CN100584318C - Sugar-free type red tangerine peel granular agent for treating productive cough - Google Patents
Sugar-free type red tangerine peel granular agent for treating productive cough Download PDFInfo
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- CN100584318C CN100584318C CN200610099306A CN200610099306A CN100584318C CN 100584318 C CN100584318 C CN 100584318C CN 200610099306 A CN200610099306 A CN 200610099306A CN 200610099306 A CN200610099306 A CN 200610099306A CN 100584318 C CN100584318 C CN 100584318C
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Abstract
The sugar-free red tangerine peel granule for treating productive cough is prepared with red tangerine peel, sessile stemona root, almond, white swallowwort, tuckahoe and other Chinese medicinal materials. It is used to treat cough, asthma with abundant phlegm, cold, bronchitis and laryngopharyngitis. The granule includes also supplementary material: dextrin, maltodextrin and corrective, which is selected from proteoglycan, sweetener and stevioside and is preferably stevioside.
Description
Technical field:
The present invention relates to a kind of activating QI to eliminate phlegm, the nourishing the lung to arrest cough granule particularly relates to the granule of being made up of flavour of a drug such as Exocarpium Citri Grandis, the Radix Stemonae, Semen Armeniacae Amarum, Rhizoma Cynanchi Stauntonii, Poria, Rhizoma Pinelliae Preparata, Fructus Schisandrae Chinensis, Radix Glycyrrhizaes, can be used for cough, asthma abundant expectoration clinically; Flu bronchitis, pharyngolaryngitis.
Background technology:
The product Juhong Tanke granule prescription that has gone on the market comes from the 14 the 199th page of Chinese drug standard, its prescription " also record in Juhong Tanke liquid for 2005 editions one one 657 pages by Chinese pharmacopoeia, form by flavour of a drug such as Exocarpium Citri Grandis, the Radix Stemonae, Semen Armeniacae Amarum, Rhizoma Cynanchi Stauntonii, Poria, Rhizoma Pinelliae Preparata, Fructus Schisandrae Chinensis, Radix Glycyrrhizaes, function cures mainly and is activating QI to eliminate phlegm, nourishing the lung to arrest cough.Be used for cough, asthma abundant expectoration due to the turbid phlegm obstructing in the lung; Flu bronchitis, pharyngolaryngitis are seen above-mentioned patient.
Juhong Tanke granule in the market all be with sucrose as correctives because the easy moisture absorption of sucrose, the granule instability, unfavorable to diabetes, obesity patient simultaneously.For a change above-mentioned defective, the present invention is through having selected a kind of novel correctives place of sucrose, add compositions such as dextrin simultaneously, make preparation of the present invention highly stable, good mouthfeel, obtained beyond thought effect, simultaneously because the variation of prescription needs new method of quality control that it is detected, so the present invention also provides new method of quality control.
Summary of the invention:
Chinese medicine granules of the present invention, its prescriptions of Chinese medicine is composed as follows:
The Exocarpium Citri Grandis 150-600g Radix Stemonae (sweet moxibustion) 15-60g Semen Armeniacae Amarum 50-200g Poria 15-60g
Rhizoma Pinelliae Preparata 15-60g Fructus Schisandrae Chinensis 10-40g Rhizoma Cynanchi Stauntonii 25-100g Radix Glycyrrhizae 5-20g
Preferably:
The Exocarpium Citri Grandis 200-400g Radix Stemonae (sweet moxibustion) 20-40g Semen Armeniacae Amarum 75-150g Poria 20-40g
Rhizoma Pinelliae Preparata 20-40g Fructus Schisandrae Chinensis 15-25g Rhizoma Cynanchi Stauntonii 40-60g Radix Glycyrrhizae 8-12g
Most preferably:
The Exocarpium Citri Grandis 300g Radix Stemonae (sweet moxibustion) 30g Semen Armeniacae Amarum 100g Poria 30g
Rhizoma Pinelliae Preparata 30g Fructus Schisandrae Chinensis 20g Rhizoma Cynanchi Stauntonii 50g Radix Glycyrrhizae 10g
Above recipe quantity calculates with the crude drug amount, can be made into medicinal granule 300-700g
Granule of the present invention wherein also comprises adjunct ingredient, and described adjunct ingredient is: dextrin, maltodextrin and correctives, correctives are selected from protein sugar, cyclamate, steviosin, most preferably steviosin.
Granule of the present invention, wherein the consumption of adjunct ingredient is:
Dextrin 300-500g, maltodextrin 50-100g, steviosin 2-8g,
Preferably:
Dextrin 350-400g, maltodextrin 60-85g, steviosin 3-5g,
Most preferably:
Dextrin 375g, maltodextrin 75g, steviosin 4g,
Above adjuvant amount is corresponding with above-mentioned prescriptions of Chinese medicine, can be made into medicinal granule 300-700g with Chinese medicine
Granule of the present invention, its preparation method is as follows:
More than eight the flavor, Exocarpium Citri Grandis, the Semen Armeniacae Amarum vapor distillation, collect distillate, Six-elements such as medicinal residues and all the other Rhizoma Pinelliae Preparata decoct with water secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain the alcohol amount and reach 75-80%, leave standstill, get supernatant and reclaim ethanol and be concentrated in right amount, obtain extractum, this extractum is formed pharmaceutically active substance of the present invention with Semen Armeniacae Amarum distillate (volatile oil), with this pharmaceutically active substance is raw material, add the adjunct ingredient that the present invention's screening obtains,, promptly get granule of the present invention through preparation method of the present invention.
The present invention adopts the direct method of granulating of clear paste, adds adjuvant and makes about 400-600g, and a day dose reduces about half.
For granule of the present invention, can adopt following method preparation:
Get extractum and dextrin, maltodextrin, the steviosin mixing adds ethanol and makes soft material, granulates, granulate, spray is with volatile oil, and airtight packing is promptly.
Specifically can be:
Get the Juhong Tanke extractum 70g that above prescription obtains, add ethanol and make that to contain alcohol amount be 60%, add steviosin 4g, dextrin 375g, maltodextrin 75g, granulate, drying is in the time of about 30 minutes about 60 ℃, with 10 mesh sieve granulate, being dried to water content in 70-80 ℃ again is 2-3%, is chilled to room temperature, spray into volatile oil, airtight 12 hours, make about 500g, promptly.
Prescription of the present invention and technology obtain through screening, and screening process is as follows:
Design five pharmaceutical formulations and compare experiment.(seeing Table 1).Each prescription is all directly made soft material with the clear paste of a recipe quantity, crosses 14 mesh sieves and granulates.60-75 ℃ of drying after the cooling, sprays into muddy hair oil, mainly with safety, mouthfeel, hygroscopicity, serve as that the examination evaluation index compares test towards dissolubility, price and granulation situation, table 2 as a result:.
Table 1 preparation experimental formula
The different pharmaceutical formulation moulding process of table 2 comparative result
The above results shows: (caking of granulating is few, and sticking sieve is not serious, and fine powder about 12% in the granule, and mouthfeel is suitable, and good towards dissolubility, cost is lower, and dextrin, maltodextrin, steviosin are safe for prescription 2.Lump, glue sieve but all have in various degree during all prescription granulations, operating difficulties because clear paste viscosity is big, stirs not open, and makes granule inhomogeneous.So this product pharmaceutical formulation can adopt prescription 2.The problem of its caking, sticking sieve can an amount of ethanol is rare to be solved by adding in clear paste.
Concentration of alcohol and consumption in the wetting agent when select granulating, having done following granulation with prescription 2 for material tests: three parts of clear paste promptly getting a recipe quantity, add not commensurability 95% ethanol respectively to containing alcohol amount 40%, 50%, 60%, stirring and dissolving is as the binding agent of granulating, and gets adjuvant 3 equal portions of a recipe quantity by prescription 2, with the clear paste granulation of above-mentioned different ethanol concentration, whether smooth when gluing sieve, caking, granulate during with granulation, particulate qualification rate is the examination index, and the result is a following table 3:
Table 3 wetting agent concentration of alcohol examination table
The result: 60% ethanol clear paste granulation granulate is more smooth, and the granule qualification rate reaches 89%, and better mobile, hydroscopicity is lower, and the easily sticking sieve of 40 gentle 0%% alcohol granulations, caking, the granulate difficulty, the granule qualification rate is lower.So selecting 60% ethanol clear paste is that directly granulation is more suitable for wetting agent.
According to experiment, determine that 1000g preparation prescription, method for making are as follows:
Preparation prescription Juhong Tanke clear paste 70g
Dextrin, 375g
Maltodextrin 75g
Steviosin 5g
Volatile oil 0.3ml
Method for making: get the Juhong Tanke clear paste 70g of recipe quantity, add ethanol and reach 60% to containing the alcohol amount, add steviosin 5g, mixing adds dextrin 375g, maltodextrin 75g again, granulates, and drying after the cooling, sprays into muddy hair oil, airtight 12 hours, makes about 500g, promptly.
The present invention also comprises the method for quality control of granule of the present invention, and this method may further comprise the steps:
Character is observed, differentiate, check steps such as assay.
Concrete steps are:
[character] this product is the light brown yellow granule, sweet, little hardship of distinguishing the flavor of.
[discriminating] (1) gets that this product is an amount of, and porphyrize takes by weighing 2.5g, adds water 10ml and makes dissolving, extracts 2 times with the ethyl acetate jolting, each 15ml, and combined ethyl acetate liquid, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.Other gets Exocarpium Citri Grandis control medicinal material 0.3g, adds methanol 10ml and puts in the water-bath reflux 20 minutes, filters, and filtrate evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, in contrast medical material solution.According to thin layer chromatography (appendix VI method) test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (2: 3: 0.3: 0.3) upper solution was developing solvent, launched, and took out, and dried with toluene-ethyl acetate-formic acid-water.Spray is with the aluminum chloride alcoholic solution.Put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(2) get this product porphyrize, take by weighing 9g, add 90% ethanol 60ml and 2% hydrochloric acid 3ml, refluxed 20 minutes, placement is spent the night, and filters, evaporate to dryness, residue add water 5ml makes dissolving, adds strong ammonia solution again and transfers more than the PH to 10, adding chloroform extracts three times, (30ml, 20ml, 20ml), combined chloroform solution, evaporate to dryness, residue adds 90% ethanol 1ml makes dissolving, as need testing solution.Other gets radix stemonae tuberosae control medicinal material 0.5g, shines medical material solution in pairs with legal system.According to thin layer chromatography (appendix VI method) test, draw each 6 μ l of need testing solution and control medicinal material solution, put respectively on same silica gel g thin-layer plate, be developing solvent with chloroform-methanol (8: 0.6), launch, take out, to dry, spray is with bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
[inspection] should meet every regulation relevant under the granule item (appendix VIIG).
[assay] measured according to high performance liquid chromatography (appendix VID).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.1% phosphoric acid water (21: 79) is a mobile phase; The detection wavelength is 283nm, and theoretical cam curve should be not less than 2000 by the naringin peak.
The preparation of reference substance solution: it is an amount of that precision takes by weighing 110 ℃ of naringin reference substances that are dried to constant weight, adds methanol and make the solution that every 1ml contains 70 μ g, promptly.
The preparation of need testing solution: get the content of this product content uniformity, porphyrize is got 0.5g, the accurate title, decide, and puts in the tool plug triangular flask, and precision adds methanol 25ml, weigh, ultrasonic 20 minutes (power 100W, frequency 40KHz) put cold, add methanol and supply the weight that subtracts mistake, filter, get subsequent filtrate and filter, promptly through microporous filter membrane (0.45 μ m).
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
This product contains Exocarpium Citri Grandis with naringin (C for every bag
10H
10O
4) meter, must not be less than 11.0mg.
The specific embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
Embodiment 1
The preparation of active component
Prescription
The Exocarpium Citri Grandis 300g Radix Stemonae (sweet moxibustion) 30g Semen Armeniacae Amarum 100g Poria 30g
Rhizoma Pinelliae Preparata 30g Fructus Schisandrae Chinensis 20g Rhizoma Cynanchi Stauntonii 50g Radix Glycyrrhizae 10g
More than eight the flavor, Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, the collection distillate, Six-elements such as medicinal residues and all the other Rhizoma Pinelliae Preparata decoct with water secondary, each 2 hours, collecting decoction, filter, filtrate is concentrated into the thick paste shape, adds ethanol and makes and contain the alcohol amount and reach 75-80%, leave standstill, get supernatant and reclaim ethanol and be concentrated in right amount, obtain extractum, this extractum is formed pharmaceutically active substance of the present invention with Semen Armeniacae Amarum distillate (volatile oil).
Embodiment 2
The preparation of granule
Get the Juhong Tanke extractum 70g that above prescription obtains, add ethanol and make that to contain alcohol amount be 60%, add steviosin 4g, dextrin 375g, maltodextrin 75g, granulate, drying is in the time of about 30 minutes about 60 ℃, with 10 mesh sieve granulate, being dried to water content in 70-80 ℃ again is 2-3%, is chilled to room temperature, spray into volatile oil, airtight 12 hours, make about 500g, promptly.
Embodiment 3
The preparation of active component
Prescription
The Exocarpium Citri Grandis 150g Radix Stemonae (sweet moxibustion) 15g Semen Armeniacae Amarum 50g Poria 15g
Rhizoma Pinelliae Preparata 15g Fructus Schisandrae Chinensis 10g Rhizoma Cynanchi Stauntonii 25g Radix Glycyrrhizae 5g
Preparation method is with embodiment 1
Embodiment 4
The preparation of active component
Prescription
The Exocarpium Citri Grandis 600g Radix Stemonae (sweet moxibustion) 60g Semen Armeniacae Amarum 200g Poria 60g
Rhizoma Pinelliae Preparata 60g Fructus Schisandrae Chinensis 40g Rhizoma Cynanchi Stauntonii 100g Radix Glycyrrhizae 20g
Preparation method is with embodiment 1
Embodiment 5
The preparation of active component
Prescription
The Exocarpium Citri Grandis 200g Radix Stemonae (sweet moxibustion) 20g Semen Armeniacae Amarum 75g Poria 20g
Rhizoma Pinelliae Preparata 20g Fructus Schisandrae Chinensis 15g Rhizoma Cynanchi Stauntonii 40g Radix Glycyrrhizae 8g
Preparation method is with embodiment 1
Embodiment 6
The preparation of active component
Prescription
The Exocarpium Citri Grandis 400g Radix Stemonae (sweet moxibustion) 40g Semen Armeniacae Amarum 150g Poria 40g
Rhizoma Pinelliae Preparata 40g Fructus Schisandrae Chinensis 25g Rhizoma Cynanchi Stauntonii 60g Radix Glycyrrhizae 12g
Preparation method is with embodiment 1
Embodiment 7
The preparation of active component
Prescription
The Exocarpium Citri Grandis 400g Radix Stemonae (sweet moxibustion) 40g Semen Armeniacae Amarum 150g Poria 40g
Rhizoma Pinelliae Preparata 40g Fructus Schisandrae Chinensis 25g Rhizoma Cynanchi Stauntonii 60g Radix Glycyrrhizae 12g
Preparation method is with embodiment 1, and wherein steviosin is replaced with protein sugar.
Embodiment 8
The preparation of active component
Prescription
The Exocarpium Citri Grandis 400g Radix Stemonae (sweet moxibustion) 40g Semen Armeniacae Amarum 150g Poria 40g
Rhizoma Pinelliae Preparata 40g Fructus Schisandrae Chinensis 25g Rhizoma Cynanchi Stauntonii 60g Radix Glycyrrhizae 12g
Preparation method is with embodiment 1, and wherein steviosin is replaced with cyclamate.
Claims (3)
1, a kind of sugar-free type red tangerine peel granular agent for treating productive cough is characterized in that, the prescription of used raw material of Chinese medicine is as follows: Exocarpium Citri Grandis 300g, Radix Stemonae 30g, Semen Armeniacae Amarum 100g, Poria 30g, Rhizoma Pinelliae Preparata 30g, Fructus Schisandrae Chinensis, 20g Rhizoma Cynanchi Stauntonii 50g, Radix Glycyrrhizae 10g, the Juhong Tanke extractum 70g that makes with this prescription, with dextrin 375g, maltodextrin 75g, steviosin 4g is prepared into the 500g sugar-free type red tangerine peel granular agent for treating productive cough.
2, the preparation method of the granule of claim 1, it is characterized in that, process following steps: Exocarpium Citri Grandis, Semen Armeniacae Amarum vapor distillation, collect distillate, medicinal residues and all the other Six-elements decoct with water secondary, each 2 hours, collecting decoction filters, and filtrate is concentrated into the thick paste shape, adding ethanol makes the alcohol amount of containing reach 75-80%, leave standstill, get supernatant and reclaim ethanol and be concentrated in right amount, obtain extractum, this extractum is formed pharmaceutically active substance of the present invention with the Semen Armeniacae Amarum distillate, with this pharmaceutically active substance is raw material, adds adjunct ingredient, is prepared from.
3, the content assaying method of naringin in the granule of claim 1 is characterized in that, may further comprise the steps:
Assay is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-0.1% phosphoric acid water is a mobile phase; The detection wavelength is 283nm, and theoretical cam curve should be not less than 2000 by the naringin peak;
The preparation of reference substance solution: it is an amount of that precision takes by weighing 110 ℃ of naringin reference substances that are dried to constant weight, adds methanol and make the solution that every 1ml contains 70 μ g, promptly;
The preparation of need testing solution: get the content of this product content uniformity, porphyrize is got 0.5g, and accurate the title decides, and puts in the tool plug triangular flask, precision adds methanol 25ml, weighs, and ultrasonic 20 minutes, puts cold, add methanol and supply the weight that subtracts mistake, filter, get subsequent filtrate and filter, promptly through microporous filter membrane;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
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| CN200610099306A CN100584318C (en) | 2006-07-13 | 2006-07-13 | Sugar-free type red tangerine peel granular agent for treating productive cough |
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| CN200610099306A CN100584318C (en) | 2006-07-13 | 2006-07-13 | Sugar-free type red tangerine peel granular agent for treating productive cough |
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| CN100584318C true CN100584318C (en) | 2010-01-27 |
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| CN105726642B (en) * | 2014-04-14 | 2020-01-14 | 海南葫芦娃药业集团股份有限公司 | Honeysuckle flower cold granules and preparation method thereof |
| CN105943512B (en) * | 2016-06-20 | 2019-03-15 | 陆川县银湖橘红种植专业合作社 | A kind of Exocarpium Citri Rubrum lozenge and preparation method thereof |
| CN108426955A (en) * | 2018-03-11 | 2018-08-21 | 安徽省食品药品检验研究院 | The discrimination method of tuber of stemona genunie medicinal materials |
| CN108740677A (en) * | 2018-06-22 | 2018-11-06 | 化州化橘红药材发展有限公司 | A kind of Exocarpium Citri Grandis slow-release solid beverage and preparation method thereof |
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- 2006-07-13 CN CN200610099306A patent/CN100584318C/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 中华人民共和国卫生部药品标准中药成方制剂. 中华人民共和国药典委员会，z14-199. 1997 |
| 中华人民共和国卫生部药品标准中药成方制剂. 中华人民共和国药典委员会，z14-199. 1997 * |
| 无糖型清喉消炎冲剂的研制. 黎新荣等.中国医院药学杂志，第16卷第11期. 1996 |
| 无糖型清喉消炎冲剂的研制. 黎新荣等.中国医院药学杂志，第16卷第11期. 1996 * |
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