CN102018810B - Preparation method of compound Houttuynia cordata mixture - Google Patents

Preparation method of compound Houttuynia cordata mixture Download PDF

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CN102018810B
CN102018810B CN2010105791241A CN201010579124A CN102018810B CN 102018810 B CN102018810 B CN 102018810B CN 2010105791241 A CN2010105791241 A CN 2010105791241A CN 201010579124 A CN201010579124 A CN 201010579124A CN 102018810 B CN102018810 B CN 102018810B
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houttuynia cordata
ethanol
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江崇波
马全民
郑猛
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ZHEJIANG HUISONG PHARMACEUTICALS CO Ltd
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Abstract

The invention belongs to the technical field of traditional Chinese medicine, and relates to a preparation method of compound Houttuynia cordata preparation, in particular to a preparation method of compound Houttuynia cordata mixture for the treatment of sore throat and tonsillitis caused by exogenous wind heat and a preparation method of the mixture. In the preparation method of the compound Houttuynia cordata mixture, the Houttuynia cordata, Scutellaria baicalensis, isatis root, fructus forsythiae and honeysuckle which are used as bulk drug and prepared with auxiliary materials, the method comprises the following steps: extracting, filtering, concentrating and preparing the mixture, wherein the extraction step refers to distill the Houttuynia cordata, fructus forsythiae and honeysuckle with steam in advance and extract aromatic water, then, water is added to decoct drug residues, filtering is performed, and the obtained decoction liquid is mixed with the decoction liquid of the Scutellaria baicalensis and the isatis root, and the mixed liquid is filtered and concentrated. The preparation method of compound Houttuynia cordata mixture can fully use volatile components, which have functions of cooling, eliminating pathogens and removing wind heat, of the Houttuynia cordata, the fructus forsythiae and the honeysuckle, so that alcoholicity of alcohol precipitation process is lowered, and loss of components having functions of clearing heat and detoxicating in the formula is reduced.

Description

A kind of method for preparing of compound houttuynin mixture
Technical field
The invention belongs to technical field of Chinese medicines, relate to a kind of method for preparing of Herba Houttuyniae preparation, specifically a kind of be used for that affection due to external wind and heat causes have sore throat, the method for preparing of tonsillitic compound houttuynin mixture, the invention still further relates to the method for preparing of this mixture.
Background technology
Upper respiratory tract infection is commonly encountered diseases, frequently-occurring disease.In recent years, because the mobile personnel is frequent, each mobile link orientation is ineffective, and sickness rate is on the rise.The upper respiratory tract infection four seasons all can take place, and see the propagation of Along with season property in You Yichun, winter more; Sickness rate concentrates on the thick place of crowd; And because of upper respiratory tract infection has certain infectiousness, very high at susceptible sickness rate in season, the oncoming force is more violent; The people threat not strong to child, old man and immunity of organisms is very big, people ' s health is produced with work also often brought considerable influence.
What upper respiratory tract infection caused has sore throat, and card such as tonsillitis belongs to the traditional Chinese medical science " external wind heat syndrome " category.Affection due to external wind and heat is that heresy just disaccords by the heresy of wind heat invasion and attack flesh table, and battalion defends and becomes estranged, the excess of YANG in outside and cause a disease." warm opinion " pointed out: " warm pathogen tend to attack the upper orifices, attacking the lung first ".Wind is first of the six climate exopathogens, the invasion of wind heat pathogenic factor, and the lunar lung of hands stands in the breach, as Ye Tianshi " 3 o'clock latent pathogen diseases caused by exogenous pathogenic factor pieces of writing " opinion " the lung position is the highest, and heresy must be hindered earlier ".Heresy is attacked part of the body cavity above the diaphragm housing the heart and lungs lung and is defended, and lung governing qi belongs to be defended, and lung associating with skin and hair and unite and defend table to become estranged, and Lung Qi obstraction, pathological changes be from the beginning of promptly seeing heating, micro evil wind, and sweating is not smooth.Wind heat is violated table, and so vital QI resisting pathogen is heating.Wind-heat troubling is distending pain in the head then, and the heresy of wind heat is stifling cleans the street, so laryngopharynx swelling and pain, parched throat is thirsty, turbid nasal discharge.Disease sees that pharyngeal pharyngeal tonsils is high swollen and the root foot is brought together, and the surface is uneven, and is peony, and the little punctate opacity of the cornea of white or yellow-white appears in the affected part sometimes, or a yellow-white pus appearance membranoid substance is arranged, and is easy to wipe away brokenly, and is also not hemorrhage after wiping away.This moment treatment is when be crucial with eliminating evil, and is pointed like " pestilence opinion ": " exopathogen is expensive generally early controls, and takes advantage of people's QI and blood not disorderly, and muscle does not disappear, and body fluid does not consume, and patient is unlikely in great danger, throws that agent is unlikely keeps in check, also is prone to calm down after healing.Desire is completely safe plan person, but knows the place of heresy.Early take out old complaint " for wanting ear.So should be main with wind and heat dispersing, subduing swelling and detoxicating.In the side, Herba Houttuyniae, hot, be slightly cold, return lung meridian, the function heat-clearing and toxic substances removing, the evacuation of pus detumescence, with the pyretic toxicity of clear part of the body cavity above the diaphragm housing the heart and lungs edema caused by disorder of QI, consumption is solely heavy, is our monarch drug.Radix Scutellariae, bitter, cold, function heat clearing and damp drying, eliminating fire and detoxication.Radix Isatidis, bitter, cold, function heat-clearing and toxic substances removing, removing heat from blood sore-throat relieving.Last two flavors assist monarch drug to strengthen heat-clearing and toxic substances removing, and the removing heat from blood sore-throat relieving is ministerial drug.Flos Lonicerae, sweet, cold, function heat-clearing and toxic substances removing, dispelling wind-heat.Fructus Forsythiae, bitter, cold, function heat-clearing and toxic substances removing, Flos Lonicerae and Fructus Forsythiae are adjuvant drug altogether, the heresy that still can suffering except that effects for removing toxic heat is arranged cools completely, dispelling wind-heat share at medicine and to play heat-clearing and toxic substances removing altogether, and the merit of dispelling wind-heat is used for having sore throat tonsillitis due to the affection due to external wind and heat.
The shortcoming that the method for preparing of existing compound houttuynin preparation exists, 1. fail to utilize Herba Houttuyniae, Fructus Forsythiae and Flos Lonicerae contained have the suffering heresy that cools completely, a fragrant ingredient of dispelling wind-heat function.2. precipitate with ethanol operation alcohol content is too high, and the composition loss that has effects for removing toxic heat in the side of causing is too much.Disclose a kind of nano mixed heartleaf houttuynia herb preparation medicine and application number is the one Chinese patent application of CN01100711.7, it is with the nanometer Herba Houttuyniae, nano Radix Isatidis; The nanometer Radix Scutellariae, nanometer gold Flos Lonicerae, nanometer Fructus Forsythiae are raw material; New pharmaceutical preparation is processed in preparation in proportion, and its fineness of the particles reaches the 1200-1500 order; Particle diameter is 0.1-200nm, and wherein most particle diameters are less than 100nm, and has new rerum natura.Adopt steps such as microwave extracting, concentrating under reduced pressure, supersonic jet technology spray drying to process.The deficiency of this method is that used production equipment is unconventional equipment, costs an arm and a leg, and production cost is high, and product price will significantly improve, and causes the patient burden to increase the weight of.
Summary of the invention
The defective that the present invention is directed to prior art provides a kind of method for preparing of compound houttuynin mixture, this method to keep the functional component in the crude drug to greatest extent, has reduced production cost simultaneously.
Above-mentioned technical problem of the present invention is able to implement through following technical scheme:
A kind of method for preparing of compound houttuynin mixture; By Herba Houttuyniae, Radix Scutellariae, Radix Isatidis, Fructus Forsythiae, Flos Lonicerae is that crude drug adds the adjuvant preparation, and this method comprises extraction, filtration, concentrated, mixture preparation, and described extraction is after in advance Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae being extracted Aromatic water with vapor distillation; Medicinal residues are decocte with water again; Filter, the decoction liquor of decoction liquor that obtains and Radix Scutellariae, Radix Isatidis merges, and filters and concentrates.And prior art is that whole medical materials are together decocted, and fails to collect the contained fragrant ingredient of Herba Houttuyniae, Fructus Forsythiae and Flos Lonicerae.The present invention extracts earlier the fragrant ingredient of Herba Houttuyniae, Fructus Forsythiae and Flos Lonicerae, and then decocts, the suffering that the has improved product heresy that cools completely, dispelling wind-heat effect.The compound houttuynin mixture heat-clearing and toxic substances removing that the present invention makes, be used for that affection due to external wind and heat causes have sore throat tonsillitis.Compare with the compound houttuynin mixture that conventional method makes, functional component content is high, is example with the baicalin, and content has improved more than 3 times; Reduce dose, be reduced to each 1 by each 3.
Method for preparing of the present invention also comprises the precipitate with ethanol step, and specifically: get and concentrate the concentrated solution that obtains, add ethanol and make ethanol content reach 50~60 wt%, stir, leave standstill, get supernatant, continuing to be concentrated into relative density is 1.26~1.30.Ethanol content reaches 70% and compares during with the prior art precipitate with ethanol, has kept the water-soluble components that has heat-clearing toxin-expelling functions in Radix Scutellariae, Flos Lonicerae and the Fructus Forsythiae more.
As preferably, described supernatant reclaims ethanol in 65~70 ℃.Reduce because the too high destruction that functional component is caused of temperature.
As preferably, the decocting that described medicinal residues add 8~10 times of weight boiled 1~1.5 hour.As much as possible functional component is extracted fully.
As preferably; Described Radix Scutellariae, Radix Isatidis decocte with water twice, primary amount of water are Radix Scutellariae, Radix Isatidis gross weight 10~12 times, decoct 1.5~2 hours; Secondary amount of water is Radix Scutellariae, Radix Isatidis gross weight 8~10 times, decocts 1~1.5 hour.As much as possible functional component is extracted fully.
As preferably, the weight portion of described crude drug of the inventive method and adjuvant consists of: Herba Houttuyniae 245-250 part, Radix Scutellariae 63-65 part; Radix Isatidis 63-65 part, Fructus Forsythiae 25-28 part, Flos Lonicerae 25-28 part; Sucrose 60-62 part; Mel 200-210 part, sodium benzoate 2-3 part, ethyl hydroxybenzoate 0.5-0.6 part.This component is compared with existing component, can heighten the effect of a treatment to reduce dose simultaneously.
Active component houttuynine sodium bisulfite (decanoylacetaldehyde), methylnonanone, α-thujene, australene, linalool, eugenol etc. that the present invention contains Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae volatile oil propose earlier; Again water soluble ingredient phillyrin, Forsythinol glycosides, baicalin, ursolic acid, rutin, chlorogenic acid, isochlorogenic acid, indigo, indirubin, Isatis indigotica Fort. glycosides, cupreol, several amino acids etc. are passed through water boiling and extraction; After concentrating, adopt low precipitate with ethanol, reduce the too much loss of heat-clearing toxin-expelling functions composition as far as possible; Keep more effective ingredient; Therefore, this method has the functional component reservation fully, the advantage that reduces production costs simultaneously.
The compound houttuynin mixture heat-clearing and toxic substances removing that the present invention makes, be used for that affection due to external wind and heat causes have sore throat tonsillitis.Compare with the method for preparing of existing compound houttuynin preparation, the invention has the advantages that: 1. can make full use of Herba Houttuyniae, Fructus Forsythiae and Flos Lonicerae contained have the suffering heresy that cools completely, a volatile ingredient of dispelling wind-heat function.2. reduce the alcohol content of precipitate with ethanol operation, have the loss of the composition of effects for removing toxic heat in the minimizing side.3. active constituent content is higher, thinks the baicalin example, and content of baicalin is more than the 1.5mg/ml in the mixture that the present invention makes, and the prior preparation method content of baicalin is merely about 0.5mg/ml.
Through clinical research; The general curative effect result of the compound houttuynin mixture that the present invention makes is (240 example) as follows: clinical recovery 46 examples (19.2%), produce effects 97 examples (40.4%), effective 79 examples (32.9%), invalid 18 examples (7.5%); Total obvious effective rate 59.6%, total effective rate 92.5%.There is notable difference treatment back aspect symptoms such as pharyngalgia, pharyngeal dryness and heat, dysphagia, red swelling of the pharynx, thirsty, cough, heating, aversion to cold, nasal obstruction watery nasal discharge with before the treatment, explain that compound houttuynin mixture treatment Chinese medical discrimination of the present invention belongs to external wind heat syndrome and has significant curative effect.
The specific embodiment
It below is specific embodiment of the present invention; These embodiment can do further to replenish and explanation to the present invention; But the present invention is not limited to these embodiment.
Employed technology in following examples unless stated otherwise, is routine techniques known to those skilled in the art; Employed instrument and equipment, reagent etc., only this description specifies, what the research that is this area and technical staff can be through public approach acquisitions.
Table 1
Figure 2010105791241100002DEST_PATH_IMAGE002
Embodiment 1-3:
1. extract
Press the proportioning of table 1, Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae are added 10 times of amounts (weight, down together) water, extract Aromatic water 160ml device preservation in addition with vapor distillation, medicinal residues add 8 times of amount decoctions of water 1 hour, filter, and are subsequent use.Radix Scutellariae, Radix Isatidis decocte with water twice add 10 times of amounts of water for the first time, decoct 1.5 hours; For the second time add 8 times of amounts of water, decocted 1 hour.
2. filter, concentrate
Merge decoction liquor, natural subsidence was got supernatant more than 8 hours, and lower sediment is filtered with 100 mesh sieves, merging filtrate and supernatant.Get filtrate and carry out vacuum concentration in 70~80 ℃, being concentrated into relative density is 1.18-1.20.
3. precipitate with ethanol
Get concentrated solution, slowly add 85% ethanol, make to contain alcohol amount and reach 55wt%, stir, left standstill 24 hours.Slowly draw the precipitate with ethanol supernatant, discard deposition.Get supernatant and reclaim ethanol in 65~70 ℃, and continue to be concentrated into relative density and reach 1.26-1.30, obtain precipitate with ethanol extractum.
4. mixture preparation
1. water precipitating
Get the precipitate with ethanol extractum that a step obtains, add the purified water of 3 times of amounts, after stirring, left standstill 10 hours.Draw the water precipitating supernatant with siphonage.
2. dosing
Adjuvant (sucrose, Mel, sodium benzoate, ethyl hydroxybenzoate) in water intaking heavy supernatant, Aromatic water and the table 1 adds purified water to 1000ml, and under agitation heated and boiled stirred 15 minutes, was cooled to 30-40 ℃, transfers pH to 5.0 with citric acid or sodium citrate.
3. filter
Draw supernatant with siphonage, lower sediment is filtered the back with flannelette and is merged with supernatant, the inspection medicinal liquid clarity, and qualified back cold preservation is subsequent use.
5. packing: get cold preservation filtrating, loading amount is adjusted in 15-18ml.The inspection loading amount.
6. sterilization: set 100 ℃ of sterilising temps, sterilization time is 45 minutes.
The content of baicalin of the compound houttuynin mixture that embodiment 1,2,3 makes is respectively 1.78,1.63,1.92mg/ml.Existing product is with five common decocte with water twice of medical material, and each 2 hours, collecting decoction filtered, and filtrating is concentrated into the clear paste that relative density is 1.18~1.20 (60~80 ℃); Adding ethanol is 70% to containing the alcohol amount, stirs, and leaves standstill 24 hours, filters; Decompression filtrate recycling ethanol also is concentrated in right amount, dosing, and the adjustment total amount stirs to ormal weight; Filter, fill, sterilization, content of baicalin is 0.52-0.59mg/ml.
Embodiment 4:
Concrete scheme is with embodiment 1, and difference is first three step, and is specific as follows:
1. extract
Press the proportioning of table 1, Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae are added 12 times of water gagings, extract Aromatic water 200ml device preservation in addition with vapor distillation, medicinal residues add 10 times of water gagings and decocted 1 hour, filter, and are subsequent use.Radix Scutellariae, Radix Isatidis decocte with water twice add 12 times of water gagings for the first time, decoct 1.5 hours; For the second time add 10 times of water gagings, decocted 1 hour.
2. filter, concentrate
Merge decoction liquor, natural subsidence was got supernatant more than 8 hours, and lower sediment is filtered with 100 mesh sieves, merging filtrate and supernatant.Get filtrate and carry out vacuum concentration in 70 ℃, being concentrated into relative density is 1.18.
3. precipitate with ethanol
Get concentrated solution, slowly add 85% ethanol, make to contain alcohol amount and reach 60 wt%, stir, left standstill 24 hours.Slowly draw the precipitate with ethanol supernatant, discard deposition.Get supernatant and reclaim ethanol in 65~70 ℃, and continue to be concentrated into relative density and reach 1.26.
The content of baicalin of the compound houttuynin mixture that present embodiment makes is 2.15mg/ml.
Embodiment 5:
Concrete scheme is with embodiment 1, and difference is first three step, and is specific as follows:
1. extract
Press the proportioning of table 1, Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae are added 12 times of water gagings, extract Aromatic water 200ml device preservation in addition with vapor distillation, medicinal residues add 10 times of water gagings and decocted 1 hour, filter, and are subsequent use.Radix Scutellariae, Radix Isatidis decocte with water twice add 11 times of water gagings for the first time, decoct 1.5 hours; For the second time add 9 times of water gagings, decocted 1 hour.
2. filter, concentrate
Merge decoction liquor, natural subsidence was got supernatant more than 8 hours, and lower sediment is filtered with 100 mesh sieves, merging filtrate and supernatant.Get filtrate and carry out vacuum concentration in 80 ℃, being concentrated into relative density is 1.20.
3. precipitate with ethanol
Get concentrated solution, slowly add 85% ethanol, make to contain alcohol amount and reach 50 wt%, stir, left standstill 24 hours.Slowly draw the precipitate with ethanol supernatant, discard deposition.Get supernatant and reclaim ethanol in 65~70 ℃, and continue to be concentrated into relative density and reach 1.30.
The content of baicalin of the compound houttuynin mixture that present embodiment makes is 2.06mg/ml.
Specific embodiment described in the present invention only is that the present invention's spirit is illustrated.Person of ordinary skill in the field of the present invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.
Although the present invention has been made detailed explanation and has quoted some instantiations as proof, to those skilled in the art, only otherwise leave that the spirit and scope of the present invention can be done various variations or correction is obvious.

Claims (5)

1. the method for preparing of a compound houttuynin mixture is that crude drug adds the adjuvant preparation by Herba Houttuyniae, Radix Scutellariae, Radix Isatidis, Fructus Forsythiae, Flos Lonicerae, and this method comprises that extractions, filtrations, concentrated, precipitate with ethanol, mixture prepare, and it is characterized in that concrete grammar is following:
A, extraction: after in advance Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae being extracted Aromatic water with vapor distillation, medicinal residues are decocte with water again, filters, and the decoction liquor of decoction liquor that obtains and Radix Scutellariae, Radix Isatidis merges;
B, filtration and concentrated;
C, precipitate with ethanol: get and concentrate the concentrated solution that obtains, add ethanol and make ethanol content reach 50~60 wt%, stir, leave standstill, get supernatant, continuing to be concentrated into relative density is 1.26~1.30;
D, mixture preparation:
1. water precipitating is got the precipitate with ethanol extractum that a step obtains, and adds the water of 3 times of amounts, after stirring, leaves standstill 10 hours;
2. the heavy supernatant of dosing water intaking, Aromatic water and adjuvant add an amount of purified water, and under agitation heated and boiled stirs, and is cooled to 30-40 ℃, transfer pH to 5.0 with citric acid or sodium citrate;
3. filter with siphonage and draw supernatant, lower sediment is filtered the back with flannelette and is merged with supernatant, the inspection medicinal liquid clarity, and qualified back cold preservation is subsequent use.
2. method for preparing according to claim 1 is characterized in that: described supernatant reclaims ethanol in 65~70 ℃.
3. method for preparing according to claim 1 is characterized in that: the decocting that described medicinal residues add 8~10 times of weight boiled 1~1.5 hour.
4. method for preparing according to claim 1; It is characterized in that: twice of described Radix Scutellariae, Radix Isatidis decocte with water; Primary amount of water is Radix Scutellariae, Radix Isatidis gross weight 10~12 times; Decocted 1.5~2 hours, secondary amount of water is Radix Scutellariae, Radix Isatidis gross weight 8~10 times, decocts 1~1.5 hour.
5. according to each described method for preparing in the claim 1~4, it is characterized in that the weight portion of described crude drug and adjuvant consists of: Herba Houttuyniae 245-250 part, Radix Scutellariae 63-65 part; Radix Isatidis 63-65 part, Fructus Forsythiae 25-28 part, Flos Lonicerae 25-28 part; Sucrose 60-62 part; Mel 200-210 part, sodium benzoate 2-3 part, ethyl hydroxybenzoate 0.5-0.6 part.
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CN102429994B (en) * 2011-12-29 2013-09-18 浙江康恩贝中药有限公司 Compound heartleaf houttuynia herb mixture and preparation method thereof
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