CN103356739B - A kind of Shuanghuanglian oral liquid for livestock and extracting method thereof - Google Patents

A kind of Shuanghuanglian oral liquid for livestock and extracting method thereof Download PDF

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CN103356739B
CN103356739B CN201210097155.2A CN201210097155A CN103356739B CN 103356739 B CN103356739 B CN 103356739B CN 201210097155 A CN201210097155 A CN 201210097155A CN 103356739 B CN103356739 B CN 103356739B
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weight
extract
flos lonicerae
temperature
volume
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CN103356739A (en
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张许科
刘兴金
张晓会
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Luoyang Huizhong Animal Medicine Co Ltd
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Luoyang Huizhong Animal Medicine Co Ltd
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Abstract

The invention provides a kind of 'Shuang Hualian ' for animals, be made up of active component and adjuvant, wherein, active component is Radix Scutellariae 20%-25% weight, Flos Lonicerae 20%-25% weight, Fructus Forsythiae 50%-60% weight.Active component is pressed primary crude drug and is calculated.The preparation method that present invention also offers above-mentioned 'Shuang Hualian ', is processed by extract at low temperature, it is achieved that simplify extraction process, improves production efficiency, and is effectively improved purity and the stability of multiple 'Shuang Hualian ' finished product.

Description

A kind of Shuanghuanglian oral liquid for livestock and extracting method thereof
Technical field
The present invention relates to a kind of 'Shuang Hualian ' and preparation method thereof, particularly relate to a kind of Shuanghuanglian oral liquid for livestock and extract and refining method.
Background technology
In recent years, along with development and the popularization of aquaculture, livestock and poultry variation day by day, complication, substantial amounts of chemicals uses in Production of Livestock and Poultry, the abuse of medicine makes pathogenic microorganism toleration increase, and not only increases the difficulty for the treatment of disease, and also the health of the mankind in serious threat.Along with people's living standard raising and cultivation idea renewal, treat and prevent Animal diseases with Chinese medicine and day by day praised highly.
SHUANGHUANGLIAN KOUFUYE is that veterinary clinic uses the wider pure compound Chinese medicinal preparation of one, it is made up of Radix Scutellariae, Flos Lonicerae, 3 kinds of medicines of Fructus Forsythiae, have heat-clearing and toxic substances removing, dispelling wind dissipates the effects such as table, there is effect antibacterial, antiviral, raising immunity of organisms, the antibacterials such as staphylococcus aureus, streptococcus pneumoniae, Hemolytic streptococcus, dysentery bacterium are all had inhibitory action, and the pneumonia that respiratory tract infection and viral disease are caused has peculiar curative effect.
At present, in the production of SHUANGHUANGLIAN KOUFUYE, traditional process for extracting such as the method for " People's Republic of China's veterinary drug allusion quotation (version two in 2010) ", it is necessary to medicine material is repeatedly decocted, lixiviate multiple times of filtration repeatedly, operating procedure is complicated, relatively costly.And said method is insufficient for the extraction of effective ingredient, extraction efficiency is low, and the production cycle is longer, and production cost is higher, and impurity content is high, and the stability of finished product needs to improve further.
Summary of the invention
In view of this, a kind of 'Shuang Hualian ' of offer is provided, it has obvious bacteriostasis, as a further improvement on the present invention, the invention provides the easy extracting method of a kind of 'Shuang Hualian ' and the product using the method to prepare, to realize simplifying extraction process, improve production efficiency, and be effectively improved purity and the stability of 'Shuang Hualian ' finished product.
The present invention is achieved through the following technical solutions:
A kind of 'Shuang Hualian ' for animals, is made up of active component and adjuvant, wherein, and active component Radix Scutellariae 20%-25% weight, Flos Lonicerae extract 20%-25% weight, Fructus Forsythiae extract 50%-60% weight;Adjuvant contains the carbomer of 0.2%-0.8% volume.Wherein, active component presses primary crude drug calculating.
The high molecular polymer of carbomer acrylic acid bonding allyl sucrose or tetramethylolmethane allyl ether, it is preferable that Carbopol 941, Carbopol, carbomer934, carbomer934, more preferably carbomer940.
The preparation method of a kind of 'Shuang Hualian ', comprises the following steps:
1) by Radix Scutellariae in hot reflux low-temperature extracting tank (or claiming refluxed cryogenic extraction pot), low temperature reflux extracts, and extracting concentration after terminating is clear paste, acid precipitation, is washed till neutrality with alcohol, obtains Radix Scutellariae extract;
2) Flos Lonicerae, Fructus Forsythiae being added in hot reflux low-temperature extracting tank, low temperature reflux extracts, and extracting concentration after terminating is clear paste, adds alcohol stirring, stand and leaching supernatant after cooling, it is thus achieved that Flos Lonicerae, Fructus Forsythiae extract;
3) by step 1) Radix Scutellariae extract that obtains, add carbomer, stir, mix with Fructus Forsythiae, Flos Lonicerae extract, adjustment pH value 7.0, fill sterilizing, obtain 'Shuang Hualian '.
Preferably, step 1 of the present invention) in also include use chitosan clarification Radix Scutellariae extract step.
It is highly preferred that step 1 of the present invention) in add chitosan before extracting solution sodium hydroxide is regulated pH value to 5.0-6.0, the content of the chitosan of addition is the 0.5%-2% of cumulative volume.
Preferably, the present invention, before adding Flos Lonicerae extraction pot, has carried out cellulose treatment.
It is highly preferred that the concentration of cellulase of the present invention is 0.5%-1% volume, it is 0.5-1: 1 with the volume ratio of Extraction solvent.
Preferably, step 3 of the present invention) in also include the 'Shuang Hualian ' that will obtain, after high speed centrifugation, use microporous membrane to be filtered.
It is highly preferred that high speed centrifugation method of the present invention is 8000-10000r/min high speed centrifugation;Described filter method is use the filtering with microporous membrane of 0.6-0.8 μm to process.
Preferably, step 1 of the present invention) and 2) in Radix Scutellariae with Fructus Forsythiae, Flos Lonicerae before extraction, also include the processing procedure making to be soaked in water.
Preferably, step 1 of the present invention) and 2) described in extraction time be 6-8 time, Extracting temperature is 60-80 DEG C, thickening temperature 50-70 DEG C.
Preferably, carbomer of the present invention is carbomer940, and addition is 0.2%-0.8% volume.
It is highly preferred that carbomer940 content of the present invention is 0.2%-0.5% volume.
Preferably, the preparation method of 'Shuang Hualian ' of the present invention, comprise the following steps:
1) Radix Scutellariae is added in traditional Chinese herbs by thermal reflux low-temperature extracting tank, add the water of 10-15 times, control pressure 40-50Kpa, soak 30-60min and make medical material drench;At temperature 60-80 DEG C, extract 6-8 time, each 20-30min, until extracting solution is substantially colorless, extracts whole extracting solution out to concentration tank, control temperature 50-70 DEG C and be concentrated into the clear paste that proportion is 1.05-1.10, regulate pH value to 5.0-6.0 with sodium hydroxide, add the 0.5%-2% volume chitosan of total measurement (volume), stir, stand 12h, filter, take supernatant, with salt acid for adjusting pH value to 1.5-2.0,80 DEG C of insulation 1h, standing 3-5h, taking precipitation, to be washed to pH value be 5.0, and continuation 70%-75% ethanol is washed till pH value 7.0, dry, obtain Radix Scutellariae extract;
2) extracting honeysuckle, pulverizes, adds the water of 4-6 times by Flos Lonicerae weight, add 0.5%-1% volume cellulase by the amount of solvent volume 50%-100%, regulate temperature and be 35-40 DEG C, enzymolysis 3-4h, raise temperature to 70-80 DEG C, maintain 20-30min, make enzyme-deactivating;
3) take Fructus Forsythiae, with step 2) process after Flos Lonicerae together with add in extraction pot, add dry weight 12-15 times of weight of medical material water, in control tank, temperature 60-80 DEG C carries out extract at low temperature, extracts 6-8 time, each 20-30min, filter, be concentrated into the clear paste that proportion is 1.2-1.3 at temperature 60-70 DEG C, when being cooled to 40 DEG C, be slowly added to ethanol, alcohol content is made to reach 75%, it is sufficiently stirred for, stands 12h, leaching supernatant, reclaim ethanol to without alcohol taste, obtaining the extract of Flos Lonicerae, Fructus Forsythiae.
4) taking Radix Scutellariae extract, the hot sodium hydroxide with 10% dissolves, and adds carbomer by the amount of cumulative volume 0.2%-0.8%, stir, mix with Fructus Forsythiae, Flos Lonicerae extract, regulate pH value 7.0, stirring, 4-8 DEG C of cold preservation 24h, filter, adding water to scale, correction pH value also adds water to scale, 8000-10000r/min high speed centrifugation, the filtering with microporous membrane in 0.6-0.8 μm of aperture, fill, sterilizing, obtain 'Shuang Hualian '.
As seen from the above, the present invention can obtain a kind of novel 'Shuang Hualian ', and described preparation is granule, spray, oral liquid or capsule.
Preferably, preparation of the present invention is oral liquid.
Therefore, the present invention can provide above-mentioned 'Shuang Hualian ', the application in the veterinary drug preparing antibacterial, antiviral, raising immunity of organisms.
Technique effect
The 'Shuang Hualian ' of the present invention at least has the advantage that
1. remaining the active component in Chinese medicine to greatest extent, extract more abundant, extraction ratio is higher;
2. shorten technological process, save extraction time;
3. the extract clarity obtained is higher, is long placed in and not easily precipitates;
4. suppress growth of microorganism, it is easy to reach limitation standard in microbe.
Detailed description of the invention
The 'Shuang Hualian ' of the embodiment of the present invention, refers to and is made up of active component and adjuvant, wherein, activity extract is Radix Scutellariae 20%-25% weight, Flos Lonicerae 20%-25% weight, Fructus Forsythiae 50%-60% weight;Adjuvant contains the carbomer of 0.2%-0.8% volume.Wherein, active component presses primary crude drug calculating.
The carbomer of the embodiment of the present invention is the high molecular polymer of acrylic acid bonding allyl sucrose or tetramethylolmethane allyl ether, wherein, it is preferable that carbomer940.
The Chinese crude drug of the embodiment of the present invention is common Radix Scutellariae and Flos Lonicerae, Fructus Forsythiae medical material, it is possible to use the roughing raw materials such as section commonly used in the art, decoction pieces.
The 'Shuang Hualian ' of the embodiment of the present invention is drink form, it is also possible to be the forms such as granule, spray or capsule;As after obtaining Shuang Huanglian liquid extract, the means such as lyophilization or spray drying can adopted to obtain SHUANGHUANLIAN solid dosage forms, and add the form such as adjuvant or carrier acquisition granule, spray or capsule.
The preparation method of the 'Shuang Hualian ' of the embodiment of the present invention, extracts the extract obtaining Radix Scutellariae extract and Flos Lonicerae, Fructus Forsythiae respectively mainly by low temperature reflux;It is not required to high temperature decoct and long-time immersion, effectively reduces raw material of Chinese medicine loss of effective ingredient in extraction process, it is ensured that the quality of the 'Shuang Hualian ' of the present invention and clinical effectiveness.
In the preparation method of the 'Shuang Hualian ' of the embodiment of the present invention, chitosan clarification Radix Scutellariae extracting solution is employed when extracting Radix Scutellariae, inventor have found that and can be formed active group by chitosan in acid condition, the materials such as the protein in Radix Scutellariae extracting solution, polysaccharide, tannin can be played adsorption, eliminate the process that in conventional method, acid is repeatedly dissolved after sinking, precipitated, the retention rate of effective ingredient baicalin is high, save the time of remove impurity, reduce production cost, and the 'Shuang Hualian ' solution clarification obtained, it does not have wall cling phenomenon.Addition chitosan carries out clarification and can also carry out after acid precipitation processes, but preferably, adds chitosan and clarify, it is possible to reduce the step of acid precipitation, improve the efficiency of acid precipitation after obtaining Radix Scutellariae clear paste;It is highly preferred that extracting solution sodium hydroxide is regulated pH value to 5.0-6.0 before adding chitosan in the embodiment of the present invention, the content of the chitosan of addition is the 0.5%-2% of cumulative volume.
Extracting Flos Lonicerae, the problem that in cell, the chlorogenic acid rate of transform is low for traditional extraction process, the embodiment of the present invention, before adding Flos Lonicerae extraction pot, has carried out cellulose treatment.By adding cellulose treatment, it is possible to destroying the cell wall of plant, being more beneficial for the dissolution of intracellular organic matter, thus improve leaching rate and the extraction ratio of effective ingredient such as chlorogenic acid in Flos Lonicerae.Preferably, the concentration of cellulase described in the embodiment of the present invention is 0.5%-1% volume, is 0.5-1: 1 with the volume ratio of Extraction solvent.
In the preparation method of the 'Shuang Hualian ' of the embodiment of the present invention, also use high speed centrifugation, with hyperfiltration process, 'Shuang Hualian ' has been carried out further refinement treatment;High speed centrifugation method described in the embodiment of the present invention is 8000-10000r/min high speed centrifugation;Described filter method is use the filtering with microporous membrane of 0.6-0.8 μm to process;It is used in combination with filtering with microporous membrane process by high speed centrifugation, it is possible to eliminating the fine particles in 'Shuang Hualian ' system, obtained oral liquid formulation clarity is higher, is long placed in and is not easily layered, and stability is better.
Finally, the embodiment of the present invention adds in prepared by oral liquid the carbomer of 0.2%-0.8% volume, not only inhibit mycete and the growth of antibacterial in oral liquid, extend the shelf-life;And the oral liquid finished product stability that obtains 'Shuang Hualian ' is better, and there is no wall cling phenomenon.
Extraction equipment used in the present embodiment is traditional Chinese herbs by thermal reflux extract at low temperature concentration unit, and Xi'an Ya Bao pharmaceutical machine factory produces, unit type: TN0.1/20.Baikal skullcap root, Flos Lonicerae, Fructus Forsythiae are all purchased from Kang Xin prepared slices of Chinese crude drugs company limited, and wherein Hebei, Radix Scutellariae original producton location, Shandong, the Flos Lonicerae place of production, Fructus Forsythiae original producton location is Shanxi.Chitosan, Jinan Haidebei Marine Organism Engineering Co., Ltd., deacetylation: 85.5%.Cellulase, Shenzhen Lv Weikang biological engineering company limited.Microporous filter membrane, Tian Jinjin rises experimental facilities company limited.Carbomer940, Haidian, Beijing fellow member of an association or organization's Fine Chemical Works.Acetic acid, Chengdu Ke Long chemical reagent factory.Other reagent are common agents in market, are analytical pure.
Below in conjunction with specific embodiment further describe the present invention, advantages of the present invention and feature will be with describe apparent.But these embodiments are only exemplary, the scope of the present invention is not constituted any restriction.It will be understood by those skilled in the art that and the details of technical solution of the present invention and form can be modified or replace lower without departing from the spirit and scope of the present invention, but these amendments and replacement each fall within protection scope of the present invention.
Embodiment 1, SHUANGHUANGLIAN KOUFUYE preparation preparation example 1
Radix Scutellariae 25%, Flos Lonicerae 25%, Fructus Forsythiae 50% (above medicine weighs by weight percentage), then it is prepared by the following step:
A, baikal skullcap root decoction pieces, add in the filling of traditional Chinese herbs by thermal reflux extract at low temperature, add water again by medical material weight 12, control pressure 50Kpa, soak 1h.Passing into vapours, control temperature 70 C and carry out extract at low temperature, repeatedly extract 6 times, each 30min, extracting solution is substantially colorless, and extraction terminates.Extract whole extracting solution out to concentration tank, control temperature 60 C and be concentrated into the clear paste that proportion is 1.10, add the chitosan (with 1% acetic acid for solvent) of 1% in medicinal liquid 1: 1 ratio, stir, stand 12h, filter, take supernatant.With salt acid for adjusting pH value to 1.5-2.0,80 DEG C of insulation 1h, stand 3-5h, taking precipitation, to be washed to pH value be 5.0, continues to be washed till pH value 7.0 with 75% ethanol, drying, standby.
B, being pulverized by Flos Lonicerae, add the water of 6 times by Flos Lonicerae weight, add 0.5% cellulase, cellulase and water volume ratio are 1: 1, regulate temperature and are 35-40 DEG C, after enzymolysis 4h, raise temperature to 80 DEG C, maintain 20min, make enzyme-deactivating.
C, Fructus Forsythiae is added in extraction pot together with Flos Lonicerae, add water again by Fructus Forsythiae weight 12.Pass into vapours, control temperature 80 DEG C in tank and carry out extract at low temperature, extract 6 times, each 30min.Extraction terminates, and filters, and 60-70 DEG C is concentrated into the clear paste that proportion is 1.25, is slowly added to ethanol when being cooled to 40 DEG C, make alcohol content reach 75%, be sufficiently stirred for, and stands 12h, leaching supernatant, reclaims ethanol to without alcohol taste, standby.
D, taking Radix Scutellariae extract, the hot sodium hydroxide 2L with 10% dissolves, and adds carbomer940 by the amount of cumulative volume 0.2%, stir, add Fructus Forsythiae, Flos Lonicerae extract mixing, regulate pH value 7.0, stirring, 4 DEG C of cold preservation 24h, filter, adding water to scale (every milliliter containing primary crude drug 1g), correction pH value also adds water to scale, 8000r/min high speed centrifugation 10min, the filtering with microporous membrane that aperture is 0.65 μm, fill, 100 DEG C of high pressure 30min sterilizings, to obtain final product.
Embodiment 2, SHUANGHUANGLIAN KOUFUYE preparation preparation example 2
Radix Scutellariae 20%, Flos Lonicerae 20%, Fructus Forsythiae 60% (above medicine weighs by weight percentage), then it is prepared by the following step:
A, baikal skullcap root decoction pieces, add in the filling of traditional Chinese herbs by thermal reflux extract at low temperature, add the water of 10 times amount by weight, control pressure 45Kpa, soak 30min.Pass into vapours, control temperature 80 DEG C in tank and carry out extract at low temperature, extract 8 times, each 20min.Extraction terminates, and extracts whole extracting solution out to concentration tank, controls temperature 70 C and is concentrated into the clear paste that proportion is 1.10, chitosan clarifier, makes the content of chitosan reach 1%.Stir, stand 12h, filter, take supernatant.Being incubated 1h with salt acid for adjusting pH value to 2.0,80 DEG C, stand 3-5h, taking precipitation, to be washed to pH value be 5.0, continues to be washed till pH value 7.0 with 70% ethanol, drying, standby.
B, by Flos Lonicerae sample comminution, add the water of 4 times amount by weight, add 0.5% cellulase by 1: 1 volume, regulate temperature and be 35-40 DEG C, enzymolysis 3.5h, raise temperature to 75 DEG C, maintain 20min, make enzyme-deactivating.
C, Fructus Forsythiae is added in extraction pot together with Flos Lonicerae, add water again by Flos Lonicerae volume 12.Pass into vapours, control temperature 75 DEG C in tank and carry out extract at low temperature, extract 7 times, each 30min.Extraction terminates, and filters, and 65 DEG C are concentrated into the clear paste that proportion is 1.3, are slowly added to ethanol when being cooled to 40 DEG C, make alcohol content reach 75%, be sufficiently stirred for, and stands 12h, leaching supernatant, reclaims ethanol to without alcohol taste, standby.
D, taking Radix Scutellariae extract, the hot sodium hydroxide 8L with 10% dissolves, and adds carbomer940 by the amount of cumulative volume 0.4%, stir, mix with Fructus Forsythiae, Flos Lonicerae extract, regulate pH value 7.0, stirring, 4 DEG C of cold preservation 24h, filter, adding water to scale, correction pH value also adds water to scale, 10000r/min high speed centrifugation, the filtering with microporous membrane that aperture is 0.8 μm, fill, 115 DEG C of high pressure 20min sterilizings, to obtain final product.
Embodiment 3, SHUANGHUANGLIAN KOUFUYE preparation preparation example 3
Radix Scutellariae 23%, Flos Lonicerae 23%, Fructus Forsythiae 56% (above medicine weighs by weight percentage), then it is prepared by the following step:
A, baikal skullcap root decoction pieces, add in the filling of traditional Chinese herbs by thermal reflux extract at low temperature, add the water of 10 times amount by weight, control pressure 45Kpa, soak 30min.Pass into vapours, control temperature 80 DEG C in tank and carry out extract at low temperature, extract 8 times, each 20min.Extraction terminates, and extracts whole extracting solution out to concentration tank, controls temperature 70 C and is concentrated into the clear paste that proportion is 1.10, chitosan clarifier, makes the content of chitosan reach 1%.Stir, stand 12h, filter, take supernatant.Being incubated 1h with salt acid for adjusting pH value to 2.0,80 DEG C, stand 3-5h, taking precipitation, to be washed to pH value be 5.0, continues to be washed till pH value 7.0 with 70% ethanol, drying, standby.
B, by Flos Lonicerae sample comminution, add the water of 4 times amount by weight, add 0.5% cellulase by 1: 1 volume, regulate temperature and be 35-40 DEG C, enzymolysis 3.5h, raise temperature to 75 DEG C, maintain 20min, make enzyme-deactivating.
C, Fructus Forsythiae is added in extraction pot together with Flos Lonicerae, add water again by Flos Lonicerae volume 12.Pass into vapours, control temperature 75 DEG C in tank and carry out extract at low temperature, extract 7 times, each 30min.Extraction terminates, and filters, and 65 DEG C are concentrated into the clear paste that proportion is 1.3, are slowly added to ethanol when being cooled to 40 DEG C, make alcohol content reach 75%, be sufficiently stirred for, and stands 12h, leaching supernatant, reclaims ethanol to without alcohol taste, standby.
D, taking Radix Scutellariae extract, the hot sodium hydroxide 8L with 10% dissolves, and adds carbomer940 by the amount of cumulative volume 0.8%, stir, mix with Fructus Forsythiae, Flos Lonicerae extract, regulate pH value 7.0, stirring, 4 DEG C of cold preservation 24h, filter, adding water to scale, correction pH value also adds water to scale, 9000r/min high speed centrifugation, the filtering with microporous membrane that aperture is 0.8 μm, fill, sterilizing, to obtain final product.
Embodiment 3, the present invention extracting method compare with other extracting method
Sample 1: take the embodiment of the present invention 1 and prepare the sample of gained.
Sample 2: adopt People's Republic of China's veterinary drug allusion quotation (version two in 2010) to prepare sample, extracting honeysuckle 375g, Radix Scutellariae 375g, Fructus Forsythiae 750g, carry out as follows: Radix Scutellariae is cut into slices, boiling 3 times, 1st 2h, 2nd, 3 each 1h, collecting decoction, filter, filtrate concentration also adds 2mol/L hydrochloric acid solution and regulates pH value in right amount to 1.0-2.0 when 80 DEG C, insulation 1h, stand 12h, filter, precipitation adds 6-8 times amount water, it is adjusted to pH value to 7.0 with 40% sodium hydroxide solution, add the ethanol of equivalent again, it is stirred to dissolve, filter, filtrate with 2mol/L salt acid for adjusting pH value to 2.0, 60 DEG C of insulation 30min, stand 12h, filter, precipitation adds ethanol and is washed till pH value 7.0, wave most ethanol standby.Flos Lonicerae, Fructus Forsythiae adds water warm macerating 30min, decoct 2 times, each 1.5h, collecting decoction, filter, it is 1.2-1.25 that filtrate is concentrated into relative density, it is slowly added to ethanol when being cooled to 40 DEG C, alcohol content is made to reach 75%, it is sufficiently stirred for, stand 12h, leaching supernatant, residue adds 75% appropriate amount of ethanol, stir evenly, stand 12h, filter, merge ethanol, reclaim ethanol to without alcohol taste, add Radix Scutellariae extract, and it is appropriate to add water, adjust pH value to 7.0 with 40% sodium hydroxide solution, stir evenly, cold preservation (4-8 DEG C) 72h, filter, filtrate regulates pH value to 7.0, add water and make 1000ml, stir evenly, stand 12h, filter, fill, 100 DEG C of 30min autoclavings, obtain.
Sample 3: adopt the method for People's Republic of China's veterinary drug allusion quotation (version two in 2010) to prepare Radix Scutellariae, Flos Lonicerae, Fructus Forsythiae extract, the amount pressing medicinal liquid cumulative volume 0.2% when extract mixes adds carbomer940, and remaining steps is prepared with sample 2.
In SHUANGHUANLIAN, the detection method under content reference " neutralizing people's republic's veterinary drug allusion quotation " version SHUANGHUANGLIAN KOUFUYE item in 2010 of main component baicalin, chlorogenic acid, phillyrin carries out.
Stability: take the sample that above 2 kinds of methods prepare, fill, 250ml/ bottle, sterilizing, sealing, left at room temperature 60 days, seen whether precipitation, lamination.
Microbial check: carry out with reference to membrane-filter procedure under " neutralizing people's republic's veterinary drug allusion quotation " version annex 101 limit test of microbe item in 2010.Method is as follows: takes 2 bottles of sample, aseptic mix homogeneously, extracts 10ml, adds the aseptic pH7.0 sodium chloride-peptone buffer agent of 90ml, mixing.Take 10ml to filter, then rinse with sodium chloride-peptone buffer agent, 500ml/ film.Aseptic taking-up filter membrane, faces up and is affixed on Nutrient agar and Rose Bengal Sodium agar surface, covers pottery FE Tiler, puts into calorstat and cultivates.Nutrient agar puts into 35 DEG C of cultivations, and Rose Bengal Sodium agar is put into (25 DEG C) under room temperature and cultivated, and observes the growing state of bacterium colony in each culture dish.
The SHUANGHUANGLIAN KOUFUYE of table 1 present invention obtains preparation with additive method and compares
Conclusion:, content identical in each medical material ratio is suitable, (every milliliter containing 1.5g primary crude drug, and Radix Scutellariae, Flos Lonicerae, Fructus Forsythiae ratio are 1: 1: 2), utilize the time that the method for the present invention is extracted used by SHUANGHUANGLIAN KOUFUYE comparatively short, be only 2-3 days.And this method utilizes extract at low temperature, concentration, Radix Scutellariae extracting solution adopts chitosan precipitation, carries out high speed centrifugation and filtering with microporous membrane processes before fill, and obtained medicinal liquid clarity is higher, and stability is higher, and the content of 3 kinds of effective ingredient is above official method.Sample is after autoclaving, and without bacterial growth, after adding carbomer, the growth and breeding of fungus is suppressed, hence it is evident that less than pharmacopeia matched group, and after official method addition carbomer, fungus colony number significantly reduces.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.

Claims (5)

1. the preparation method of a 'Shuang Hualian ' for animals, it is characterised in that comprise the following steps:
1) Radix Scutellariae is added in traditional Chinese herbs by thermal reflux low-temperature extracting tank, add the water of 10-15 times, control pressure 40-50Kpa, soak 30-60min and make medical material drench;At temperature 60-80 DEG C, extract 6-8 time, each 20-30min, until extracting solution is substantially colorless, extracts whole extracting solution out to concentration tank, control temperature 50-70 DEG C and be concentrated into the clear paste that proportion is 1.05-1.10, regulate pH value to 5.0-6.0 with sodium hydroxide, add the 0.5%-2% volume chitosan of total measurement (volume), stir, stand 12h, filter, take supernatant, with salt acid for adjusting pH value to 1.5-2.0,80 DEG C of insulation 1h, standing 3-5h, taking precipitation, to be washed to pH value be 5.0, and continuation 70%-75% ethanol is washed till pH value 7.0, dry, obtain Radix Scutellariae extract;
2) extracting honeysuckle, pulverizes, adds the water of 4-6 times by Flos Lonicerae weight, add 0.5%-1% volume cellulase by the amount of solvent volume 50%-100%, regulate temperature and be 35-40 DEG C, enzymolysis 3-4h, raise temperature to 70-80 DEG C, maintain 20-30min, make enzyme-deactivating;
3) take Fructus Forsythiae, with step 2) process after Flos Lonicerae together with add in extraction pot, add dry weight 12-15 times of weight of medical material water, in control tank, temperature 60-80 DEG C carries out extract at low temperature, extracts 6-8 time, each 20-30min, filter, be concentrated into the clear paste that proportion is 1.2-1.3 at temperature 60-70 DEG C, when being cooled to 40 DEG C, be slowly added to ethanol, alcohol content is made to reach 75%, it is sufficiently stirred for, stands 12h, leaching supernatant, reclaim ethanol to without alcohol taste, obtaining the extract of Flos Lonicerae, Fructus Forsythiae;
4) taking Radix Scutellariae extract, the hot sodium hydroxide with 10% dissolves, and adds carbomer by the amount of cumulative volume 0.2%-0.8%, stir, mix with Fructus Forsythiae, Flos Lonicerae extract, regulate pH value 7.0, stirring, 4-8 DEG C of cold preservation 24h, filter, adding water to scale, correction pH value also adds water to scale, 8000-10000r/min high speed centrifugation, the filtering with microporous membrane in 0.6-0.8 μm of aperture, fill, sterilizing, obtain 'Shuang Hualian '
Wherein, the active component of described 'Shuang Hualian ' is Radix Scutellariae 20%-25% weight, Flos Lonicerae 20%-25% weight, Fructus Forsythiae 50%-60% weight;Wherein, active component presses primary crude drug calculating.
2. the preparation method of 'Shuang Hualian ' according to claim 1, it is characterised in that described carbomer940 content is 0.2%-0.5% volume.
3. the 'Shuang Hualian ' for animals that prepared by a preparation method according to claim 1, it is characterised in that being made up of active component and adjuvant, wherein, active component is Radix Scutellariae 20%-25% weight, Flos Lonicerae 20%-25% weight, Fructus Forsythiae 50%-60% weight;Adjuvant contains the carbomer940 of 0.2%-0.8% volume;Wherein, active component presses primary crude drug calculating.
4. 'Shuang Hualian ' according to claim 3, it is characterised in that described preparation is oral liquid.
5. the application of the 'Shuang Hualian ' according to any one of claim 3-4, it is characterised in that be applicable to prepare veterinary drug antibacterial, antiviral, raising immunity of organisms aspect.
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