in that: discrimination method comprises following all or part of content:

A. the thin layer chromatography of Radix Gei japonici is differentiated in the preparation

It is an amount of to get this product powder, adds the methanol supersound extraction, and extracting solution evaporate to dryness, residue add water makes dissolving, adds the ethyl acetate jolting and extracts, and acetic acid ethyl fluid evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other the Radix Myricae rubrae control medicinal material of fetching water is an amount of, adds the ethyl acetate supersound extraction, and extracting solution evaporate to dryness, residue add methanol makes dissolving, in contrast medical material solution; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution respectively, put on same silica gel g thin-layer plate, be developing solvent with chloroform-acetone=5: 0.5, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;

B. one or both thin layer chromatography discriminating in Radix Ardisiae Crenatae medical material, the Bergeninum in the preparation

It is an amount of to get this product powder, adds the methanol supersound extraction, and extracting solution concentrates, as need testing solution; Get the Radix Ardisiae Crenatae control medicinal material, shine medical material solution in pairs with legal system; Other gets the Bergeninum reference substance, adds methanol and makes reference substance solution; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, and be developing solvent with chloroform-ethyl acetate-ethanol=5: 4: 3, launch, take out, dry, spray to contain the developer that mixes of ferric chloride and the potassium ferricyanide; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

C. the thin layer chromatography of Radix Platycodonis is differentiated in the preparation

It is an amount of to get this product powder, add the mixed solution of 7% ethanol solution of sulfuric acid-water=1: 3, reflux is put cold, adding the chloroform jolting extracts, chloroform liquid adds water washing, discards water liquid, chloroform liquid anhydrous sodium sulfate dehydration, filter, filtrate evaporate to dryness, residue add methanol makes dissolving, as need testing solution; Other gets the Radix Platycodonis control medicinal material, shines medical material solution in pairs with legal system; According to thin layer chromatography test, it is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-ether=4: 6, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the principal spot of same color;

D. the thin layer chromatography of Herba Menthae medical material, Mentholum is differentiated in the preparation

It is an amount of to get this product powder, adds the petroleum ether jolting and extracts, and extracting solution is as need testing solution; Other gets the Herba Menthae medical material, shines medical material solution in pairs with legal system; Get the Mentholum reference substance, add petroleum ether and make reference substance solution; According to the thin layer chromatography test, it is an amount of to draw above-mentioned three kinds of solution, puts respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate-chloroform=9: 2: 1 was developing solvent, launched, and took out, dry, spray is with the vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with contrast chromatograph corresponding position on, show the speckle of same color.

10, according to the quality control method of the clear preparation of throat of any described treatment laryngopharyngeal diseases in the claim 1～7, it is characterized in that: content assaying method comprises following all or part of content:

A. the high performance liquid chromatography assay of Bergeninum in the preparation

It is an amount of to get this product powder, accurate claims surely, puts in the tool plug conical flask, and the accurate methanol that adds claims decide weight, and supersound process is put coldly, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes reference substance solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, with methanol-water=15～21: 85～79 is mobile phase; The detection wavelength is 270～280nm; Accurate respectively absorption reference substance solution and need testing solution are an amount of, inject chromatograph of liquid, measure; Calculate with one point external standard method or standard curve method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 1.5mg every day;

B. the gas chromatography assay of Mentholum in the preparation

It is an amount of to get this product powder, and accurate the title decides, and puts in the tool plug conical flask, the accurate dehydrated alcohol that adds, supersound process is placed to room temperature, claim again to decide weight, supply the weight that subtracts mistake, shake up with dehydrated alcohol, centrifugal, it is an amount of that precision is measured supernatant, and the accurate again inner mark solution that adds is an amount of, adds dehydrated alcohol and is settled to debita spissitudo, shake up, as need testing solution; It is an amount of that naphthalene decided in accurate title, adds anhydrous alcohol solution and make inner mark solution; Other gets the Mentholum reference substance, and accurate the title decides, and the accurate inner mark solution that adds is an amount of, adds dehydrated alcohol and makes reference substance solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 8～12%; Column temperature is 110～150 ℃; Draw an amount of inject gas chromatograph of reference substance solution, calculate than positive divisor; The absorption need testing solution is an amount of, and inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 15mg every day.

11, according to the quality control method of the clear preparation of throat of the described treatment laryngopharyngeal diseases of claim 10, it is characterized in that: content assaying method comprises following all or part of content:

A. the high performance liquid chromatography assay of Bergeninum in the preparation

Get this product, porphyrize is got about 0.2g, accurate claims surely, puts in the tool plug conical flask, and the accurate methanol 25ml that adds claims decide weight, and supersound process 1 hour is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with methanol, shakes up, and filtration is got subsequent filtrate, as need testing solution; Accurate title Bergeninum reference substance is an amount of, adds methanol and makes the solution that every 1ml contains 0.05mg, in contrast product solution; According to high performance liquid chromatography test, be filler with 18 silylation bonded silica gels, be mobile phase with methanol-water=18: 82; The detection wavelength is 275nm; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure; Calculate with one point external standard method, this product contains the Rhizoma Seu Herba Bergeniae element with dosage and must not be less than 3.0mg every day;

B. the gas chromatography assay of Mentholum in the preparation

It is an amount of to get this product, and porphyrize is got 1g, and accurate the title decides, put in the tool plug conical flask, the accurate dehydrated alcohol 20ml that adds claims to decide weight, ice-bath ultrasonic was handled 30 minutes, was placed to room temperature, claimed to decide weight again, supply the weight that subtracts mistake with dehydrated alcohol, shake up, centrifugal, precision is measured supernatant 5ml, puts in the 10ml measuring bottle, the accurate inner mark solution 2ml that adds, add dehydrated alcohol to scale, shake up, as need testing solution; Get naphthalene 150mg, the accurate title, decide, and puts in the 100ml measuring bottle, adds anhydrous alcohol solution and be diluted to scale, as inner mark solution; Other gets Mentholum reference substance 10mg, and accurate the title decides, and puts in the 10ml measuring bottle, and the accurate inner mark solution 2ml that adds adds dehydrated alcohol to scale, shakes up, in contrast product solution; According to the gas chromatography test, be immobile phase with Polyethylene Glycol-20M, coating concentration is 10%; With Chromosorb W (AW-DMCS) (60-80 order) is carrier, and column temperature is 140 ℃; Draw reference substance solution 1 μ l, inject gas chromatograph calculates than positive divisor; Draw need testing solution 1 μ l, inject gas chromatograph is measured; This product contains Mentholum with dosage and must not be less than 20mg every day.