CN105823852A

CN105823852A - Quality control method for traditional Chinese medicine composition and traditional Chinese medicine composition

Info

Publication number: CN105823852A
Application number: CN201610309595.8A
Authority: CN
Inventors: 李兴惠
Original assignee: Individual
Current assignee: Individual
Priority date: 2016-05-11
Filing date: 2016-05-11
Publication date: 2016-08-03

Abstract

The invention relates to a quality control method for a traditional Chinese medicine composition and a traditional Chinese medicine composition, in particular to a method for conducting quality control over the traditional Chinese medicine composition. The method includes the step that whether honeysuckle flower is used in the traditional Chinese medicine composition or not is detected by using high performance liquid chromatography, and an index component used for detection is specific component of largeflower-like honeysuckle flower saponin. The invention further relates to the traditional Chinese medicine composition and a preparing method thereof. Product quality can be controlled effectively, and the prepared traditional Chinese medicine composition has excellent characteristics.

Description

The method of quality control of Chinese medicine composition and Chinese medicine composition

Technical field

The invention belongs to pharmaceutical technology field, be specifically related to a kind of Chinese medicine composition, particularly relate to the method for quality control of Chinese medicine composition.The present invention relates particularly to a kind of Chinese medicine composition.

Background technology

'Shuang Hualian ', including SHUANGHUANGLIAN KOUFUYE, SHUANGHUANGLIAN PIAN, SHUANGHUANLIAN bolt, SHUANGHUANGLIAN JIAONANG, SHUANGHUANGLIAN KELI, Suanghuanglian eye-drops etc., these preparations are to be formed by extracted the refining of Flos Lonicerae, Radix Scutellariae and Fructus Forsythiae, there is relieving the exterior syndrome with drugs of pungent in flavor and cool in nature, heat-clearing toxin-expelling functions, it is adaptable to the antibacterial such as upper respiratory tract infection that anemopyretic cold causes, tonsillitis, pharyngitis, viral pneumonia and disease of viral infection have certain curative effect.'Shuang Hualian ' has good curative effect to anemopyretic cold.

The adaptation disease that 'Shuang Hualian ' treatment is treated be epidemic febrile disease from the beginning of, heating micro evil wind is trembled with fear, lossless or have antiperspirant smooth, has a headache thirsty, pharyngalgia of coughing.Western medicine diagnose is influenza, upper respiratory tract infection, and measles is from the beginning of, acute tonsillitis, parotitis, the initial stage such as encephalitis B.'Shuang Hualian ' has relieving the exterior syndrome with drugs of pungent in flavor and cool in nature, effect of heat-clearing and toxic substances removing.It is applicable to virus and antibacterial infects pneumonia, tracheitis, bronchitis, pharyngitis, the upper respiratory tract infection such as tonsillitis and the flu caused, viral influenza causes heating, pharyngalgia, cough and Senile Asthma etc..

The effects such as animal experiment study confirms, SHUANGHUANGLIAN KOUFUYE has wider antimicrobial spectrum, has antibacterial, antipyretic, antiinflammatory, antiviral, dampness removing, jaundice eliminating.In side, Flos Lonicerae is conventional heat and toxic materials clearing away medicine, for epidemic febrile disease from the beginning of induce sweat, heat clearing away, removing toxic substances, dysentery relieving；Radix Scutellariae is conventional heat clearing and damp drying, removing toxic substances, removing heat from blood, eliminating the pathogens from the lung gunpowder；Fructus Forsythiae have clear away heart-fire, the heat of lung, stomach, dissipate pathogenic warmth, solve the effect such as sore.Three medicines play heat-clearing and toxic substances removing, the function of diuresis removing heat from blood altogether.

SHUANGHUANLIAN bolt passes through rectal absorption medicine, it is directly entered blood circulation, play general action, major advantage is a cancellation that oral medicine is easily destroyed by gastro-intestinal Fluid and liver first-pass effect, medicine is to unfavorable factors such as the stimulations of gastric mucosa, it is applicable to child, it is simultaneously available for the treatment of woman vagina and inflammation of uterus, in Animal diseases are treated, also has good application prospect.

The 'Shuang Hualian ' that 2015 editions existing Chinese Pharmacopoeias record, including SHUANGHUANGLIAN KOUFUYE, SHUANGHUANGLIAN PIAN, SHUANGHUANLIAN bolt, SHUANGHUANGLIAN JIAONANG, SHUANGHUANGLIAN KELI, Suanghuanglian eye-drops.In the quality control standard of these kinds, use the medical material Flos Lonicerae differentiating in preparation to chlorogenic acid more.

But, owing to the price of Flos Lonicerae is more and more higher, present market occurs in that use Flos Lonicerae replaces Flos Lonicerae to prepare the phenomenon of SHUANGHUANGLIAN KOUFUYE, uses the above-mentioned medical material Flos Lonicerae differentiating in preparation to chlorogenic acid unreliable.

Owing to Flos Lonicerae and Flos Lonicerae are all very different in terms of source and character or its chemical composition etc., if using Flos Lonicerae to replace Flos Lonicerae to prepare SHUANGHUANGLIAN KOUFUYE, the curative effect of SHUANGHUANGLIAN KOUFUYE can be produced strong influence.

Flos Lonicerae is dry flower or the first flower opened of band of caprifoliaceae plant Radix Ophiopogonis.Flos Lonicerae is dry flower or the first flower opened of band of caprifoliaceae plant largeflower-like honeysuckle flower, Flos Lonicerae or Lonicera confusa.Although both containing chlorogenic acid, but other effective ingredient such as rutin, luteoloside, three chemical compositions of Quercetin are more is distributed in Flos Lonicerae, and more containing largeflower-like honeysuckle flower saponin second and dipsacoside in Flos Lonicerae.

Therefore, a part of 'Shuang Hualian ' that 2015 editions existing Chinese Pharmacopoeias record, including SHUANGHUANGLIAN JIAONANG and eye drop of double rhizoma coptidis, use high performance liquid chromatography that the Flos Lonicerae in preparation differentiates the index components particularly differentiating the most whether contain largeflower-like honeysuckle flower this Flos Lonicerae of saponin second.

Although SHUANGHUANLIAN bolt and other 'Shuang Hualian ' are essentially identical in crude drug processing mode, see 2015 editions Chinese Pharmacopoeias one 735-741 page, expect that can use for reference the above-mentioned method for SHUANGHUANGLIAN JIAONANG and eye drop of double rhizoma coptidis differentiates the most whether to contain the index components of largeflower-like honeysuckle flower this Flos Lonicerae of saponin second.Regrettably, above-mentioned official method is not particularly suited for SHUANGHUANLIAN bolt.

CN104880528A (Chinese Patent Application No. 201510299374.2, Xinxiang) disclose the construction method of a kind of SHUANGHUANGLIAN KOUFUYE finger printing, wherein said SHUANGHUANGLIAN KOUFUYE is made up of Flos Lonicerae, Radix Scutellariae, Fructus Forsythiae, sucrose and essence, described construction method includes preparing need testing solution, use high performance liquid chromatography to detect the active component of described SHUANGHUANGLIAN KOUFUYE, and detect whether containing dipsacoside；Wherein chromatographic condition is: chromatographic column: WatersAcquitvUPLCBEHRP18；Flowing phase: acetonitrile-0.4% glacial acetic acid water；Gradient elution: 0-10min, 15%A-85%B；2-4min, 25%A-75%B；4-8min, 37%A-63%B；8-10min, 56%A-44%B；10-11min, 93%A-7%B；Column temperature: 35 DEG C；Detection wavelength: 300nm.It is believed that this invention builds the finger printing of SHUANGHUANGLIAN KOUFUYE, can detect whether SHUANGHUANGLIAN KOUFUYE contains dipsacoside composition simultaneously, provide basis for setting up SHUANGHUANGLIAN KOUFUYE quality supervision system.But, the method for above-mentioned CN104880528A extremely bothers, and the conventional sense operability as medicine is the strongest.

Therefore, this area still expects there is new, simple method to control the medical material particularly Flos Lonicerae used in 'Shuang Hualian ' such as SHUANGHUANLIAN suppository, for example whether there is the situation using Flos Lonicerae to replace Flos Lonicerae.

Summary of the invention

It is an object of the invention to provide a kind of new, simple method and SHUANGHUANLIAN suppository is carried out quality control, expect that these methods can efficiently control the medical material particularly Flos Lonicerae used in 'Shuang Hualian ' such as SHUANGHUANLIAN suppository, for example whether there is the situation using Flos Lonicerae to replace Flos Lonicerae.It has been unexpectedly discovered that the excellent properties in terms of using the inventive method to present at least one.

To this end, first aspect present invention provides the method that SHUANGHUANLIAN suppository is carried out quality control, the method includes using the high performance liquid chromatography step to whether using Flos Lonicerae to check in suppository.

The method of any embodiment according to a first aspect of the present invention, wherein uses high performance liquid chromatography to include operating as follows to the step whether using Flos Lonicerae to check in suppository:

(1) specification in the high performance liquid chromatography that four general rules 0512 of Chinese Pharmacopoeia version in 2015 are contained is measured；

(2) chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With water as mobile phase A, with acetonitrile as Mobile phase B, the regulation according to the form below carries out gradient elution, column temperature 32 DEG C；Evaporative light scattering detector detects；Number of theoretical plate calculates with largeflower-like honeysuckle flower saponin second should be not less than 5000；

The preparation of reference substance solution: take largeflower-like honeysuckle flower saponin second reference substance appropriate, accurately weighed, add 50% methanol and make every 1ml solution containing 0.1mg, to obtain final product.

The preparation of need testing solution: take suppository 1, put in 50ml measuring bottle, adds 50% methanol appropriate, puts heating, supersound process (power 250W in 60 DEG C of water-baths, frequency 40kHz) make dissolving, put cold place and make matrix set, add 50% methanol to scale, shake up, filter, take subsequent filtrate, to obtain final product；

Measure: accurate absorption reference substance solution and each 20 μ l of need testing solution, be injected separately into hplc determination, record and compare need testing solution chromatogram and reference substance solution chromatogram.

, wherein for using Flos Lonicerae rather than the suppository of Flos Lonicerae, in need testing solution chromatogram, should there is not the chromatographic peak corresponding with reference substance solution chromatographic peak retention time in the method for any embodiment according to a first aspect of the present invention.Otherwise, if pretending to be Flos Lonicerae for preparing SHUANGHUANLIAN bolt with Flos Lonicerae, then in need testing solution chromatogram, there will be the chromatographic peak corresponding with reference substance solution chromatographic peak retention time, the chromatographic peak of largeflower-like honeysuckle flower saponin second i.e. occurs.

The method of any embodiment according to a first aspect of the present invention, the most also includes the operation differentiating Radix Scutellariae and Flos Lonicerae.

The method of any embodiment according to a first aspect of the present invention, the operation wherein differentiated Radix Scutellariae and Flos Lonicerae comprises the steps: to take this product 1, and add water 20ml, put in tepidarium, with 10% sodium hydroxide solution regulation pH value to 7.0～7.5, make fusing, put cold place and make matrix set, filter, take filtrate 1ml, add dehydrated alcohol 4ml, put shaking several minutes in water-bath, place, take supernatant as need testing solution；Separately take baicalin reference substance, chlorogenic acid reference substance and make every 1ml solution respectively containing 0.4mg, as reference substance solution with ethanol respectively；Test according to thin layer chromatography (Chinese Pharmacopoeia four general rules 0502 of version in 2015), draw above-mentioned three kinds of solution each 3～5 μ l, put respectively on same silica gel g thin-layer plate, with the upper solution of butyl acetate-formic acid-water (7:4:3) as developing solvent, put presaturation 30 minutes in expansion cylinder, launch, take out, dry, put and inspect under ultra-violet lamp (365nm), and comparative result.For the product of conformance with standard specification, in its test sample chromatograph, with on the corresponding position of baicalin reference substance chromatograph, show the speckle of same color；With on the corresponding position of chlorogenic acid reference substance chromatograph, show the fluorescence speckle of same color.

The method of any embodiment according to a first aspect of the present invention, the most also includes the operation differentiating Fructus Forsythiae.

The method of any embodiment according to a first aspect of the present invention, the operation wherein differentiated Fructus Forsythiae comprises the steps:

Taking this product 1, add water 20ml, puts heating in hot bath and makes molten, takes out, put cold place and make matrix set, filter, take filtrate 10ml, be evaporated, and residue adds methanol 5ml supersound process makes dissolving, takes supernatant as need testing solution.Separately taking Fructus Forsythiae control medicinal material 0.5g, add methanol 10ml, be heated to reflux 20 minutes, filter, filtrate is as control medicinal material solution.Test according to thin layer chromatography (general rule 0502), draw each 10 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (5:1) as developing solvent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear, and comparative result.For the product of conformance with standard specification, in its test sample chromatograph, on position corresponding with control medicinal material chromatograph, the speckle of aobvious same color.

The method of any embodiment according to a first aspect of the present invention, the most also includes the operation that Radix Scutellariae carries out assay.

The method of any embodiment according to a first aspect of the present invention, the operation that Radix Scutellariae wherein carries out assay comprises the steps:

Specification according to Chinese Pharmacopoeia four contained high performance liquid chromatography of general rule 0512 of version in 2015 measures；

Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With methanol-water-glacial acetic acid (40:60:1) for flowing phase；Detection wavelength is 276nm.Number of theoretical plate is calculated by glycosides peaks such as Huangs should be not less than 1500；The preparation of reference substance solution: take baicalin reference substance appropriate, accurately weighed, add 50% methanol and make every 1ml solution containing 0.1mg, to obtain final product；

The preparation of need testing solution: take suppository 10, accurately weighed, grind, take about 0.3g, accurately weighed, put in beaker, add water 40ml, put and tepidarium makes dissolving, with 10% sodium hydroxide solution regulation pH value to 7.0～7.5, move in 50ml measuring bottle, let cool, add water to scale, shake up, filtering, precision measures subsequent filtrate 2ml, puts in 10ml measuring bottle, add water to scale, shake up, to obtain final product；

Algoscopy: precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, measures, to obtain final product.Generally, for the product of conformance with standard specification, SHUANGHUANLIAN suppository every in terms of baicalin (C21H18O11), should be no less than 65mg containing Radix Scutellariae.

The method of any embodiment according to a first aspect of the present invention, the most also includes the operation that Fructus Forsythiae carries out assay.

The method of any embodiment according to a first aspect of the present invention, the operation that Fructus Forsythiae wherein carries out assay comprises the steps:

Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With acetonitrile-water (21:79) for flowing phase；Detection wavelength is 278nm.Number of theoretical plate is calculated by phillyrin peak should be not less than 6000；

The preparation of reference substance solution: take phillyrin reference substance appropriate, accurately weighed, add methanol and make every 1ml solution containing 0.1mg, to obtain final product；

The preparation of need testing solution: take this product 10, accurately weighed, grind, take about 1.5g, accurately weighed, put in tool plug conical flask, precision adds water 50ml, close plug, put heating in water-bath to make to leach for 80 minutes, shake up, take out, quick freeze (-4～-3 DEG C) 80 minutes (being as the criterion not freeze), filter, precision measures subsequent filtrate 10ml, it is evaporated, the residue 1ml that adds water makes dissolving, put neutral alumina column (100～200 mesh, 6g, internal diameter is 1cm) on, with 70% ethanol 60ml eluting, collect eluent, it is concentrated to dryness, it is appropriate that residue adds 50% methanol, warm makes dissolving, move in 5ml measuring bottle, and add 50% methanol to scale, shake up, obtain；

Algoscopy: precision draws reference substance solution and each 10 μ l of need testing solution respectively, notes people's chromatograph of liquid, measures, to obtain final product.Generally, for the product of conformance with standard specification, SHUANGHUANLIAN suppository every in terms of phillyrin (C27H34O11), must not be less than 2.0mg containing Fructus Forsythiae.

The method of any embodiment according to a first aspect of the present invention, wherein said SHUANGHUANLIAN bolt prepares according to following method:

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 10～30mg (such as 15～25mg, e.g., from about 20mg) sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

Further, second aspect present invention provides a kind of SHUANGHUANLIAN suppository composition, is made up of Flos Lonicerae 2500g, Fructus Forsythiae 5000g, Radix Scutellariae 2500g and pharmaceutic adjuvant for its every 1000.

SHUANGHUANLIAN suppository composition according to a second aspect of the present invention, it prepares according to following method:

Any embodiment of the either side of the present invention, can be combined with other embodiment, as long as they do not have contradiction.Additionally, in any embodiment of either side of the present invention, arbitrary technical characteristic goes for this technical characteristic in other embodiment, as long as they do not have contradiction.The invention will be further described below.

All documents recited in the present invention, their full content is incorporated herein by, and if time implication expressed by these documents is inconsistent with the present invention, it is as the criterion with the statement of the present invention.In addition, various terms and phrase that the present invention uses have and well known to a person skilled in the art general sense, nonetheless, the present invention remains desirable at this, these terms and phrase are described in more detail and explained, the term mentioned and phrase, if any inconsistent with common art-recognized meanings, are as the criterion with the implication that the present invention is stated.

In Examples below 1～8, although assay method disclosure satisfy that the requirement of each side, but, have been found that, when preparing need testing solution, after need testing solution through filtering at room temperature places more than 1 hour, all there will be muddiness, the time starting to become turbid is all in the range of 1.07～1.73 hours.Although HPLC can be completed after prepared by sample within an hour as soon as possible analyze work, but this is unacceptable for conventional sense.The present inventor has been surprisingly found that in test, when when preparing need testing solution, after adding 0.2% (w/v) formic acid in a solvent, after all need testing solution at room temperature places more than 10 hours, all do not become turbid, and use this solvent process gained need testing solution in follow-up mensuration and unaffected, the most do not affect the result judgement that Flos Lonicerae checks.Therefore, in one embodiment of the invention, during whether using Flos Lonicerae to check in using high performance liquid chromatography to suppository, need testing solution is prepared: take suppository 1 according to following operation, put in 50ml measuring bottle, 50% methanol adding interpolation 0.2% (w/v) formic acid is appropriate, put heating, supersound process (power 250W in 60 DEG C of water-baths, frequency 40kHz) make dissolving, put cold place and make matrix set, add 50% methanol of interpolation 0.2% (w/v) formic acid to scale, shake up, filter, take subsequent filtrate, to obtain final product.

Study on the stability: by preparation example 1-preparation example 6 gained suppository, totally 6 suppository samples, they are packed, place 8 months at a temperature of being placed in 33 ± 1 DEG C, for every batch of suppository, measure they content of baicalin when 0 month and during August respectively, baicalin remnants percent when being calculated as follows this batch of suppository August: remaining percent=(0 month content of baicalin of content of baicalin ÷ in August) × 100%.Result shows, the baicalin remnants percent of preparation example 1-preparation example 55 batches of suppositorys of gained is all in the range of 97.6%～99.3%；And the baicalin remnants percent of preparation example 6 gained suppository is 91.2%；Additionally it is measured in the same method the baicalin remnants percent of test sample used by embodiment 2-7, all in the range of 88.3～92.6%；Although preparation example 6 suppository baicalin remnants percent such as grade is more than 90%, but still near or below 90% this unacceptable limit.Visible, adding appropriate sodium borate in particular step when preparing suppository is useful, is of value to the performance improving suppository product.But, when changing substrate used by preparation example 1-preparation example 6 into PEG4000/PEG1000 (10/90, w/w) and time other formulation and technology is constant, 6 batches of suppository ibid methods of gained measure baicalin remnants percents in August, result is all in the range of 89.7～93.6%.

SHUANGHUANLIAN bolt is brown or dark-brown suppository.'Shuang Hualian ' is used for heat-clearing and toxic substances removing, for cold, fever, cough, pharyngalgia.Reliable to the determined curative effect of influenza, it is the most ideal treatment of influenza medicine.Use virus bridging enzyme linked immunosorbent assay quick diagnosis infected by influenza recall rate higher, quick and precisely, treat pneumonia, bronchitis, tonsillitis effect notable simultaneously, without obvious toxic-side effects, long-term or repeat to take and do not produce residual hazard and Drug resistance, there is taking convenience simultaneously, without pain, the advantage such as rapid-action.Relieving the exterior syndrome with drugs of pungent in flavor and cool in nature, heat-clearing and toxic substances removing.It is applicable to virus and antibacterial infects pneumonia, tracheitis, bronchitis, pharyngitis, the upper respiratory tract infection such as tonsillitis and the flu caused, viral influenza causes heating, pharyngalgia, cough and Senile Asthma etc..The effects such as animal experiment study confirms, SHUANGHUANGLIAN KOUFUYE has wider antimicrobial spectrum, has antibacterial, antipyretic, antiinflammatory, antiviral, dampness removing, jaundice eliminating.In side, Flos Lonicerae is conventional heat and toxic materials clearing away medicine, for epidemic febrile disease from the beginning of induce sweat, heat clearing away, removing toxic substances, dysentery relieving；Radix Scutellariae is conventional heat clearing and damp drying, removing toxic substances, removing heat from blood, eliminating the pathogens from the lung gunpowder；Fructus Forsythiae have clear away heart-fire, the heat of lung, stomach, dissipate pathogenic warmth, solve the effect such as sore.Three medicines play heat-clearing and toxic substances removing, the function of diuresis removing heat from blood altogether.

Method/product that the present invention provides has the character of excellence.

Detailed description of the invention

The present invention can be conducted further description by the following examples, but, the scope of the present invention is not limited to following embodiment.One of skill in the art is it is understood that on the premise of without departing substantially from the spirit and scope of the present invention, can carry out various change and modification to the present invention.The present invention to test used in material and test method carry out generality and/or concrete description.Although by realize many materials that the object of the invention used and operational approach is to it is known in the art that but the present invention still describes in detail as far as possible at this.Following example further illustrate the present invention rather than limit the present invention.

Preparation example 1: preparation SHUANGHUANLIAN bolt

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 20mg sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

Preparation example 2: preparation SHUANGHUANLIAN bolt

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 10mg sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

Preparation example 3: preparation SHUANGHUANLIAN bolt

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 30mg sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

Preparation example 4: preparation SHUANGHUANLIAN bolt

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 15mg sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

Preparation example 5: preparation SHUANGHUANLIAN bolt

By the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, add 2mol/L hydrochloric acid solution when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, standing 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, add equivalent ethanol, be stirred to dissolve, filter.Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol.Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste.Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 25mg sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

Preparation example 6: preparation SHUANGHUANLIAN bolt

Embodiment 1, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z19993355, Yantai Rongchang Pharmaceutical Co., Ltd. produces)

B) thing for the purpose of largeflower-like honeysuckle flower saponin second, the step detecting Flos Lonicerae in suppository includes operating as follows:

, there is not the chromatographic peak corresponding with reference substance solution chromatographic peak retention time, shows not use in suppository Flos Lonicerae in result: in need testing solution chromatogram.

Embodiment 2, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z20****34, Heilungkiang company produces, the authentication code of commercially available product and production firm's breviary, lower same)

Embodiment 3, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z20****64, Shaanxi company produces)

Embodiment 4, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z20****38, Ningxia company produces)

Embodiment 5, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z20****43, Hubei company produces)

Embodiment 6, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z20****76, Shaanxi company produces)

Embodiment 7, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: commercially available SHUANGHUANLIAN bolt (traditional Chinese medicines quasi-word Z20****44, Jiangxi company produces)

Embodiment 8, for the purpose of largeflower-like honeysuckle flower saponin second thing, Flos Lonicerae in suppository is detected

A) test sample: preparation example 1～six batches of suppository samples of preparation example 6

Result: all in need testing solution chromatogram, the chromatographic peak corresponding with reference substance solution chromatographic peak retention time does not occurs, shows not use Flos Lonicerae in whole 6 batches of suppositorys.

Embodiment 9, the quality investigation that SHUANGHUANLIAN bolt is carried out

Test sample: the test sample that preparation example 1～preparation example 6 gained suppository, embodiment 1～embodiment 7 are used, totally 13 suppository samples

(1) Radix Scutellariae and Flos Lonicerae are differentiated:

Taking this product 1, add water 20ml, puts in tepidarium, with 10% sodium hydroxide solution regulation pH value to 7.0～7.5, make fusing, put cold place and make matrix set, filter, take filtrate 1ml, add dehydrated alcohol 4ml, put shaking several minutes in water-bath, place, take supernatant as need testing solution；Separately take baicalin reference substance, chlorogenic acid reference substance and make every 1ml solution respectively containing 0.4mg, as reference substance solution with ethanol respectively；Test according to thin layer chromatography (Chinese Pharmacopoeia four general rules 0502 of version in 2015), draw above-mentioned three kinds of solution each 3～5 μ l, put respectively on same silica gel g thin-layer plate, with the upper solution of butyl acetate-formic acid-water (7:4:3) as developing solvent, put presaturation 30 minutes in expansion cylinder, launch, take out, dry, put and inspect under ultra-violet lamp (365nm), and comparative result.For the product of conformance with standard specification, in its test sample chromatograph, with on the corresponding position of baicalin reference substance chromatograph, show the speckle of same color；With on the corresponding position of chlorogenic acid reference substance chromatograph, show the fluorescence speckle of same color.Result shows, 13 batches of suppository samples all meet above-mentioned standard criterion.

(2) Fructus Forsythiae is differentiated:

Taking this product 1, add water 20ml, puts heating in hot bath and makes molten, takes out, put cold place and make matrix set, filter, take filtrate 10ml, be evaporated, and residue adds methanol 5ml supersound process makes dissolving, takes supernatant as need testing solution.Separately taking Fructus Forsythiae control medicinal material 0.5g, add methanol 10ml, be heated to reflux 20 minutes, filter, filtrate is as control medicinal material solution.Test according to thin layer chromatography (general rule 0502), draw each 10 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (5:1) as developing solvent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear, and comparative result.For the product of conformance with standard specification, in its test sample chromatograph, on position corresponding with control medicinal material chromatograph, the speckle of aobvious same color.Result shows, 13 batches of suppository samples all meet above-mentioned standard criterion.

(3) Radix Scutellariae is carried out assay:

Algoscopy: precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, measures, to obtain final product.Generally, for the product of conformance with standard specification, SHUANGHUANLIAN suppository every in terms of baicalin (C21H18O11), should be no less than 65mg containing Radix Scutellariae.Result shows, 13 batches of suppository samples all meet above-mentioned standard criterion, every containing Radix Scutellariae in terms of baicalin (C21H18O11) all in the range of 74～86mg.

(4) Fructus Forsythiae is carried out assay:

Result shows, 13 batches of suppository samples all meet above-mentioned standard criterion, every containing Fructus Forsythiae in terms of phillyrin (C27H34O11) all in the range of 2.7～4.1mg.

Embodiment described above is only the preferred embodiment lifted by absolutely proving the present invention, and protection scope of the present invention is not limited to this.The equivalent that those skilled in the art are made on the basis of the present invention substitutes or conversion, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.

Claims

1. pair method that SHUANGHUANLIAN suppository carries out quality control, the method includes using the high performance liquid chromatography step to whether using Flos Lonicerae to check in suppository.

Method the most according to claim 1, wherein uses high performance liquid chromatography to include operating as follows to the step whether using Flos Lonicerae to check in suppository:

The preparation of reference substance solution: take largeflower-like honeysuckle flower saponin second reference substance appropriate, accurately weighed, add 50% methanol and make every 1ml solution containing 0.1mg, to obtain final product；

The preparation of need testing solution: take suppository 1, put in 50ml measuring bottle, adds 50% methanol appropriate, puts heating, supersound process (power 250W in 60 DEG C of water-baths, frequency 40kHz) make dissolving, put cold place and make matrix set, add 50% methanol to scale, shake up, filter, take subsequent filtrate, to obtain final product；[or, taking suppository 1, put in 50ml measuring bottle, 50% methanol adding interpolation 0.2% (w/v) formic acid is appropriate, put heating, supersound process (power 250W in 60 DEG C of water-baths, frequency 40kHz) make dissolving, put cold place and make matrix set, add 50% methanol of interpolation 0.2% (w/v) formic acid to scale, shake up, filter, take subsequent filtrate, to obtain final product]；

, wherein for using Flos Lonicerae rather than the suppository of Flos Lonicerae, in need testing solution chromatogram, should there is not the chromatographic peak corresponding with reference substance solution chromatographic peak retention time in method the most according to claim 1；Otherwise, if pretending to be Flos Lonicerae for preparing SHUANGHUANLIAN bolt with Flos Lonicerae, then in need testing solution chromatogram, there will be the chromatographic peak corresponding with reference substance solution chromatographic peak retention time, the chromatographic peak of largeflower-like honeysuckle flower saponin second i.e. occurs.

Method the most according to claim 1, it is characterised in that:

The most also including the operation differentiating Radix Scutellariae and Flos Lonicerae, it comprises the steps: to take this product 1, and add water 20ml, put in tepidarium, with 10% sodium hydroxide solution regulation pH value to 7.0～7.5, make fusing, put cold place and make matrix set, filter, take filtrate 1ml, add dehydrated alcohol 4ml, put shaking several minutes in water-bath, place, take supernatant as need testing solution；Separately take baicalin reference substance, chlorogenic acid reference substance and make every 1ml solution respectively containing 0.4mg, as reference substance solution with ethanol respectively；Test according to thin layer chromatography (Chinese Pharmacopoeia four general rules 0502 of version in 2015), draw above-mentioned three kinds of solution each 3～5 μ l, put respectively on same silica gel g thin-layer plate, with the upper solution of butyl acetate-formic acid-water (7:4:3) as developing solvent, put presaturation 30 minutes in expansion cylinder, launch, take out, dry, put and inspect under ultra-violet lamp (365nm), and comparative result；For the product of conformance with standard specification, in its test sample chromatograph, with on the corresponding position of baicalin reference substance chromatograph, show the speckle of same color；With on the corresponding position of chlorogenic acid reference substance chromatograph, show the fluorescence speckle of same color；

Or, the most also including the operation that Fructus Forsythiae is differentiated, it comprises the steps:

Taking this product 1, add water 20ml, puts heating in hot bath and makes molten, takes out, put cold place and make matrix set, filter, take filtrate 10ml, be evaporated, and residue adds methanol 5ml supersound process makes dissolving, takes supernatant as need testing solution；Separately taking Fructus Forsythiae control medicinal material 0.5g, add methanol 10ml, be heated to reflux 20 minutes, filter, filtrate is as control medicinal material solution；Test according to thin layer chromatography (general rule 0502), draw each 10 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol (5:1) as developing solvent, launch, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear, and comparative result；For the product of conformance with standard specification, in its test sample chromatograph, on position corresponding with control medicinal material chromatograph, the speckle of aobvious same color.

Method the most according to claim 1, the most also includes the operation that Radix Scutellariae carries out assay, and it comprises the steps:

Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With methanol-water-glacial acetic acid (40:60:1) for flowing phase；Detection wavelength is 276nm；Number of theoretical plate is calculated by glycosides peaks such as Huangs should be not less than 1500；The preparation of reference substance solution: take baicalin reference substance appropriate, accurately weighed, add 50% methanol and make every 1ml solution containing 0.1mg, to obtain final product；

Algoscopy: precision draws reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, measures, to obtain final product.

Method the most according to claim 1, the most also includes the operation that Fructus Forsythiae carries out assay, and it comprises the steps:

Chromatographic condition and system suitability: with octadecylsilane chemically bonded silica as filler；With acetonitrile-water (21:79) for flowing phase；Detection wavelength is 278nm；Number of theoretical plate is calculated by phillyrin peak should be not less than 6000；

Algoscopy: precision draws reference substance solution and each 10 μ l of need testing solution respectively, notes people's chromatograph of liquid, measures, to obtain final product.

7. according to the method for any one of claim 1-5, described SHUANGHUANLIAN bolt prepares according to following method: by the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, 2mol/L hydrochloric acid solution is added when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, stands 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, adds equivalent ethanol, it is stirred to dissolve, filters；Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol；Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste；Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

8. according to the method for any one of claim 1-5, described SHUANGHUANLIAN bolt prepares according to following method: by the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, 2mol/L hydrochloric acid solution is added when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, stands 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, adds equivalent ethanol, it is stirred to dissolve, filters；Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol；Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste；Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 10～30mg (such as 15～25mg, e.g., from about 20mg) sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.

9. a SHUANGHUANLIAN suppository composition, is made up of Flos Lonicerae 2500g, Fructus Forsythiae 5000g, Radix Scutellariae 2500g and pharmaceutic adjuvant for its every 1000.

SHUANGHUANLIAN suppository composition the most according to claim 9, it prepares according to following method: by the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, and it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, 2mol/L hydrochloric acid solution is added when 80 DEG C, regulation pH value, to 1.0～2.0, is incubated 1 hour, stands 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, adds equivalent ethanol, it is stirred to dissolve, filters；Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol；Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste；Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, add 10～30mg (such as 15～25mg, e.g., from about 20mg) sodium borate, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product；

Or, it prepares according to following method: by the Radix Scutellariae boiling three times of 2500g, 2 hours for the first time, second and third time each 1 hour, collecting decoction, filters, it is 1.03～1.08 (80 DEG C) that filtrate is concentrated into relative density, adds 2mol/L hydrochloric acid solution when 80 DEG C, and regulation pH value is to 1.0～2.0, it is incubated 1 hour, stands 24 hours, filter, precipitate adds 6～8 times amount water, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, adds equivalent ethanol, it is stirred to dissolve, filters；Filtrate is with 2mol/L hydrochloric acid solution regulation pH value to 2.0, and 60 DEG C are incubated 30 minutes, stand 12 hours, filter, and precipitation washes with water to pH value to 5.0, continues and is washed till pH value 7.0 with 70% ethanol；Precipitate adds water in right amount, with 40% sodium hydroxide solution regulation pH value to 7.0～7.5, is stirred to dissolve, standby；By the Flos Lonicerae of 2500g, the Fructus Forsythiae boiling secondary of 5000g, each 1.5 hours, collecting decoction, filtering, filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (70～80 DEG C), is slowly added to ethanol when being cooled to 40 DEG C under stirring, make alcohol content reach 75%, stand 12 hours, leaching supernatant, reclaim ethanol, concentrated solution adds ethanol again makes alcohol content reach 85%, is sufficiently stirred for, and stands 12 hours, leaching supernatant, reclaims ethanol to without alcohol taste；Adding above-mentioned Radix Scutellariae extract aqueous solution, stir evenly, and regulate pH value to 7.0～7.5, concentrating under reduced pressure becomes thick paste, cold drying, pulverizes；Separately taking semi-synthetic fatty acid ester 780g, heating is dissolved, and temperature is maintained at 40 DEG C ± 2 DEG C, adds above-mentioned dried cream powder, mixing, and moulding is made 1000, to be obtained final product.