CN101628077B - Preparation method of concentrated type heat-clearing and detoxicating oral liquid - Google Patents
Preparation method of concentrated type heat-clearing and detoxicating oral liquid Download PDFInfo
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- CN101628077B CN101628077B CN2009100658496A CN200910065849A CN101628077B CN 101628077 B CN101628077 B CN 101628077B CN 2009100658496 A CN2009100658496 A CN 2009100658496A CN 200910065849 A CN200910065849 A CN 200910065849A CN 101628077 B CN101628077 B CN 101628077B
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Abstract
The invention relates to a preparation method of concentrated type heat-clearing and detoxicating oral liquid. The preparation contains twelve medicinal materials of gypsum, honeysuckle, figwort, rehmannia root, weeping forsythia, gardenia, herba gueldenstaedtiae, baikal skullcap root, rough gentian, radix isatidis, rhizoma anemarrhenae and ophiopogon root. When being prepared, an ultrasonic extraction method, a chitosan flocculation method for impurity removal and a microwave sterilization technology are adopted, so that the effective components of the medicinal materials are extracted completely, the medicine concentration is increased, and the content of the effective components is enhanced; the production efficiency is enhanced, and the production cost is lowered. As the effective concentration in the unit volume of the medicine in the invention is doubled, the oral dosage of the medicine is correspondingly reduced, taking and carrying can be more convenient, wrapping materials are saved, and the invention is beneficial to environmental protection.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, be specifically related to a kind of preparation method of concentrated type heat-clearing and detoxicating oral liquid.
Background technology
QINGRE JIEDU KOUFUYE is by Gypsum Fibrosum, Flos Lonicerae, Radix Scrophulariae, Radix Rehmanniae, Fructus Forsythiae, Fructus Gardeniae, Herba Gueldenstaedtiae, Radix Scutellariae, Radix Gentianae, Radix Isatidis, the Rhizoma Anemarrhenae, the refining extract oral liquid preparation that forms of 12 flavor medicinal material extract Radix Ophiopogonis, has the function of heat-clearing and toxic substances removing.Be used for heating flushed complexion, fidgety thirsty, laryngopharynx swelling and pain due to the hyperactivity of toxic heat; Influenza, upper respiratory tract infection are seen above-mentioned patient.Clinical usefulness should be wide, and good effect has no side effect, and is subjected to the welcome of extensive patients deeply.
In " preparation method of the QINGRE JIEDU KOUFUYE of recording in the Chinese pharmacopoeia: Gypsum Fibrosum of version in 2005, Flos Lonicerae, Radix Scrophulariae, Radix Rehmanniae, Fructus Forsythiae, Fructus Gardeniae, Herba Gueldenstaedtiae, Radix Scutellariae, Radix Gentianae, Radix Isatidis, the Rhizoma Anemarrhenae, Radix Ophiopogonis, remove Flos Lonicerae, outside the Radix Scutellariae, ten flavors such as all the other Gypsum Fibrosum add water temperature earlier and soaked 1 hour, decoct secondary (after waiting to seethe with excitement, cold rnning Flos Lonicerae and Radix Scutellariae slightly), 1 hour for the first time, 40 minutes for the second time, filter, merging filtrate, filtrate is concentrated into relative density and is about 1.17 (80 ℃), adds ethanol, makes to contain the alcohol amount and reach 65%～70%, cold preservation 48 hours, filter, reclaim ethanol, it is an amount of to add correctives, add activated carbon 5g, heated 30 minutes, and filtered, add water to full dose, filter, embedding, sterilization, promptly.The decocting that this process using is traditional boils the precipitate with ethanol preparation method, traditional water boiling and extraction method, and the active ingredient of medical material is extracted not exclusively intact, the impurity content height, the medical material utilization rate is low, and energy consumption is big; The precipitate with ethanol remove impurity, the ethanol consumption is big, and production security is poor, and the production cycle is long, the cost height; Conventional free flowing steam sterilization, sterilization time is 20-35 minute, the active ingredient chlorogenic acid that can make Flos Lonicerae makes it content and reduces because of the heated time portion of growing up destroys.In a word, the oral liquid concentration that the method is produced is low, and effective component content is low, so that each consumption is strengthened, is not easy to take and carry.
The preparation method of the concentrated type heat-clearing and detoxicating oral liquid of Chinese patent Granted publication CN100506261C, be " to adopt the doughnut membrane material to filter in the last filtration technology of the preparation method of a middle QINGRE JIEDU KOUFUYE of Chinese pharmacopoeia version in 2005, this technological operation is loaded down with trivial details, particularly slow to the rate of filtration that contains the excessive concentrated type heat-clearing and detoxicating oral liquid of medical material, length consuming time, production efficiency is low.
The disclosed publication number of Chinese patent is the preparation technology of CN101406617A QINGRE JIEDU KOUFUYE, what still adopt is that traditional water decocts extraction process, extract the gained medicinal liquid with the aperture be the supermicro filtration membrane of 20-200nm filter clear liquid, after concentrating, clear liquid adds water and correctives is mixed with medicinal liquid, carry out the secondary supermicro filtration membrane again and filter, realized not having alcoholization and produced.But it still exists (1) medicinal material extract incomplete, and active constituent content is low; (2) feasible to containing the less relatively plain edition QINGRE JIEDU KOUFUYE of medical material amount, to containing the medical material amount is that the QINGRE JIEDU KOUFUYE (concentrated type) of one times of plain edition is infeasible, because of final preparation back medicinal liquid is denseer, adopt ultrafiltration to have filtration difficulty, the shortcoming that the rate of filtration is slow.
Summary of the invention
The present invention seeks to the deficiency that exists in the above-mentioned existing product production technology, adopt ultrasonic extraction, the remove impurity of flocculate with chitosan method and microwave sterilizating technology, the preparation method that a kind of effective raising drug level and active constituent content height is provided, curative effect is more significant and can makes the little nothing alcoholization of its dose produce concentrated type heat-clearing and detoxicating oral liquid.This preparation method also has the production efficiency height, power consumption is little, cost is low, and constant product quality is good.
Purpose of the present invention can be achieved through the following technical solutions:
Concentrated type heat-clearing and detoxicating oral liquid of the present invention comprises following weight percentages: wherein Gypsum Fibrosum 42-48%, Flos Lonicerae 8-10%, Radix Scrophulariae 6-8%, Radix Rehmanniae 5-7%, Fructus Forsythiae 4-5%, Fructus Gardeniae 4-5%, Herba Gueldenstaedtiae 4-5%, Radix Scutellariae 4-5%, Radix Gentianae 4-5%, Radix Isatidis 4-5%, Rhizoma Anemarrhenae 3-4%, Radix Ophiopogonis 3-4%;
Described preparation method comprises the steps:
(a) get by weight percentage: Gypsum Fibrosum 42-48%, Radix Scrophulariae 6-8%, Radix Rehmanniae 5-7%, Fructus Forsythiae 4-5%, Fructus Gardeniae 4-5%, Herba Gueldenstaedtiae 4-5%, Radix Gentianae 4-5%, Radix Isatidis 4-5%, Rhizoma Anemarrhenae 3-4%, Radix Ophiopogonis 3-4%, the water that the 10-14 of adding said medicine raw material weight sum doubly measures, after heating is waited to seethe with excitement, stop heating, treat to add Flos Lonicerae 8-10%, Radix Scutellariae 4-5% after temperature is reduced to below the boiling point, the supersound extraction secondary, each 20-40min, filter, merging filtrate, it is 1.05-1.10 that filtrate decompression is concentrated into relative density, must extract concentrated solution; Described relative density is to record under 60 ℃ of conditions;
(b) extract a step gained concentrated solution adds concentration 0.1% under 50-70 ℃ of condition flocculate with chitosan clarifier, make that chitosan-containing reaches 0.07-0.13% in the medicinal liquid, stirred about 20 minutes, placed about 24 hours, get supernatant and filter, it is 1.18 concentrated solution that filtrate decompression is concentrated into relative density, add concentrated solution weight 2-3 pure water doubly, cold preservation 24 hours, high speed centrifugation, centrifugal liquid adds correctives, adds water afterwards and makes the medicinal liquid total amount; Described medicinal liquid total amount is a step 1/3rd of the raw material weight percent sum of getting it filled, mixing, embedding; Described relative density is to record under 80 ℃ of conditions;
(c) adopt microwave sterilizating, sterilized 3-5 minute, promptly.
Supersound extraction described in a step is to carry out under the condition of frequency 20-80KHz, power 15-20kW.
Relative density after filtrate decompression described in a step concentrates also can be about 1: 1 of percentage by weight sum of medicinal liquid weight and described each raw material.
The frequency of the microwave sterilizating described in the c step is that 12-15Hz, power are 3-6KW.
Described correctives is a kind of among disodium glycyrrhizinate, acesulfame potassium (acesulfame potassium), mogroside or the neohesperidin DC, and its addition is for for making the 0.002-2% of medicinal liquid total amount.
Beneficial effect of the present invention is as follows:
One, because the present invention adopts ultrasound wave to extract, its advantage is as follows compared to existing technology:
(1) need not high temperature, ultrasonic extraction in 40 ℃ of-50 ℃ of water temperatures does not destroy that some has thermally labile in the medical material, and the efficacy component of facile hydrolysis improves the curative effect of product;
(2) extraction efficiency height extracts and can obtain the optimum extraction rate in 20～40 minutes;
(3) less energy consumption, the supersound extraction heating-up temperature is low, and extraction time is short, therefore cuts down the consumption of energy greatly.
(4) extraction impurity is few, and effective ingredient is easy to separate, purify.
Two, because the present invention adopts the remove impurity of flocculate with chitosan method, with commonly used alcohol deposition method, membrane filter method mutually specific energy make the water extract clear and bright better, and keep effective ingredient, guarantee stability of formulation, and can enhance productivity, shorten the production cycle, reduce cost; This technology has been avoided use ethanol simultaneously, realizes not having alcoholization and produces, and makes production safer.
Three, because the present invention adopts the microwave sterilizating technology, to compare with moist heat sterilization commonly used, sterilization time is short, only needs 3-5 minute, the production efficiency height, and can guarantee in the product that thermally labile active ingredient chlorogenic acid etc. is not destroyed, and guarantees product quality and stability.
Specific embodiments
The present invention is further described below with reference to embodiment, but this should be interpreted as that scope of the present invention only limits to following example.All technology that realizes based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1:
(a) get by weight percentage: Gypsum Fibrosum 42.83%, Radix Scrophulariae 7.90%, Radix Rehmanniae 6.10%, Fructus Forsythiae 4.29%, Fructus Gardeniae 4.29%, Herba Gueldenstaedtiae 4.29%, Radix Gentianae 4.29%, Radix Isatidis 4.29%, the Rhizoma Anemarrhenae 3.45%, Radix Ophiopogonis 3.45%, the water that adds 10 times of amounts of said medicine raw material weight sum, after heating is waited to seethe with excitement, stop heating, treat to add Flos Lonicerae 9.82% after temperature is reduced to below the boiling point, Radix Scutellariae 5.00%, supersound extraction (frequency 25KHz, power 20kW) secondary, each 20min, filter, it is 1.05-1.10 (60 ℃ of surveys) that merging filtrate, filtrate decompression are concentrated into relative density, must extract concentrated solution.
(b) extract a step gained concentrated solution adds concentration 0.1% under 60 ℃ of conditions flocculate with chitosan clarifier, make that chitosan-containing reaches 0.10% in the medicinal liquid, stirred 20 minutes, placed 24 hours, get supernatant and filter, it is 1.18 concentrated solution (80 ℃ of surveys) that filtrate decompression is concentrated into relative density, the pure water that adds 2 times of concentrated solution weight, cold preservation 24 hours, high speed centrifugation, centrifugal liquid add the disodium glycyrrhizinate correctives (addition be make the medicinal liquid full dose 0.4%), add water afterwards and make the medicinal liquid total amount; Described medicinal liquid total amount is a step 1/3rd of the raw material weight percent sum of getting it filled, mixing, embedding.
(c) microwave sterilizating (frequency 15Hz, power 5KW) is adopted in sterilization, sterilizes 3 minutes, promptly.
Embodiment 2:
(a) get by weight percentage: Gypsum Fibrosum 44.64%, Radix Scrophulariae 7.13%, Radix Rehmanniae 5.33%, Fructus Forsythiae 4.46%, Fructus Gardeniae 4.46%, Herba Gueldenstaedtiae 4.46%, Radix Gentianae 4.46%, Radix Isatidis 4.46%, the Rhizoma Anemarrhenae 3.60%, Radix Ophiopogonis 3.60%, the water that adds 12 times of amounts of said medicine raw material weight sum, after heating is waited to seethe with excitement, stop heating, treat to add Flos Lonicerae 8.93% after temperature is reduced to below the boiling point, Radix Scutellariae 4.47%, supersound extraction (frequency 40KHz, power 15kW) secondary, each 30min, filter, merging filtrate, filtrate decompression are concentrated into about 1: 1 of percentage by weight sum of medicinal liquid weight and described each raw material, must extract concentrated solution.
(b) extract concentrated solution adds concentration 0.1% under 55 ℃ of conditions flocculate with chitosan clarifier, make that chitosan-containing reaches 0.11% in the medicinal liquid, stirred 20 minutes, placed 24 hours, get supernatant and filter, it is 1.18 concentrated solution (80 ℃ of surveys) that filtrate decompression is concentrated into relative density, the pure water that adds 2.5 times of concentrated solution weight, cold preservation 24 hours, high speed centrifugation, centrifugal liquid add the mogroside correctives (addition be make the medicinal liquid full dose 1.8%), add water afterwards and make the medicinal liquid total amount; Described medicinal liquid total amount is a step 1/3rd of the raw material weight percent sum of getting it filled, mixing, embedding.
(c) microwave sterilizating (frequency 13Hz, power 6KW) is adopted in sterilization, sterilizes 4 minutes, promptly.
Embodiment 3:
(a) get by weight percentage: Gypsum Fibrosum 45.10%, Radix Scrophulariae 6.00%, Radix Rehmanniae 6.50%, Fructus Forsythiae 4.60%, Fructus Gardeniae 4.60%, Herba Gueldenstaedtiae 4.60%, Radix Gentianae 4.60%, Radix Isatidis 4.60%, the Rhizoma Anemarrhenae 3.70%, Radix Ophiopogonis 3.70%, the water that adds 14 times of amounts of said medicine raw material weight sum, after heating is waited to seethe with excitement, stop heating, treat to add Flos Lonicerae 8.00% after temperature is reduced to below the boiling point, Radix Scutellariae 4.00%, supersound extraction (frequency 75KHz, power 17kW) secondary, each 40min, filter, merging filtrate, it is 1.05-1.10 (60 ℃ of surveys) that filtrate decompression is concentrated into relative density, or be concentrated into about 1: 1 of percentage by weight sum of medicinal liquid weight and described each raw material, and must extract concentrated solution, must extract concentrated solution.
(b) extract concentrated solution adds concentration 0.1% under 70 ℃ of conditions flocculate with chitosan clarifier, make that chitosan-containing reaches 0.13% in the medicinal liquid, stirred 20 minutes, placed 24 hours, get supernatant and filter, it is 1.18 concentrated solution (80 ℃ of surveys) that filtrate decompression is concentrated into relative density, the pure water that adds 3 times of concentrated solution weight, cold preservation 24 hours, high speed centrifugation, centrifugal liquid add neohesperidin DC correctives (addition be make the medicinal liquid full dose 0.0025%), add water afterwards and make the medicinal liquid total amount; Described medicinal liquid total amount is a step 1/3rd of the raw material weight percent sum of getting it filled, mixing, embedding.
(c) microwave sterilizating (frequency 12Hz, power 3KW) is adopted in sterilization, sterilizes 5 minutes, promptly.
The oral liquid of the present invention preparation is with " product that contains identical medical material amount that the method for making that Chinese pharmacopoeia version in 2005 is an one makes is compared, and quality is significantly increased.
Contain Radix Scutellariae in the oral liquid of the present invention's preparation and count 2.5-3.0mg/ml with baicalin, contain Flos Lonicerae and count 2.0-2.5mg/ml with chlorogenic acid, contain Radix Scutellariae in the oral liquid of existing prepared and count 2.1-2.5mg/ml, contain Flos Lonicerae and count 1.6-1.8mg/ml with chlorogenic acid with baicalin.
Claims (5)
1. the preparation method of a concentrated type heat-clearing and detoxicating oral liquid, comprise following weight percentages in the preparation: wherein Gypsum Fibrosum 42-48%, Flos Lonicerae 8-10%, Radix Scrophulariae 6-8%, Radix Rehmanniae 5-7%, Fructus Forsythiae 4-5%, Fructus Gardeniae 4-5%, Herba Gueldenstaedtiae 4-5%, Radix Scutellariae 4-5%, Radix Gentianae 4-5%, Radix Isatidis 4-5%, Rhizoma Anemarrhenae 3-4%, Radix Ophiopogonis 3-4%, it is characterized in that: described preparation method comprises the steps:
(a) get by weight percentage: Gypsum Fibrosum 42-48%, Radix Scrophulariae 6-8%, Radix Rehmanniae 5-7%, Fructus Forsythiae 4-5%, Fructus Gardeniae 4-5%, Herba Gueldenstaedtiae 4-5%, Radix Gentianae 4-5%, Radix Isatidis 4-5%, Rhizoma Anemarrhenae 3-4%, Radix Ophiopogonis 3-4%, the water that the 10-14 of adding said medicine raw material weight sum doubly measures, after heating is waited to seethe with excitement, stop heating, treat to add Flos Lonicerae 8-10%, Radix Scutellariae 4-5% after temperature is reduced to below the boiling point, the supersound extraction secondary, each 20-40min, filter, merging filtrate, it is 1.05-1.10 that filtrate decompression is concentrated into relative density, must extract concentrated solution; Described relative density is to record under 60 ℃ of conditions;
(b) extracting a step gained concentrated solution, to add concentration under 50-70 ℃ of condition be 0.1% flocculate with chitosan clarifier, make that chitosan-containing reaches 0.07-0.13% in the medicinal liquid, stirred 20 minutes, placed 24 hours, get supernatant and filter, it is 1.18 concentrated solution that filtrate decompression is concentrated into relative density, add concentrated solution weight 2-3 pure water doubly, cold preservation 24 hours, high speed centrifugation, centrifugal liquid adds correctives, adds water afterwards and makes the medicinal liquid total amount; Described medicinal liquid total amount is a step 1/3rd of the raw material weight percent sum of getting it filled, embedding; Described relative density is to record under 80 ℃ of conditions;
(c) adopt microwave sterilizating, sterilized 3-5 minute, promptly.
2. preparation method according to claim 1 is characterized in that: the supersound extraction described in a step is to carry out under the condition of frequency 20-80KHz, power 15-20kW.
3. preparation method according to claim 1 is characterized in that: the relative density after the filtrate decompression described in a step concentrates is 1: 1 of weight sum of medicinal liquid weight and described each raw material.
4. preparation method according to claim 1 is characterized in that: the frequency of the microwave sterilizating described in the c step is that 12-15Hz, power are 3-6KW.
5. preparation method according to claim 1 is characterized in that: described correctives is a kind of among disodium glycyrrhizinate, acesulfame potassium, mogroside or the neohesperidin DC, and its addition is the 0.002-2% that makes the medicinal liquid total amount.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101879273B (en) * | 2010-07-07 | 2012-04-18 | 贾瑞飞 | Medicament for treating cold by enema method |
| CN102319354B (en) * | 2011-09-30 | 2013-04-03 | 江西三九药业有限公司 | Heat clearing and detoxication oral liquid, and preparation method thereof |
| CN103182024A (en) * | 2013-02-07 | 2013-07-03 | 洛阳市洛铜医院 | Medicine for treating wind-heat type common cold and preparation method thereof |
| CN103735831B (en) * | 2014-01-27 | 2016-06-22 | 吉林金复康药业有限公司 | The preparation method of QINGRE JIEDU KOUFUYE |
| CN105726929A (en) * | 2014-12-10 | 2016-07-06 | 瑞普（天津）生物药业有限公司 | Preparation method of heat clearing and detoxifying soluble powder |
| CN105341930B (en) * | 2015-12-03 | 2018-06-01 | 山东禹王制药有限公司 | A kind of throat-clearing throat-moistening oral liquid and its preparation process |
| CN105560813A (en) * | 2016-01-05 | 2016-05-11 | 成都富豪斯生物科技有限公司 | Oral drug for treating swollen and sore throat caused by excess toxic heat and preparation method thereof |
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