CN105726929A - Preparation method of heat clearing and detoxifying soluble powder - Google Patents

Preparation method of heat clearing and detoxifying soluble powder Download PDF

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Publication number
CN105726929A
CN105726929A CN201410763513.8A CN201410763513A CN105726929A CN 105726929 A CN105726929 A CN 105726929A CN 201410763513 A CN201410763513 A CN 201410763513A CN 105726929 A CN105726929 A CN 105726929A
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preparation
soluble powder
parts
radix
heat
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CN201410763513.8A
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彭江宁
李旭东
刘爱玲
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Tianjin Ringpu Bio Technology Co Ltd
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Tianjin Ringpu Bio Technology Co Ltd
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Abstract

The invention discloses a preparation method of heat clearing and detoxifying soluble powder. The soluble powder is prepared on the basis of a veterinary use preparation ''Summer-heat clearing mixture'' through dosage form change and technology optimization. The drug stability and practicability are improved by changing a liquid preparation into a solid preparation, and the storage and transport are easy. A preparation technology of traditional Chinese medicine soluble powder is optimized. Chitosan and sodium alginate are combined to remove insoluble components of precipitation, insoluble suspension particles, tannin and colloid in an extracted liquid. The water soluble property of the soluble powder is improved, the administration of drinking water is facilitated, and the practicality of the drug is enhanced. The heat clearing and detoxifying soluble powder prepared by the method has the high baicalin retention rate, good water soluble property and stable quality, and is easy to store and easy to transport. The method of the invention realizes alcohol-free production. The technology is simple. The production period is short. The equipment requirement is low, and the cost is low. The preparation method of the heat clearing and detoxifying soluble powder facilitates large scale popularization, exploitation and application.

Description

A kind of preparation method of heat-clearing and toxic substances removing soluble powder
Technical field
The invention belongs to technical field of veterinary medicine pharmacy, the preparation method being specifically related to a kind of heat-clearing and toxic substances removing soluble powder.
Background technology
nullThe prescription of " Chinese veterinary pharmacopoeia " version removing summer-heat mixture in 2010 is,Gypsum Fibrosum 670g,Flos Lonicerae 140g,Radix Scrophulariae 100g,Radix Scutellariae 80g,Radix Rehmanniae 80g,Fructus Forsythiae 70 parts,Fructus Gardeniae 70g,Radix Gentianae 60g,Herba Gueldenstaedtiae 60g,Radix Isatidis 60g,Rhizoma Anemarrhenae 60g,Radix Ophiopogonis 60g,Extracting method is: above 12 tastes,Except Flos Lonicerae、Outside Radix Scutellariae,All the other 10 tastes add water warm macerating 1 hour,Decoct 2 times again,Within 1st time 1 hour, (after decocting half an hour, add Flos Lonicerae、Radix Scutellariae),Decoct 40 minutes for 2nd time,Filter,Merging filtrate,Filtrate is concentrated into relative density and is about 1.17 (90 DEG C),Add ethanol,Alcohol content is made to reach 65%-70%,Cold preservation stands 48 hours,Filter,Filtrate recycling ethanol,Add water move to 1000ml,Fill,Sterilizing,Obtain.Removing summer-heat mixture has the effect of heat-clearing and toxic substances removing.For the microbial pyretic toxicity disease of avian Escherichia coli.Poultry farming is widely used, is deeply trusted by peasant household.But oral liquid formulations quality is unstable, being long placed in or low temperature is placed and very easily produced precipitation, liquid preparation not easily transports and stores simultaneously, significantly constrains the popularization of this medicine.And need to add substantial amounts of ethanol in extracting, ensure the clarification of solution.
Chinese medicine soluble powder preparation, for solid preparation, it is easy to uses and stores and transport.The preparation of current soluble powder, generally extracting, after concentration, adopt the method remove impurity of precipitate with ethanol, is reclaimed after ethanol spray drying again, is prepared dry powder.Alcohol precipitation process is consuming time, power consumption not only, and equipment requirements is harsh, considerably increases the production cost of medicine.
Summary of the invention
The preparation method that the invention provides a kind of heat-clearing and toxic substances removing soluble powder, prescription is by weight: 67 parts of Gypsum Fibrosum, Flos Lonicerae 14 parts, Radix Scrophulariae 10 parts, Radix Scutellariae 8 parts, Radix Rehmanniae 8 parts, Fructus Forsythiae 7 parts, Fructus Gardeniae 7 parts, Radix Gentianae 6 parts, Herba Gueldenstaedtiae 6 parts, Radix Isatidis 6 parts, the Rhizoma Anemarrhenae 6 parts, Radix Ophiopogonis 6 parts, extracting method is: above 12 tastes, except Flos Lonicerae, outside Radix Scutellariae, all the other 10 tastes add water warm macerating 1 hour, decoct 2 times again, within 1st time 1 hour, (after decocting half an hour, add Flos Lonicerae, Radix Scutellariae), decoct 40 minutes for 2nd time, filter, merging filtrate, described preparation method comprises the following steps:
(1) by the filtrate concentration after merging;
(2) in concentrated solution, under agitation add chitosan solution, stand 3h, filter;
(3) above-mentioned filtrate adds sodium alginate soln, stand 6h;
(4) filtering, it is 1.1~1.2 (80 DEG C) that filtrate is concentrated into relative density, spray drying;
(5) collect xeraphium, add auxiliary materials and mixing and get final product.
It is 10:1~5:1 (V/W (L/kg)) that described step (1) filtrate is concentrated into the ratio of medicine liquid volume and medical material gross weight.
The mass concentration of described step (2) chitosan solution is 1% (W/V), and adding volume is the 4%~10% of medicine liquid volume.
The temperature of described step (2) concentrated solution is 80 DEG C~60 DEG C.
The quality solubility of described step (3) sodium alginate soln is 1% (W/V), and addition is the 1/2 of chitosan solution volume.
Adjuvant described in step (5) is glucose, sucrose, lactose, soluble starch.
The invention has the beneficial effects as follows:
The basis of veterinary drug " removing summer-heat mixture " changes liquid preparation into solid preparation, improves stability and the practicality of medicine, it is easy to store and transport;Optimizing the preparation technology that Chinese medicine soluble powder is traditional, the insoluble compositions such as the precipitation in extracting solution, insoluble particle, tannin and colloid removed by associating chitosan with sodium alginate, improve the water solublity of soluble powder, facilitate drinking water administration simultaneously.And the inventive method achieves and produces without alcoholization, technique is simple, and with short production cycle, equipment requirements is low, with low cost, consumes energy relatively low, is beneficial to large-scale promotion, development and application.
Detailed description of the invention
Embodiment 1:
(1) weigh Gypsum Fibrosum 67kg, Flos Lonicerae 14kg, Radix Scrophulariae 10kg, Radix Rehmanniae 8kg, Fructus Forsythiae 7kg, Fructus Gardeniae 7kg, Herba Gueldenstaedtiae 6kg, Radix Scutellariae 8kg, Radix Gentianae 6kg, Radix Isatidis 6kg, Rhizoma Anemarrhenae 6kg, Radix Ophiopogonis 6kg totally ten two taste medical material;
(2) 12 taste more than, except Flos Lonicerae, Radix Scutellariae, all the other 10 tastes, add 1510L water soaking 1 hour, first time decocts 1 hour (adding Flos Lonicerae, Radix Scutellariae after decocting half an hour);Second time adds 1208L soak by water 40 minutes, filters, obtains extracting solution;
(3) united extraction liquid, is concentrated into 1510L;(4) in the concentrated solution of 80 DEG C, under agitation add 60.4L1% chitosan solution, stand 3h;
(5) filter, in filtrate, add 30.2L1% sodium alginate soln, stand 6h;
(6) filtering, it is 1.1 (80 DEG C) that filtrate is concentrated into relative density, spray drying;
(7) collect xeraphium, add cane sugar powder mixing, prepare every g heat-clearing and toxic substances removing soluble powder containing 1.51g raw medicinal herbs.
Embodiment 2:
(1) weigh Gypsum Fibrosum 67kg, Flos Lonicerae 14kg, Radix Scrophulariae 10kg, Radix Rehmanniae 8kg, Fructus Forsythiae 7kg, Fructus Gardeniae 7kg, Herba Gueldenstaedtiae 6kg, Radix Scutellariae 8kg, Radix Gentianae 6kg, Radix Isatidis 6kg, Rhizoma Anemarrhenae 6kg, Radix Ophiopogonis 6kg totally ten two taste medical material;
(2) 12 taste more than, except Flos Lonicerae, Radix Scutellariae, all the other 10 tastes, add 1510L water soaking 1 hour, first time decocts 1 hour (adding Flos Lonicerae, Radix Scutellariae after decocting half an hour);Second time adds 1208L soak by water 40 minutes, filters, obtains extracting solution;
(3) united extraction liquid, is concentrated into 755L;
(4) in the concentrated solution of 60 DEG C, under agitation add 75.5L1% chitosan solution, stand 3h;
(5) filter, in filtrate, add 37.75L1% sodium alginate soln, stand 6h;
(6) filtering, it is 1.2 (80 DEG C) that filtrate is concentrated into relative density, spray drying;
(7) collect xeraphium, add the mixing of glucose sugar, prepare every g heat-clearing and toxic substances removing soluble powder containing 1.51g raw medicinal herbs.
Embodiment 3:
(1) weigh Gypsum Fibrosum 67kg, Flos Lonicerae 14kg, Radix Scrophulariae 10kg, Radix Rehmanniae 8kg, Fructus Forsythiae 7kg, Fructus Gardeniae 7kg, Herba Gueldenstaedtiae 6kg, Radix Scutellariae 8kg, Radix Gentianae 6kg, Radix Isatidis 6kg, Rhizoma Anemarrhenae 6kg, Radix Ophiopogonis 6kg totally ten two taste medical material;
(2) 12 taste more than, except Flos Lonicerae, Radix Scutellariae, all the other 10 tastes, add 1510L water soaking 1 hour, first time decocts 1 hour (adding Flos Lonicerae, Radix Scutellariae after decocting half an hour);Second time adds 1208L soak by water 40 minutes, filters, obtains extracting solution;
(3) united extraction liquid, is concentrated into 1057L;
(4) in the concentrated solution of 60 DEG C, under agitation add 74L1% chitosan solution, stand 3h;
(5) filter, in filtrate, add 37L1% sodium alginate soln, stand 6h;
(6) filtering, it is 1.15 (80 DEG C) that filtrate is concentrated into relative density, spray drying;
(7) collect xeraphium, add lactose mixing, prepare every g heat-clearing and toxic substances removing soluble powder containing 1.51g raw medicinal herbs.
Embodiment 4: the removing summer-heat mixture prepared according to the method for " Chinese veterinary pharmacopoeia " version in 2010
(1) weigh Gypsum Fibrosum 67kg, Flos Lonicerae 14kg, Radix Scrophulariae 10kg, Radix Rehmanniae 8kg, Fructus Forsythiae 7kg, Fructus Gardeniae 7kg, Herba Gueldenstaedtiae 6kg, Radix Scutellariae 8kg, Radix Gentianae 6kg, Radix Isatidis 6kg, Rhizoma Anemarrhenae 6kg, Radix Ophiopogonis 6kg totally ten two taste medical material;
(2) 12 taste more than, except Flos Lonicerae, Radix Scutellariae, all the other 10 tastes, add 1510L water soaking 1 hour, first time decocts 1 hour (adding Flos Lonicerae, Radix Scutellariae after decocting half an hour);Second time adds 1208L soak by water 40 minutes, filters, obtains extracting solution;
(3) united extraction liquid, is concentrated into relative density 1.17 (90 DEG C);
(4) add ethanol, make alcohol content reach 65%~70%;
(5) cold preservation stands 48 hours, filters, filtrate recycling ethanol, adds water move to 100L, fill, sterilizing, prepares every ml removing summer-heat mixture containing 1.51g raw medicinal herbs.
Embodiment 5: the soluble powder prepared traditionally
(1) weigh Gypsum Fibrosum 67kg, Flos Lonicerae 14kg, Radix Scrophulariae 10kg, Radix Rehmanniae 8kg, Fructus Forsythiae 7kg, Fructus Gardeniae 7kg, Herba Gueldenstaedtiae 6kg, Radix Scutellariae 8kg, Radix Gentianae 6kg, Radix Isatidis 6kg, Rhizoma Anemarrhenae 6kg, Radix Ophiopogonis 6kg totally ten two taste medical material;
(2) 12 taste more than, except Flos Lonicerae, Radix Scutellariae, all the other 10 tastes, add 1510L water soaking 1 hour, first time decocts 1 hour (adding Flos Lonicerae, Radix Scutellariae after decocting half an hour);Second time adds 1208L soak by water 40 minutes, filters, obtains extracting solution;
(3) united extraction liquid, is concentrated into relative density 1.17 (90 DEG C);
(4) add ethanol, make alcohol content reach 65%~70%;
(5) cold preservation stands 48 hours, filters, filtrate recycling ethanol;
(6) adjust filtrate relative density to 1.15 (80 DEG C), spray drying;(7) collect xeraphium, add soluble starch mixing, prepare every g heat-clearing and toxic substances removing soluble powder containing 1.51g raw medicinal herbs.
Embodiment 6: stability experiment
Taking the sample of above-described embodiment 1~5 preparation, be placed in 60 DEG C and accelerate 10 days, observe appearance character, and pH value, content of baicalin, chlorogenic acid content are detected after taking-up, experimental result is in Table 1.
160 DEG C of Acceleration study results of table
Experimental result shows, the pH value of liquid preparation is all unstable with chlorogenic acid, and the content of baicalin of embodiment 5 (alcohol precipitation process) is substantially less than embodiment 1~3 with chlorogenic acid content simultaneously.
Embodiment 7: the therapeutic effect experiment of the heat toxin syndrome that escherichia coli are caused
Select Tangshan city 3360 colibacillary white meat-type chickens of naturally-occurring of chicken house, it is classified as embodiment 2 medication therapy groups, removing summer-heat mixture treatment group, embodiment 5 medication therapy groups, often organize each 1120 chickens, embodiment 2 medicine presses 2.5g/L, removing summer-heat mixture by 2.5ml/L, embodiment 5 medicine by 2.5g/L drinking water administration, it is used in conjunction 5 days, observes the clinical efficacy experiment to 10 days.Experimental result is in Table 2.
The table 2 each medicine therapeutic effect to chicken colibacillosis
Note:##P < 0.01,#P<0.05
Test result indicate that, the cure rate of embodiment 2 medicine group is significantly higher than removing summer-heat mixture group and embodiment 5 medicine group (P < 0.01).
From the experimental result of embodiment 6,7, we can reach a conclusion that the stability of the heat-clearing and toxic substances removing soluble powder (embodiment 1~3) prepared with preparation method provided by the invention is higher than liquid preparation removing summer-heat mixture and the soluble powder (embodiment 5) prepared with traditional handicraft higher than the content of liquid preparation removing summer-heat mixture (embodiment 4), baicalin and chlorogenic acid.Simultaneously on clinical efficacy, under Isodose, the soluble powder that the cure rate of the heat-clearing and toxic substances removing soluble powder prepared with preparation method provided by the invention is significantly higher than liquid preparation and traditional handicraft prepares.And the method for the present invention, low for equipment requirements, environmental pollution is little, and step is simple, effective ingredient retention rate is high, with short production cycle, energy consumption is low, is beneficial to popularization, development and application.

Claims (6)

1. the preparation method of a heat-clearing and toxic substances removing soluble powder, prescription is by weight: 67 parts of Gypsum Fibrosum, Flos Lonicerae 14 parts, Radix Scrophulariae 10 parts, Radix Scutellariae 8 parts, Radix Rehmanniae 8 parts, Fructus Forsythiae 7 parts, Fructus Gardeniae 7 parts, Radix Gentianae 6 parts, Herba Gueldenstaedtiae 6 parts, Radix Isatidis 6 parts, the Rhizoma Anemarrhenae 6 parts, Radix Ophiopogonis 6 parts, extracting method is: above 12 tastes, except Flos Lonicerae, outside Radix Scutellariae, all the other 10 tastes add water warm macerating 1 hour, decoct 2 times again, within 1st time 1 hour, (after decocting half an hour, add Flos Lonicerae, Radix Scutellariae), decoct 40 minutes for 2nd time, filter, merging filtrate, it is characterized in that its preparation method comprises the following steps:
(1) by the filtrate concentration after merging;
(2) in concentrated solution, under agitation add chitosan solution, stand 3h, filter;
(3) above-mentioned filtrate adds sodium alginate soln, stand 6h;
(4) filtering, it is 1.1~1.2 (80 DEG C) that filtrate is concentrated into relative density, spray drying;
(5) collect xeraphium, add auxiliary materials and mixing and get final product.
2. the preparation method of a kind of heat-clearing and toxic substances removing soluble powder as claimed in claim 1, is characterized in that, the described filtrate concentration volume of step (1) is the ratio 10:1~5:1 to medicine liquid volume with medical material gross weight.
3. the preparation method of a kind of heat-clearing and toxic substances removing soluble powder as claimed in claim 1, is characterized in that, the mass concentration of described step (2) chitosan solution is 1%, and addition is the 4%~10% of medicine liquid volume.
4. the preparation method of a kind of heat-clearing and toxic substances removing soluble powder as claimed in claim 1 is characterized in that, in described step (2), the temperature of concentrated solution is 80 DEG C~60 DEG C.
5. the preparation method of a kind of heat-clearing and toxic substances removing soluble powder as claimed in claim 1, is characterized in that, in described step (3), the quality solubility of sodium alginate soln is 1%, and addition is the 1/2 of chitosan solution volume.
6. the preparation method of a kind of heat-clearing and toxic substances removing soluble powder as claimed in claim 1 is characterized in that, adjuvant described in step (5) is glucose, sucrose, lactose, soluble starch.
CN201410763513.8A 2014-12-10 2014-12-10 Preparation method of heat clearing and detoxifying soluble powder Pending CN105726929A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106110119A (en) * 2016-07-18 2016-11-16 安徽奥力欣生物科技有限公司 A kind of antipyretic and detoxicated oral liquid for animals and preparation method thereof

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106110119A (en) * 2016-07-18 2016-11-16 安徽奥力欣生物科技有限公司 A kind of antipyretic and detoxicated oral liquid for animals and preparation method thereof

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Application publication date: 20160706