CN1762465A - Rhinitis gel, its preparation method and quality control technology - Google Patents

Abstract

The invention discloses a gel for treating rhinitis, which is prepared from dahurian angelica root, siberian cocklebur fruit, asaryl, grassleaved sweetflag rhizome, flower bud of lily magnolia, Chinese ephedra extract and auxiliary materials including Carbomer, propylene glycol and polysorbate 80.

Description

Rhinitis gel and preparation method thereof, Quality Control Technology

Technical field

The invention belongs to a kind of Chinese medicine gel preparation, specifically is a kind of gel preparation that is used for the treatment of rhinitis.

Background technology

Chronic simple rhinitis is a kind of with mucosa swelling, and secretions increase is the chronic inflammatory disease of characteristics.Clinical treatment chronic simple rhinitis key is to eliminate paathogenic factor, but eliminates as early as possible or to alleviate the nasal mucosa congestive symptom very important.

Existing Chinese traditional patent formulation preparation DITONG BIYAN SHUI, develop through modern crafts by Chinese medicines such as Herba Taraxaci, Herba Asari, Radix Scutellariae, Herba Ephedrae, Rhizoma Acori Graminei, the Radixs Angelicae Dahuricae, have expelling wind and clearing away heat, the sensible effect of lung qi dispersing, be used for the treatment of the cold nasal obstruction clinically, chronic rhinitis, allergic rhinitis are for many years.Because safe, no obvious toxic-side effects is subjected to rhinitis patient's welcome.

But there is poor stability in DITONG BIYAN SHUI, and the medicine effective component content is on the low side; During nose dropping treatment, because drug wastage, nasal membrane absorbs few, has influenced its therapeutic effect.

Summary of the invention

The present invention carries out dosage changing form research to DITONG BIYAN SHUI, the development rhinitis gel, by improving the extracting mode of raw material Chinese medicine, improved the content of active ingredient in the medicine, and gel helps the absorption of nasal cavity inner membrance owing to be coated on the mucosa of nasal cavity, improve the curative effect of medicine, also reduced amount of drug.

Technical scheme of the present invention is as follows:

1, rhinitis gel is characterized in that in 100-200 milliliter gel, the weight proportion of each raw material components is in following ratio preparation:

Herba Taraxaci 12-24g Herba Asari 0.5-1.0g Radix Scutellariae 6.0-12g

Herba Ephedrae 5.0-10g Fructus Xanthii 5.0-10g Rhizoma Acori Graminei 6.0-12g

Radix Angelicae Dahuricae 2.5-5.0g Flos Magnoliae 2.5-5.0g

Disodiumedetate 0.03-0.06g carbomer 0.5-1.0g

Propylene glycol 4.0-8.0g ethyl hydroxybenzoate 0.1-0.2g, polyoxyethylene sorbitan monoleate 1.0-2.0g

Transfer pH value to 6～7 with triethanolamine

All the other are water.

2, rhinitis gel is characterized in that the weight proportion of each raw material components is in 100 milliliters of gels:

Herba Taraxaci 12-24g Herba Asari 0.5-1.0g Radix Scutellariae 6.0-12g

Herba Ephedrae 5.0-10g Fructus Xanthii 5.0-10g Rhizoma Acori Graminei 6.0-12g

Radix Angelicae Dahuricae 2.5-5.0g Flos Magnoliae 2.5-5.0g

Disodiumedetate 0.03-0,06g carbomer 0.5-1.0g

Propylene glycol 4.0-8.0g ethyl hydroxybenzoate 0.1-0.2g, polyoxyethylene sorbitan monoleate 1.0-2.0g

Transfer pH value to 6～7 with triethanolamine

All the other are water.

3, rhinitis gel is characterized in that the weight proportion of each raw material components is in 200 milliliters of gels:

Herba Taraxaci 12-24g Herba Asari 0.5-1.0g Radix Scutellariae 6.0-12g

Herba Ephedrae 5.0-10g Fructus Xanthii 5.0-10g Rhizoma Acori Graminei 6.0-12g

Radix Angelicae Dahuricae 2.5-5.0g Flos Magnoliae 2.5-5.0g

Disodiumedetate 0.03-0.06g carbomer 0.5-1.0g

Propylene glycol 4.0-8.0g ethyl hydroxybenzoate 0.1-0.2g, polyoxyethylene sorbitan monoleate 1.0-2.0g

Transfer pH value to 6～7 with triethanolamine

All the other are water.

Above 1,2,3 described rhinitis gels, it is characterized in that weight (g of the unit) proportioning of described each raw material components is:

Herba Taraxaci 12 Herba Asaris 0.5 Radix Scutellariae 6.0

Herba Ephedrae 5 Fructus Xanthii 5.0 Rhizoma Acori Graminei 6.0

The Radix Angelicae Dahuricae 2.5 Flos Magnoliaes 2.5

Disodiumedetate 0.03 carbomer 0.5

Propylene glycol 4.0 ethyl hydroxybenzoates 0.1, polyoxyethylene sorbitan monoleate 1.0

Transfer pH value to 6～7 with triethanolamine

All the other are water.

Above 1,2,3 described rhinitis gels, it is characterized in that weight (g of the unit) proportioning of described each raw material components is:

Herba Taraxaci 24.0 Herba Asaris 1.0 Radix Scutellariaes 12.0

Herba Ephedrae 10.0 Fructus Xanthii 10.0 Rhizoma Acori Graminei 12

The Radix Angelicae Dahuricae 5.0 Flos Magnoliaes 5.0

Disodiumedetate 0.06 carbomer 1.0

Propylene glycol 8.0 ethyl hydroxybenzoates 0.2, polyoxyethylene sorbitan monoleate 2.0

Transfer pH value to 6～7 with triethanolamine

All the other are water.

The preparation method of described rhinitis gel, it is characterized in that may further comprise the steps: take by weighing the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae by prescription, use vapor distillation, it is standby to collect distillate, and medicinal residues and Herba Taraxaci, Radix Scutellariae decoct with water, decocting liquid filters, filtrate is concentrated into the thick paste shape, adds ethanol and stirs evenly, and leaves standstill, get supernatant and reclaim ethanol and be concentrated into nothing alcohol flavor, standby; After other gets disodiumedetate and adds suitable quantity of water and make dissolving, add carbomer, leave standstill and stir evenly, carbomer gel; Get propylene glycol, add ethyl hydroxybenzoate, polyoxyethylene sorbitan monoleate, above-mentioned distillate and medicinal liquid, be added to behind the mixing in the carbomer gel, stir evenly, transfer pH value to 6～7, add the gel that water is made set amount, promptly with triethanolamine.

The preparation method of described rhinitis gel, it is characterized in that may further comprise the steps: get the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae and add 10 times of water gagings distillations 3 hours, wherein volatile oil content is stable to measuring to collect distillate, medicinal liquid filters, standby, medicinal residues add Herba Taraxaci and Radix Scutellariae, add 10 times of water gagings and decoct secondary, each 1.5 hours, collecting decoction filters, and filtrate is concentrated into the thick paste that relative density is 1.15～1.20 (50 ℃), add 4 times of amounts of ethanol, stir evenly, standing over night is got supernatant and is reclaimed ethanol, being concentrated into does not have the alcohol flavor, standby; After other gets disodiumedetate and adds suitable quantity of water and make dissolving, add carbomer approximately, left standstill 12～24 hours, stir evenly, carbomer gel; Get propylene glycol, add ethyl hydroxybenzoate, polyoxyethylene sorbitan monoleate, above-mentioned distillate and medicinal liquid, be added to behind the mixing in the carbomer gel, stir evenly, transfer pH value to 6～7, add the gel that water is made set amount, promptly with triethanolamine.

The Herba Taraxaci main component is taraxol, taraxerol, α-taraxasterol, taraxasterol, cupreol etc.; The Herba Asari main component is that volatile oil has methyleugenol, saishinone, asarinin, kakuol, australene, camphene, nopinene, myrcene etc.; The Radix Scutellariae main component is baicalin, chrysin, stigmasterol, sitosterol etc.; The Herba Ephedrae main component is an ephedrine, pseudoephedrine, ephedine etc.; The Fructus Xanthii main component is cupreol, xanthostrumarin, resin, alkaloid etc.; The Rhizoma Acori Graminei main component is volatile ingredient beta-Asarone, asaricin, caryophyllene, asarylaldehyde etc.; Radix Angelicae Dahuricae main component is byak-angelicin, Byakangelicol, oxypeucedanin, Petroselinum second element, auraptin etc.; The Flos Magnoliae main component is australene, camphene, nopinene, limonene etc.

The present invention is according to the physicochemical property of each flavour of a drug main component, and cures mainly in conjunction with its function, and the extraction process parameter of its effective components of Chinese medicinal is optimized.

1, the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae Six-element Chinese medicine distillation time determines

Take by weighing Six-element 430g such as the Radix Angelicae Dahuricae in the prescription ratio, add the water distillation, every certain interval of time is collected distillate and is measured the volatilization oil mass, carries oil after 3 hours, and oil mass tends towards stability substantially, so determine that distillation time is 3 hours.Promptly when collecting distillate, adjusted a speed (about 5ml/min kg) in 3 hours by distillation.

2, the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae Six-element Chinese medicine amount of water determines

Take by weighing Six-element 215g such as the Radix Angelicae Dahuricae in proportion, 3g adds 10 times of water gagings altogether, distilled 3 hours, and collected the about 200ml of distillate, medicinal liquid filters, medicinal residues respectively add Herba Taraxaci 120g, Radix Scutellariae 60g, add 8,10,12 times of water gagings respectively and decoct secondary, each 1.5 hours, collecting decoction, filter, filtrate is concentrated into the thick paste shape, measures ephedrine hydrochloride content, the results are shown in following table.

Different amount of water are to the influence of ephedrine hydrochloride content

Amount of water (doubly)	Ephedrine hydrochloride amount (g)		x
				1	2
	8 10 12	0.50 0.57 0.54				0.49 0.56 0.58	0.50 0.56 0.56

As seen from the above table, the ephedrine hydrochloride amount carried of 10 times of amounts and 12 times of water gagings is suitable, all high than 8 times of amounts.In order to shorten extracting cycle, reduce the medicine heated time, so determine that amount of water is that 10 times of amounts are advisable.

3, the preceding relative density of precipitate with ethanol determines

Take by weighing Six-element 860g such as the Radix Angelicae Dahuricae by prescription, add 10 times of water gaging distillations 3 hours, collect the about 800ml of distillate, medicinal liquid filters, medicinal residues add Herba Taraxaci 480g, Radix Scutellariae 240g, add 10 times of water gagings and decoct secondary, each 1.5 hours, collecting decoction, decocting liquid one is divided into four, and being concentrated into relative density respectively is 1.10,1.15,1.20,1.25 (50 ℃), and each adds 4 times of amount ethanol, stir evenly standing over night.Get supernatant and reclaim ethanol, be concentrated into the extractum that does not have the alcohol flavor, measure its ephedrine hydrochloride content respectively, measurement result shows that relative density is that 1.15～1.20 (50 ℃) are comparatively suitable before the selection precipitate with ethanol.When relative density is big, may produce the parcel phenomenon, effective ingredient is lost.

Getting the rhinitis gel extraction process according to above result of study is: get the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae and add 10 times of water gagings distillations 3 hours, collect the about 200ml of distillate, medicinal liquid filters, standby, medicinal residues add Herba Taraxaci and Radix Scutellariae, add 10 times of water gagings and decoct secondary, each 1.5 hours, collecting decoction, filter, filtrate is concentrated into the thick paste that relative density is 1.15～1.20 (50 ℃), adds 4 times of amounts of ethanol, stirs evenly, standing over night, get supernatant and reclaim ethanol, being concentrated into does not have the alcohol flavor, promptly.

The preparations shaping Journal of Sex Research

1, prescription design considerations

Select carbomer as gelatinizing agent, carbomer is the water-soluable gel material of using always, the moderate and low price of its viscosity.Adopt a certain amount of carbomer as gel-type vehicle, release is fast, and no greasy easily is coated with exhibition, and to skin and mucosa nonirritant, energy and aqueous solution, and energy absorptive tissue dissolution fluid help the eliminating of secretions.Owing to contain more oil droplet in this product Aromatic water, for making preparation even, so in preparation, add a certain amount of solubilizing agent or dispersant, find through experiment, adding an amount of propylene glycol and polyoxyethylene sorbitan monoleate can make oil droplet be uniformly dispersed, get the preparation of clear, and mix and use independent result of use more obvious.

Ethyl hydroxybenzoate can suppress gel effectively and grow mycete as antibacterial; Disodiumedetate (EDTA-2Na) has complexing as stabilizing agent to metal ion, can effectively avoid the viscosity reduction phenomenon of gel.

Under the situation that medicament composing prescription is determined, it is 0.1% that the antibacterial in the preparation and the consumption of stabilizing agent are decided to be ethyl hydroxybenzoate routinely; EDTA-2Na is 0.03%;

The optimum amount of propylene glycol, polyoxyethylene sorbitan monoleate, carbomer on the basis of trial test by orthonormal design of experiments, by its optimum amount is: propylene glycol 4%, polyoxyethylene sorbitan monoleate 1%, carbomer 0.5%.

Carbomer is rich in carboxyl, is acid after water-soluble, in order to reduce the stimulation to nasal mucosa, adopts an amount of triethanolamine to regulate between pH to 6～7.

The gel of the present invention's preparation, good stability has no side effect, and the energy holdup time of prolong drug in nasal cavity, to improving bioavailability positive effect is arranged.

The specific embodiment

All can implement by the various prescriptions that the present invention is listed, no longer repeat, only enumerate an example with explanation now at this.

One, prescription

Raw material: Herba Taraxaci 120g Herba Asari 5g Radix Scutellariae 60g

Herba Ephedrae 50g Fructus Xanthii 50g Rhizoma Acori Graminei 60g

Radix Angelicae Dahuricae 25g Flos Magnoliae 25g

Adjuvant: disodiumedetate 0.3g Acritamer 940 5g

Propylene glycol 40g ethyl hydroxybenzoate 1g polyoxyethylene sorbitan monoleate 10g

Transfer pH value to 6～7 with triethanolamine

All the other are water,

More than make 1000 milliliters.

Two, method for making

Get the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae and add 10 times of water gagings distillations 3 hours, collect the about 200ml of distillate, the medicinal liquid filtration, standby, medicinal residues add Herba Taraxaci and Radix Scutellariae, add 10 times of water gagings and decoct secondary, each 1.5 hours, collecting decoction filtered, filtrate is concentrated into the thick paste that relative density is 1.15～1.20 (50 ℃), adds 4 times of amounts of ethanol, stirs evenly, standing over night, get supernatant and reclaim ethanol, being concentrated into does not have the alcohol flavor, standby; After other gets disodiumedetate and adds suitable quantity of water and make dissolving, add the about 5g of carbomer, left standstill 12～24 hours, stir evenly, must carbomer gel; Get propylene glycol 40g, add ethyl hydroxybenzoate 1g, polyoxyethylene sorbitan monoleate 10g, above-mentioned distillate and medicinal liquid, be added to behind the mixing in the carbomer gel, stir evenly, transfer pH value to 6～7, add water and make 1000ml with triethanolamine, packing, promptly.

Three, preparation stabilization Journal of Sex Research

Rhinitis gel is placed 39 ℃ ± 1 ℃ respectively, and in 25 ± 3 ℃ of super utmost point temperature chambers and 5 ± 2 ℃ of refrigerators 30 days, the temperature of simulation different regions was observed its denseness, color and luster, pH value, is had or not phenomenon such as go mouldy.Result of the test as can be known, this product is under above-mentioned experimental condition, its denseness, color and luster, pH value have no significant change, and do not have mildew phenomena.

The external release comparative study of rhinitis gel and DITONG BIYAN SHUI

According to the accumulated time permeability result and the transdermal penetration curvilinear trend of rhinitis gel and DITONG BIYAN SHUI, by analysis as can be known, the T of rhinitis gel ₅₀=4.42h, T _d=8.00h, the T of DITONG BIYAN SHUI ₅₀=6.97h, T _d=9.38h, and both accumulative total release rate no significant differences.DITONG BIYAN SHUI transformation of the way rhinitis gel, its advantage is the energy holdup time of prolong drug in nasal cavity, to improving bioavailability positive effect is arranged.

Four, the Quality Control Technology of rhinitis gel is to carry out following mensuration and discriminating:

[character]:

This product rhinitis gel is brown stiff shape liquid; Gas fragrance, mildly bitter flavor;

[discriminating]:

(1), get this product 20g, add water 10ml and shake up, regulate PH1～2 with dilute hydrochloric acid, with ether extraction 3 times, each 30ml, water liquid is standby, merges ether solution, water bath method, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Herba Taraxaci control medicinal material 2g, adds water 100ml heated and boiled 1 hour, filters with absorbent cotton, and filtrate is concentrated into 30ml, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 10 μ l, control medicinal material solution 8 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with toluene-ethyl acetate-formic acid (9: 4: 1) is developing solvent, take out, put to place in the air and spend the night, put under the ultra-violet lamp (365nm) and inspect; For looking in the product chromatograph, with the corresponding position of control medicinal material chromatograph on, the fluorescence speckle of apparent same color;

(2), get discriminating (1) water liquid down, add 5% sodium hydroxide solution and regulate more than the PH10, with ether extraction 3 times, 30ml at every turn, low temperature is flung to ether, regulates PH1～2 with dilute hydrochloric acid, water bath method, residue add methanol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methanol and makes the solution that every ml contains 2mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 3 μ l, reference substance solution 8 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-methanol-strong aqua ammonia (20: 5: 0.5) is developing solvent, launches below 25 ℃, takes out, dry, 50 ℃ of bakings 40 minutes, spray be with ninhydrin solution, and it is clear to be heated to speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(3), get this product 20g, add water 10ml, shake up, with ethyl acetate extraction 3 times, each 30ml discards acetic acid ethyl fluid, water saturation n-butanol extraction 3 times of water liquid, each 30ml merges n-butyl alcohol liquid, add water washing 2 times, each 40ml discards water lotion, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, add methanol and make the solution that every ml contains 1mg, product solution according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, is drawn need testing solution 4 μ l, reference substance solution 8 μ l in contrast, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose that contains 4% sodium acetate, (5: 3: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4), get this product 30g, put in the round-bottomed flask, add water 200ml, connect volatile oil extractor, add ethyl acetate 2ml, reflux 2 hours is divided and is got acetic acid ethyl fluid, as need testing solution; Other gets Rhizoma Acori Graminei control medicinal material 1g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively in same be on the silica GF254 lamellae of binding agent with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (8: 2) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

[inspection]:

Aristolochic Acid is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D);

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water-acetic acid (65: 35: 1) is mobile phase, and the detection wavelength is 390nm, and number of theoretical plate calculates by the aristolochic acid A peak should be not less than 2000;

It is an amount of that the preparation precision of reference substance solution takes by weighing the aristolochic acid A reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;

The accurate about 10ml of this product that draws of the preparation of need testing solution adds water to 40ml, about the HCl accent pH value to 2.0 with 6mol/L, 3 (50ml of reuse ether extraction, 40ml 40ml), merges ether solution, water-bath volatilizes, residue adds dissolve with methanol and standardize solution in the 2ml measuring bottle, shakes up, and filters through microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

This product should detect aristolochic acid A (C ₁₇H ₁₁NO ₇);

Other should meet the pertinent regulations (two appendix IU of Chinese Pharmacopoeia version in 2000) under the gel item;

[assay] Herba Ephedrae is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D);

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and acetonitrile-0.1% phosphoric acid solution (6: 94) is a mobile phase, and the detection wavelength is 207nm; Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 3000;

It is an amount of that the ephedrine hydrochloride reference substance that is dried to constant weight is got in the preparation of reference substance solution, and accurate the title decides, and 50% methanol that adds 0.5% hydrochloric acid is made the solution that every 1ml contains 50 μ g, shakes up, promptly;

The accurate this product 2.0ml that draws of the preparation of need testing solution puts in the 25ml measuring bottle, and 50% methanol solution that adds 0.5% hydrochloric acid is to nearly scale, supersound process 20min, 50% methanol solution that adds 0.5% hydrochloric acid is diluted to scale, shakes up, microporous filter membrane (0.45 μ m) filters, promptly;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

The every ml of this product contains Herba Ephedrae with ephedrine hydrochloride (C ₁₀H ₁₅NO.HCl) meter must not be less than 0.15mg.

Claims (8)

1, rhinitis gel is characterized in that in 100-200 milliliter gel, the weight proportion of each raw material components is in following ratio preparation:

Herba Taraxaci 12-24g Herba Asari 0.5-1.0g Radix Scutellariae 6.0-12g

Herba Ephedrae 5.0-10g Fructus Xanthii 5.0-10g Rhizoma Acori Graminei 6.0-12g

Radix Angelicae Dahuricae 2.5-5.0g Flos Magnoliae 2.5-5.0g

Disodiumedetate 0.03-0.06g carbomer 0.5-1.0g

Propylene glycol 4.0-8.0g ethyl hydroxybenzoate 0.1-0.2g, polyoxyethylene sorbitan monoleate 1.0-2.0g

Transfer pH value to 6～7 with triethanolamine

All the other are water.

2, rhinitis gel according to claim 1 is characterized in that the weight proportion of each raw material components is in 100 milliliters of gels:

Herba Taraxaci 12-24g Herba Asari 0.5-1.0g Radix Scutellariae 6.0-12g

Herba Ephedrae 5.0-10g Fructus Xanthii 5.0-10g Rhizoma Acori Graminei 6.0-12g

Radix Angelicae Dahuricae 2.5-5.0g Flos Magnoliae 2.5-5.0g

Disodiumedetate 0.03-0.06g carbomer 0.5-1.0g

Propylene glycol 4.0-8.0g ethyl hydroxybenzoate 0.1-0.2g, polyoxyethylene sorbitan monoleate 1.0-2.0g

Transfer pH value to 6～7 with triethanolamine

All the other are water.

3, rhinitis gel according to claim 1 is characterized in that the weight proportion of each raw material components is in 200 milliliters of gels:

Herba Taraxaci 12-24g Herba Asari 0.5-1.0g Radix Scutellariae 6.0-12g

Herba Ephedrae 5.0-10g Fructus Xanthii 5.0-10g Rhizoma Acori Graminei 6.0-12g

Radix Angelicae Dahuricae 2.5-5.0g Flos Magnoliae 2.5-5.0g

Disodiumedetate 0.03-0.06g carbomer 0.5-1.0g

Propylene glycol 4.0-8.0g ethyl hydroxybenzoate 0.1-0.2g, polyoxyethylene sorbitan monoleate 1.0-2.0g

Transfer pH value to 6～7 with triethanolamine

All the other are water.

4,, it is characterized in that the weight proportion of described each raw material components is according to claim 1 or 2 or 3 described rhinitis gels:

Herba Taraxaci 12 Herba Asaris 0.5 Radix Scutellariae 6.0

Herba Ephedrae 5 Fructus Xanthii 5.0 Rhizoma Acori Graminei 6.0

The Radix Angelicae Dahuricae 2.5 Flos Magnoliaes 2.5

Disodiumedetate 0.03 carbomer 0.5

Propylene glycol 4.0 ethyl hydroxybenzoates 0.1, polyoxyethylene sorbitan monoleate 1.0

Transfer pH value to 6～7 with triethanolamine

All the other are water.

5,, it is characterized in that the weight proportion of described each raw material components is according to claim 1 or 2 or 3 described rhinitis gels:

Herba Taraxaci 24.0 Herba Asaris 1.0 Radix Scutellariaes 12.0

Herba Ephedrae 10.0 Fructus Xanthii 10.0 Rhizoma Acori Graminei 12

The Radix Angelicae Dahuricae 5.0 Flos Magnoliaes 5.0

Disodiumedetate 0.06 carbomer 1.0

Propylene glycol 8.0 ethyl hydroxybenzoates 0.2, polyoxyethylene sorbitan monoleate 2.0

Transfer pH value to 6～7 with triethanolamine

All the other are water.

6, the preparation method of rhinitis gel according to claim 1, it is characterized in that may further comprise the steps: take by weighing the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae by prescription, use vapor distillation, it is standby to collect distillate, and medicinal residues and Herba Taraxaci, Radix Scutellariae decoct with water, decocting liquid filters, filtrate is concentrated into the thick paste shape, adds ethanol and stirs evenly, and leaves standstill, get supernatant and reclaim ethanol and be concentrated into nothing alcohol flavor, standby; After other gets disodiumedetate and adds suitable quantity of water and make dissolving, add carbomer, leave standstill and stir evenly, carbomer gel; Get propylene glycol, add ethyl hydroxybenzoate, polyoxyethylene sorbitan monoleate, above-mentioned distillate and medicinal liquid, be added to behind the mixing in the carbomer gel, stir evenly, transfer pH value to 6～7, add the gel that water is made set amount, promptly with triethanolamine.

7, the preparation method of rhinitis gel according to claim 6, it is characterized in that may further comprise the steps: get the Radix Angelicae Dahuricae, Fructus Xanthii, Herba Asari, Rhizoma Acori Graminei, Flos Magnoliae, Herba Ephedrae adds 10 times of water gaging distillations 3 hours, wherein volatile oil content is stable to measuring to collect distillate, medicinal liquid filters, standby, medicinal residues add Herba Taraxaci and Radix Scutellariae, add 10 times of water gagings and decoct secondary, each 1.5 hours, collecting decoction filters, and filtrate is concentrated into the thick paste that relative density is 1.15～1.20 (50 ℃), add 4 times of amounts of ethanol, stir evenly, standing over night is got supernatant and is reclaimed ethanol, being concentrated into does not have the alcohol flavor, standby; After other gets disodiumedetate and adds suitable quantity of water and make dissolving, add carbomer approximately, left standstill 12～24 hours, stir evenly, carbomer gel; Get propylene glycol, add ethyl hydroxybenzoate, polyoxyethylene sorbitan monoleate, above-mentioned distillate and medicinal liquid, be added to behind the mixing in the carbomer gel, stir evenly, transfer pH value to 6～7, add the gel that water is made set amount, promptly with triethanolamine.

8, the Quality Control Technology of rhinitis gel is characterized in that carrying out following mensuration and discriminating:

[character]:

This product rhinitis gel is brown stiff shape liquid; Gas fragrance, mildly bitter flavor;

[discriminating]:

(1), get this product 20g, add water 10ml and shake up, regulate PH1～2 with dilute hydrochloric acid, with ether extraction 3 times, each 30ml, water liquid is standby, merges ether solution, water bath method, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Herba Taraxaci control medicinal material 2g, adds water 100ml heated and boiled 1 hour, filters with absorbent cotton, and filtrate is concentrated into 30ml, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 10 μ l, control medicinal material solution 8 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with toluene-ethyl acetate-formic acid (9: 4: 1) is developing solvent, take out, put to place in the air and spend the night, put under the ultra-violet lamp (365nm) and inspect; For looking in the product chromatograph, with the corresponding position of control medicinal material chromatograph on, the fluorescence speckle of apparent same color;

(2), get discriminating (1) water liquid down, add 5% sodium hydroxide solution and regulate more than the PH10, with ether extraction 3 times, 30ml at every turn, low temperature is flung to ether, regulates PH1～2 with dilute hydrochloric acid, water bath method, residue add methanol 1ml makes dissolving, as need testing solution; Other gets the ephedrine hydrochloride reference substance, adds methanol and makes the solution that every ml contains 2mg, in contrast product solution; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 3 μ l, reference substance solution 8 μ l, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose, with chloroform-methanol-strong aqua ammonia (20: 5: 0.5) is developing solvent, launches below 25 ℃, takes out, dry, 50 ℃ of bakings 40 minutes, spray be with ninhydrin solution, and it is clear to be heated to speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(3), get this product 20g, add water 10ml, shake up, with ethyl acetate extraction 3 times, each 30ml discards acetic acid ethyl fluid, water saturation n-butanol extraction 3 times of water liquid, each 30ml merges n-butyl alcohol liquid, add water washing 2 times, each 40ml discards water lotion, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the baicalin reference substance, add methanol and make the solution that every ml contains 1mg, product solution according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B) test, is drawn need testing solution 4 μ l, reference substance solution 8 μ l in contrast, put respectively in same be on the silica gel g thin-layer plate of binding agent with the sodium carboxymethyl cellulose that contains 4% sodium acetate, (5: 3: 1: 1) be developing solvent, expansion was taken out with ethyl acetate-butanone-formic acid-water, dry, spray is with 1% ferric chloride alcoholic solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;

(4), get this product 30g, put in the round-bottomed flask, add water 200ml, connect volatile oil extractor, add ethyl acetate 2ml, reflux 2 hours is divided and is got acetic acid ethyl fluid, as need testing solution; Other gets Rhizoma Acori Graminei control medicinal material 1g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw need testing solution 10 μ l, control medicinal material solution 2 μ l, put respectively in same be on the silica GF254 lamellae of binding agent with the sodium carboxymethyl cellulose, with petroleum ether (60～90 ℃)-ethyl acetate (8: 2) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (254nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;

[inspection]:

Aristolochic Acid is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D);

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water-acetic acid (65: 35: 1) is mobile phase, and the detection wavelength is 390nm, and number of theoretical plate calculates by the aristolochic acid A peak should be not less than 2000;

It is an amount of that the preparation precision of reference substance solution takes by weighing the aristolochic acid A reference substance, adds methanol and make the solution that every 1ml contains 0.4mg, promptly;

The accurate about 10ml of this product that draws of the preparation of need testing solution adds water to 40ml, about the HCl accent pH value to 2.0 with 6mol/L, 3 (50ml of reuse ether extraction, 40ml 40ml), merges ether solution, water-bath volatilizes, residue adds dissolve with methanol and standardize solution in the 2ml measuring bottle, shakes up, and filters through microporous filter membrane (0.45 μ m), get subsequent filtrate, promptly;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

This product should detect aristolochic acid A (C ₁₇H ₁₁NO ₇);

Other should meet the pertinent regulations (two appendix I of Chinese Pharmacopoeia version in 2000 U) under the gel item;

[assay] Herba Ephedrae is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 D);

Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and acetonitrile-0.1% phosphoric acid solution (6: 94) is a mobile phase, and the detection wavelength is 207nm; Number of theoretical plate calculates by the ephedrine hydrochloride peak should be not less than 3000;

It is an amount of that the ephedrine hydrochloride reference substance that is dried to constant weight is got in the preparation of reference substance solution, and accurate the title decides, and 50% methanol that adds 0.5% hydrochloric acid is made the solution that every 1ml contains 50 μ g, shakes up, promptly;

The accurate this product 2.0ml that draws of the preparation of need testing solution puts in the 25ml measuring bottle, and 50% methanol solution that adds 0.5% hydrochloric acid is to nearly scale, supersound process 20min, 50% methanol solution that adds 0.5% hydrochloric acid is diluted to scale, shakes up, microporous filter membrane (0.45 μ m) filters, promptly;

Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;

The every ml of this product contains Herba Ephedrae with ephedrine hydrochloride (C ₁₀H ₁₅NO.HCl) meter must not be less than 0.15mg.