CN101352494B - Children's granules for clearing heat and suppressing cough and preparation method thereof - Google Patents
Children's granules for clearing heat and suppressing cough and preparation method thereof Download PDFInfo
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- CN101352494B CN101352494B CN2008100625619A CN200810062561A CN101352494B CN 101352494 B CN101352494 B CN 101352494B CN 2008100625619 A CN2008100625619 A CN 2008100625619A CN 200810062561 A CN200810062561 A CN 200810062561A CN 101352494 B CN101352494 B CN 101352494B
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Abstract
The invention discloses a heat clearing and cough relieving granule for children and a preparation method thereof; the heat clearing and cough relieving granule for children is prepared by the raw materials of Chinese ephedra, (fried) bitter almond, gypsum, liquorice, radix scutellariae, radix isatidis and rhizoma menispermi; the weight of each raw material required for preparing 1000g of the heat clearing and couch relieving granule for children is as follows: 100-200g of Chinese ephedra, 180-220g of (fried) bitter almond, 400-500g of gypsum, 180-220g of liquorice, 270-330g of radix scutellariae, 280-320g of radix isatidis and 130-180g of rhizoma menispermi. The granule of the invention has remarkable functions of clearing heat, ventilating the lung and relieving asthma as well as definite and good curative effects on the symptoms caused by exogenous infection of children such as fever with chilliness, cough with yellow sputum, tachypnea, hyperpnea, dry mouth, raucity, swollen sore throat, tonsillitis, and the like; furthermore, the granule of the invention has good taste, does not contain any preservatives and is especially suitable for children.
Description
Technical field
The present invention relates to a kind of infantile heat-clearing and antitussive granule and preparation method thereof, belong to technical field of Chinese medicine.
Background technology
Upper respiratory tract infection is the most common disease of child, often causes heating by diseases caused by exogenous pathogenic factor, cough expectorant Huang, asthma, diseases such as laryngopharynx swelling and pain.Often adopt Chinese patent drugs for treatment such as chemicalses such as antibiotic, antipyretic analgesic, relieving cough and resolving phlegm medicine and oral liquid for cough and asthma of children, infantile lung heat cough with asthma oral liquid at present clinically.But childhood upper respiratory tract infection mostly belongs to viral infection, and antibiotic often is difficult to take effect, and easily produces drug resistance again, and other chemical medicine also can only symptomatic treatment, and some Chinese patent medicines are owing to reasons such as its prescription and dosage, and onset time is slower, and curative effect is limited.
Summary of the invention
Technical problem to be solved by this invention is to propose a kind of steady quality, and method of quality control is scientific and reasonable, and mouthfeel is better, is suitable for infantile heat-clearing and antitussive granule of child's use and preparation method thereof.
For solving the problems of the technologies described above, a kind of infantile heat-clearing and antitussive granule of the present invention is that feedstock production forms with Herba Ephedrae, Semen Armeniacae Amarum (stir-fry), Gypsum Fibrosum, Radix Glycyrrhizae, Radix Scutellariae, Radix Isatidis, Rhizoma Menispermi, the weight of making required each raw material of every 1000g infantile heat-clearing and antitussive granule is Herba Ephedrae 100-200g, Semen Armeniacae Amarum (stir-fry) 180-220g, Gypsum Fibrosum 400-500g, Radix Glycyrrhizae 180-220g, Radix Scutellariae 270-330g, Radix Isatidis 280-320g, Rhizoma Menispermi 130-180g.
Above-mentioned a kind of infantile heat-clearing and antitussive granule, the weight of required each raw material of described every 1000g granule is Herba Ephedrae 150g, Semen Armeniacae Amarum (stir-fry) 200g, Gypsum Fibrosum 450g, Radix Glycyrrhizae 150g, Radix Scutellariae 300g, Radix Isatidis 300g, Rhizoma Menispermi 150g.
Above-mentioned a kind of infantile heat-clearing and antitussive granule, it also comprises adjuvant, every 1000g granule adds following adjuvant: citric acid 5-10g, sodium cyclamate 5-10g, sucrose 450-500g, dextrin is an amount of.
Above-mentioned a kind of infantile heat-clearing and antitussive granule, required each adjuvant of every 1000g granule is citric acid 8g, sodium cyclamate 8g, sucrose 486g, dextrin 240-340g.
The particulate preparation method of a kind of infantile heat-clearing and antitussive comprises the steps: (1) extraction: get Herba Ephedrae 150g and Gypsum Fibrosum coarse powder 450g, add the water of 8 times of amounts, heated and boiled 30 minutes; Radix Glycyrrhizae 150g, Radix Scutellariae 300g, Radix Isatidis 300g, all the other Chinese medicine of the five flavours such as Semen Armeniacae Amarum (stir-fry) 200g, Rhizoma Menispermi 150g are added, add and drink make a living 4 times of amounts of medicine of the water yield, boiled 2 hours; Decocting liquid is emitted through piping filter; For the second time add 3 times of amounts that water is crude drug, boiled 1 hour; Decocting liquid is emitted through piping filter; Merge decocting liquid twice, be evaporated to about 1/3 amount of fried liquid, emit standing over night; Draw supernatant, filter, filtrate continuation is concentrated into heat and surveys (60 ℃) relative density 1.35～1.38, and thick paste is measured water content and accurately metering; (2) preparation, granulation: get thick paste, add sodium cyclamate 8g, citric acid 8g stirs and makes dissolving; It is an amount of to take by weighing cane sugar powder 486g and dextrin, fully behind the mixing, adds the thick paste mixture, and mixing adds an amount of 95% ethanol and regulates the soft material humidity, and 16 mesh sieves are granulated, and granule finally makes infantile heat-clearing and antitussive granule granule 1000g in 75～80 ℃ of dryings.
The present invention has been owing to adopted above-mentioned prescription and preparation method, the Herba Ephedrae of adopting in the side, and arduous temperature, diffusing lung, relieving exterior syndrome is to relieving asthma.Gypsum Fibrosum, in hot sweet Great Cold, the heat of letting out the lung stomach clearly is to promote the production of body fluid.Two medicines are made as usefulness mutually, can lung qi dispersing, can expel the heat-evil again; Can relieving asthma, can promote the production of body fluid again.Though a hot temperature, one is hot cold, hot cold greater than hot temperature, makes we not lose the agent of hot cold, and two medicines are monarch drug altogether.The Semen Armeniacae Amarum hardship is fallen, tepor, and the sending down the abnormal ascending QI relieving cough and asthma falls one liter with Herba Ephedrae one, declares smooth lung qi, relieving cough and asthma.Radix Scutellariae, bitter cold, clearing away heat-fire, eliminating heat from the lung is longer than in detoxifcation.Radix Isatidis, bitter cold, heat-clearing and toxic substances removing, removing heat from blood sore-throat relieving.Rhizoma Menispermi, bitter cold, heat-clearing and toxic substances removing helps the cold and cool property of Gypsum Fibrosum, lets out lung excess of the stomach fire clearly, and detoxifcation is promoted the production of body fluid, and separates all diseases of betraing of fever of the body dry pharynx laryngalgia.Four medicines are adjuvant drug altogether.Radix Glycyrrhizae, sweet flat, coordinating the actions of various ingredients in a prescription is with protecting stomach-QI, makes unlikely injuring one's stomach in Great Cold such as Gypsum Fibrosum, and Radix Glycyrrhizae gets the Gypsum Fibrosum promoting production of body fluid with drugs sweet in flavor and cold in nature, Herba Ephedrae, almond cough-relieving eliminate the phlegm, for making.All medicines share, and have significant heat clearing away, lung qi dispersing, antiasthmatic effect, are used for the treatment of diseases such as the children's exogenous fever with chills that causes, cough expectorant Huang, tachypnea are panted, xerostomia hoarseness, laryngopharynx swelling and pain, tonsillitis redness clinically, show definite and good curative effect.Granule of the present invention has that steady quality, method of quality control are scientific and reasonable, steady quality, long shelf-life, be convenient to keeping transportation, mouthfeel and better, do not contain advantages such as antiseptic and medicine valency are lower, is suitable for the child especially and uses.
Description of drawings
Fig. 1 is the canonical plotting of the linear relationship of expression ephedrine hydrochloride.
The specific embodiment
Embodiment one:
1, process study
1.1 prescription: Herba Ephedrae 150g, Semen Armeniacae Amarum (stir-fry) 200g, Gypsum Fibrosum 450g, Radix Glycyrrhizae 150g, Radix Scutellariae 300g, Radix Isatidis 300g, Rhizoma Menispermi 150g.
1.2 extract: get Herba Ephedrae, Gypsum Fibrosum coarse powder, add the water of 8 times of amounts, heated and boiled 30 minutes.All the other Chinese medicine of the five flavours such as Radix Glycyrrhizae, Radix Scutellariae, Radix Isatidis, Semen Armeniacae Amarum (stir-fry), Rhizoma Menispermi are added, and interpolation water is 4 times of amounts of crude drug (being meant total whole middle dose), boils 2 hours.Decocting liquid is emitted through piping filter.Adding for the second time water is 3 times of amounts of crude drug (being meant total whole middle dose), boils 1 hour.Decocting liquid is emitted through piping filter.Merge decocting liquid twice, be evaporated to about 1/3 amount of fried liquid, emit standing over night.Draw supernatant, filter, filtrate continuation is concentrated into heat and surveys (60 ℃) relative density 1.35～1.38.Thick paste is measured water content and accurately metering.
1.3 preparation, granulation
1.3.1 preparation prescription
Thick paste (extracted amount), citric acid 8g, sodium cyclamate 8g, sucrose 486g, dextrin (in right amount).
Make 1000g infantile heat-clearing and antitussive granule.
1.3.2 adjuvant pre-treatment
Sucrose is pulverized with 80 orders annular sieve on Universalpulverizer, takes by weighing Icing Sugar by recipe quantity during preparation.
1.3.3 batch mixing
Sodium cyclamate and citric acid are crystalline solid, and quantity is little, do when mixing to be difficult for and the unclassified stores mixing, and in the granule of making white point is arranged, but both water solublity are good, it can be added in the thick paste, and stirring makes molten.After treating Icing Sugar and dextrin mix homogeneously, again the thick paste compound is added, be mixed to the mastic homodisperse.Look soft material and do wet degree, add an amount of 95% ethanol and regulated.
1.3.4 granulation, drying
The soft material paste containing amount is bigger, and thick paste relative density height, and viscosity is stronger, should use the squash type comminutor to granulate.Wet grain is controlled at 75～80 ℃ by 80 ℃ of dryings of standard code in the production.Dried granule is pressed regulation under the granule item, and the whole sieve of warp screens out No. 1 sieve and goes up coarse granule and sieve fine powder down for No. 4.Finally make infantile heat-clearing and antitussive granule 1000g.
1.3.5 packing
The composite membrane packing of qualified granule, every bag of 6g.Per 6 bags with adorning box behind the plastic bag sealing.
This product is faint yellow to brown yellow granule, and it is sweet to distinguish the flavor of, little hardship.Usage and dosage is: boiled water is taken after mixing it with water.One-year-oldly once obeyed 2-3g to two years old, once obeyed 3-6g, once obeyed 6-9g, 3 times on the one in six years old to 14 years old in three years old to five years old.
1.4. the selection of correctives and consumption
1.4.1 sweeting agent
Sodium cyclamate chemistry sodium cyclamate by name is a kind of non-sugar sweetener that is widely used in food industry.Ministry of Public Health had been issued tentative standard [WS-096 (X-66)-91] in 1991, and " Chinese pharmacopoeia is recorded by 2000 editions in the back.This sweeting agent sugariness is 50 times of sucrose, and mouthfeel is good, and calorific value is little, and is safe in utilization.The oral LD of toxicology test mice
50Be 17000mg/kg (bw) that FAO/WHO regulation acceptable daily intake ADI value is 11mg/kg (bw), China's " food additive is used sanitary standard " (GB-2760-1996) in the regulation food maximum addition be 8.0g/kg.The infantile heat-clearing and antitussive granule is write out a prescription with 0.8% amount.Product are quantitatively taken by system because of medicine, by the usage and dosage of this product, far below the FAO/WHO prescribed limit, see following table with body weight=2 * age+7～8 (kg) calculating intake every day for details:
| Age | Body weight kg | The granule day dose g of regulation | Sodium cyclamate amount mg wherein | Allow intake mg |
| 1～2 year old | 9～11 | 6～9 | 48～72 | 99～121 |
| 3～5 years old | 13～17 | 9～18 | 72～144 | 143～198 |
| 6～14 years old | 19～35 | 18～27 | 144～216 | 198～297 |
1.4.2 acidity regulator
Suitable tart flavour can further be covered up bitterness, increases local flavor.Citric acid tart flavour is mellow and full, plentiful, and is safe in utilization, and the inhibition action of microorganisms is arranged.Do not stipulate use amount in " food additive use sanitary standard ", can " need an amount of the use " by producing.We are according to result of the test, and the dosage with 0.8% in this granule is more satisfactory.
1.4.3 diluent
This product is that Chinese medicine extract (thick paste) adds the granule that adjuvant is made, because thick paste water content height, viscosity is big, must use good medicinal diluent to dilute and finish system granule technology.And the dextrin that the present invention adopts is a kind of pharmaceutic adjuvant of super quality and competitive price commonly used, and its consumption is just can draw after calculating according to the moisture content of each Chinese medicine extract (thick paste) with by the theoretical grain amount of finally making of prescription.The dextrin amount ranges that makes infantile heat-clearing and antitussive granule 1000g is at 240-340g.
2, adjuvant source and quality standard
Adjuvant title source quality standard
Sucrose Guangxi land-reclaimable sugar industry group " Chinese pharmacopoeia
Dextrin Zhejiang Jiaxing whitecap starch-based product company limited " Chinese pharmacopoeia
Zhongshan city, sodium cyclamate Guangdong food additive factory " Chinese pharmacopoeia
Citric acid Wuxi City No.2 Pharmaceutical Factory " Chinese pharmacopoeia
3. the physicochemical property relevant with quality standard
The contained main chemical compositions of medicine 3.1 respectively distinguish the flavor of in the prescription
Herba Ephedrae: mainly contain multiple alkaloid and a small amount of volatile oil.Main component is 1 one ephedrines, 1-N monomethyl ephedrine, d-N monomethyl pseudoephedrine, ephedine alkali in the alkaloid; Containing 1-d one terpinol, 2,3,5,6 one tetramethyls in the volatile oil adjoins and tremnbles (I) and 1-d one terpinenol (II).
Semen Armeniacae Amarum: contain effective ingredient amygdalin about 3%.
Gypsum Fibrosum: the main component of Gypsum Fibrosum is hydrous calcium sulfate (CaSO
42H
2O), small amount of impurities, still contain Fe
2+, Mg
2+Deng, also contain usnic acid.
Radix Glycyrrhizae: contain triterpenoid compound glycyrrhizin and 24 1 antelopes base enoxolone etc.Also contain flavone compound.
Radix Scutellariae: contain the intoxicated analog derivative of multiple Huang, wherein mainly contain Radix Scutellariae glycoside 4.0-5.2%, baicalin, wogonoside, skullcapflavone I, II etc., other contains β one sitosterol, campesterol, stigmasterol etc.
Radix Isatidis: contain sinigrin, isatin, β one sitosterol etc., and contain propylhomoserin, γ one aminobutyric acid etc. clearly.
Rhizoma Menispermi: containing multiple alkaloid, be mainly dauricine, is nor-dauricine secondly, different nor-dauricine, Rhizoma Menispermi phenol alkali, magnoline etc.
4. character
This product is faint yellow to brown yellow granule, sweet, little hardship of distinguishing the flavor of.
5. differentiate
5.1 differentiate (1)
5.1.1 representative flavour of a drug: Herba Ephedrae
5.1.2 method
Get this product 15g, porphyrize adds strong ammonia solution 0.5ml, and chloroform 30ml reflux, extract, 30 minutes is put coldly, filters, and filtrate evaporate to dryness, residue add ethanol 1ml dissolving, as need testing solution.Other gets the ephedrine hydrochloride reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw above-mentioned two kinds of each 10ul of solution, put respectively in same and contain on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binding agent,--methanol--strong ammonia solution (20: 5: 0.5) is developing solvent with chloroform, launch, take out, dry, spray is with ninhydrin solution, about 5 minutes of 105 ℃ of bakings.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
5.1.3 test method and result
5.1.3.1 the preparation of negative controls
Get other medical material that removes Herba Ephedrae in the prescription, prepare negative controls by the preparation method of test sample in 2. method for making items and the 5.1.2 discrimination method item.
5.1.3.2 preparation for test agent solution and reference substance solution
Get three batch samples, prepare test sample and positive reference substance solution respectively by the preparation method of test sample in the 5.1.2 discrimination method item by 2. method for making items preparations.
5.1.3.3 test method and result
Get above-mentioned negative controls, need testing solution, each 10 μ l of reference substance solution, carry out the thin layer test by the 5.1.2 method.The result is in thin-layer chromatogram, present a brownish red speckle in the ephedrine hydrochloride reference substance chromatograph, the negative fluid chromatograph that lacks Herba Ephedrae is at ephedrine hydrochloride reference substance chromatograph relevant position immaculate, and the test sample chromatograph is then presenting an identical brownish red speckle with ephedrine hydrochloride reference substance chromatograph relevant position.
5.1.4 conclusion
Material does not disturb the discriminating of this product epheday intermedia in the negative controls, promptly increase correctives sodium cyclamate, citric acid after, detecting of this product epheday intermedia do not produced interference.
5.2 differentiate (2)
5.2.1 representative flavour of a drug: Radix Scutellariae
5.2.2 method
Get this product 15g, porphyrize adds methanol 20ml, and reflux, extract, 30 minutes filters, and filtrate evaporate to dryness, residue add water 10ml dissolving, add ethyl acetate and wash 2 times, and each 15ml discards ethyl acetate liquid, and water layer evaporate to dryness, residue add methanol 1ml dissolving, as need testing solution.Other gets the baicalin reference substance and adds methanol and make the solution that every 1ml contains 1mg, product solution in contrast, test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2000), draw above-mentioned two kinds of each 10ul of solution, put respectively, with ethyl acetate-butanone-formic acid-water (5: 3: 1: 1) be developing solvent the containing on the silica gel g thin-layer plate that sodium carboxymethyl cellulose is a binding agent of same usefulness 4% sodium acetate solution preparation, launch, take out, airing, spray is with the alcoholic solution of 2% ferric chloride.In the test sample chromatograph, with reference substance chromatograph relevant position on, show the speckle of same color.
5.2.3 test method and result
5.2.3.1 the preparation of negative controls
Get other medical material that removes Radix Scutellariae in the prescription, prepare negative controls by the preparation method of test sample in 2. method for making items and the 5.2.2 discrimination method item.
5.2.3.2 preparation for test agent solution and reference substance solution
Get three batch samples, prepare test sample and positive reference substance solution respectively by the preparation method of test sample in the 5.2.2 discrimination method item by 2. method for making items preparations.
5.2.3.3 test method and result
Get above-mentioned negative controls, need testing solution, each 10 μ l of reference substance solution, carry out the thin layer test by the 5.2.2 method.The result presents a brownish black speckle in the baicalin reference substance chromatograph in thin-layer chromatogram, the negative fluid chromatograph that lacks Radix Scutellariae is at the same position immaculate, and is presenting an identical brownish black speckle with baicalin reference substance chromatograph relevant position in the test sample chromatograph.
5.2.5 conclusion
Material does not disturb the discriminating of Radix Scutellariae in this product in the negative fluid, promptly increase correctives sodium cyclamate, citric acid after, detecting of Radix Scutellariae in this product do not produced interference.
5.3 assay
5.3.1 assay method
The about 15mg of ephedrine hydrochloride reference substance is got in the preparation of reference substance solution, accurate claims surely, puts in the 100ml measuring bottle, is dissolved in water and is diluted to scale, shakes up, and promptly gets (the hydrochloric ephedrine 0.15mg of every 1ml).
The preparation precision of standard curve is measured reference substance solution 0.2ml, 0.4ml, 0.8ml, 1.2ml, 1.6ml, place the 60ml separatory funnel respectively, add water respectively and complement to 6ml, adding citric acid more respectively--sodium citrate buffer (is got 0.1mol/L citric acid 20ml, add the 0.1mol/L sodium citrate and transfer PH to 5.4, i.e.) 10ml, 0.1% bromothymol blue test solution (is got natrium carbonicum calcinatum 0.1g, in the rearmounted 100ml measuring bottle that is dissolved in water, add bromothymol blue 0.1g, add water to scale, shake up, be i.e.) 2ml, shake up, add chloroform, violent jolting is extracted 3 times (14,5,5ml), divide and get chloroform solution, be incorporated in the 25ml measuring bottle, add chloroform and be diluted to scale, shake up.Other 6ml that fetches water makes blank solution by last method.According to spectrophotography (appendix V of Chinese Pharmacopoeia version in 2000) test, measure trap at 413nm wavelength place, be abscissa with concentration, trap is a vertical coordinate, the drawing standard curve.
Algoscopy is got this product 25g, the accurate title, decide, add sodium chloride 4g and 40% sodium hydroxide solution 5ml, use steam distillation, and make absorption liquid with dilute hydrochloric acid 10ml, and put in the 200ml measuring bottle, collect the about 195ml of distillate, thin up is to scale, shake up, the accurate 3ml that draws puts in the 60ml separatory funnel, by above-mentioned standard curve item down from " add citric acid more respectively--sodium citrate buffer solution 10ml ", with method operation, measure trap at 413nm wavelength place, obtain the concentration of ephedrine hydrochloride the need testing solution from standard curve, calculate, promptly.
The every 1g of this product contains Herba Ephedrae with ephedrine hydrochloride (C
10H
15NOHCl) meter should be 0.20～1.10mg.
5.3.2 measuring principle and methodology test
This product epheday intermedia is monarch drug, and the ephedrine in the Herba Ephedrae is one of active component wherein, and reference literature has carried out assay to the ephedrine in the Herba Ephedrae.Utilize the principle of acid-dye colorimetry, make preparation epheday intermedia base become ion pair with the quantitative complexation of the bromothymol blue dissociated anion of institute, discharge stable yellow solution, the concentration with in the colorimetry measurement test liquid can calculate the Herba Ephedrae content that measures with ephedrine hydrochloride in this product.
5.3.2.1 the interference of the definite and negative fluid of maximum absorption wavelength
5.3.2.1.1 the preparation of negative controls
Get other medical material that removes Herba Ephedrae in the prescription, prepare negative controls by 2. method for making items and 5.1 determinations.
5.3.2.1.2 the preparation of reference substance solution
After getting the ephedrine hydrochloride reference substance and making the hydrochloric ephedrine 0.15mg of every 1ml molten by the preparation method of reference substance solution in 5.1, the accurate again 1ml that draws is prepared into reference substance solution by determination.
5.3.2.1.3 preparation for test agent solution
Three batch samples of getting by the preparation of 2. method for making items prepare need testing solution by 5.1 determinations.
5.3.2.1.4 the preparation of blank solution
The accurate purified water 6ml that draws prepares blank solution by 5.1 determinations.
5.3.2.1.5 test method and result
Divide and get above-mentioned reference substance solution, negative controls, need testing solution, all the blank solution with the 5.3.1.4 preparation is a blank, in the 300nm-500nm wave-length coverage, do ultraviolet absorpting spectrum with step-length 0.1nm with the TU-1800 ultraviolet-uisible spectrophotometer, and the gained collection of illustrative plates is carried out the peak inspection.Reference substance solution as a result, need testing solution has absorption maximum respectively near the 413nm wavelength, and negative fluid does not almost have absorption at this wavelength.
5.3.2.1.6 conclusion
Negative fluid does not disturb in this product Determination of Ephedrine Hydrochloride to measure, promptly increase adjuvant sodium cyclamate, citric acid after, measure noiseless to Determination of Ephedrine Hydrochloride in this product.
5.3.2.2 the standard curve and the range of linearity
Ephedrine hydrochloride 0.2ml, the 0.4ml of the accurate 0.1567mg/ml of absorption, 0.8ml, 1.2ml, 1.6ml operate according to 5.1 assay items, and measurement result is as follows:
With concentration is vertical coordinate, is abscissa with the trap, draws standard curve as shown in Figure 1.Equation of linear regression: C=1.0804A+0.0318 correlation coefficient: the r=0.9994 range of linearity: 1.254 * 10
-3Mg/ml-1.003 * 10
-2Mg/ml
Ephedrine hydrochloride is good in above-mentioned scope internal linear relation as a result.
5.3.2.3 determining of water vapour distillate volume
Precision takes by weighing this product 25g, according to 5.1 determination operations, collects distillate respectively, and volume is respectively 75ml, 100ml, 125ml, 150ml, 175ml, 195ml, 200ml
Measurement result is as follows:
Determine that collecting amount is 195ml.
5.3.2.4 repeatability experiment
Same sample is got 5 parts, presses content assaying method respectively and measures, and the result is as follows:
5.3.2.5 average recovery
Get a duplicate samples, carry out assay by the quality standard method, the result is 0.516mg/g; Get the ephedrine hydrochloride reference substance, claim surely with 100,000/balance is accurate, weight is 39.611mg, puts in the 50ml volumetric flask, is dissolved in water and is diluted to scale, and is standby.Precision takes by weighing the above-mentioned sample 12.5g of known accurate content, and the accurate again reference substance solution 5ml that adds above-mentioned concentration known (0.7922mg/ml) measures by 5.1 content assaying methods.The result is as follows:
5.3.2.6 the mensuration of sample
5.3.3 conclusion
By the test of above methodology, this method is measured applicable to increasing after adjuvant sodium cyclamate, the citric acid in this product Determination of Ephedrine Hydrochloride.
Stability study testing data of the present invention
1. general introduction
According to Chinese Pharmacopoeia appendix medicine stability test guideline, three batches of this product have been carried out long term test, in the hope of the stability of research this product.
2. sample situation
2.1 sample source: capsule particle agent preproduction
2.2 sample requirement: three batches of products, commercially available back are that composite membrane adds aluminium foil bag and carton package.
2.3 sample lot number: 01,02,03
3. investigation project
Character, moisture, granularity, melting, microbial limit, content
4. test method
With three batches of products, after the packing, place under 25 ℃ ± 2 ℃, the condition of relative humidity 60% ± 10% and placed 3 years, and, detect respectively by above-mentioned investigation project the 0th, 3,6,9,12,18,24 and 36 sampling at the end of month.
5. result of the test sees the following form.
6. conclusion
The equal conformance with standard regulation of each time assay illustrates that this product can quality keep stable in 2 years effect duration.
Embodiment two:
1, prescription
Herba Ephedrae 1.8kg Semen Armeniacae Amarum (stir-fry) 2.4kg Gypsum Fibrosum 5.4kg Radix Glycyrrhizae 1.8kg
Radix Scutellariae 3.6kg Radix Isatidis 3.6kg Rhizoma Menispermi 1.8kg sucrose 5.832kg
Citric acid 0.096kg sodium cyclamate 0.096kg dextrin is an amount of
Make 12.0kg (6g * 2000 bag) infantile heat-clearing and antitussive granule
2, method for making
Get Herba Ephedrae, Gypsum Fibrosum coarse powder, add the drinking water (58L) of 8 times of amounts, heated and boiled 30 minutes.All the other Chinese medicine of the five flavours such as Radix Glycyrrhizae, Radix Scutellariae, Radix Isatidis, Semen Armeniacae Amarum (stir-fry), Rhizoma Menispermi are added, and adding drinking water is 4 times of amounts (82L) of crude drug, boils 2 hours.Decocting liquid is emitted through piping filter.For the second time add 3 times of amounts (61L) that water is crude drug, boiled 1 hour.Decocting liquid is emitted through piping filter.Merge decocting liquid twice, be evaporated to about 1/3 amount of fried liquid, emit standing over night.Draw supernatant, filter, filtrate continuation is concentrated into heat and surveys (60 ℃) relative density 1.35～1.38.Thick paste is measured water content and accurately metering.Get thick paste, add sodium cyclamate 0.096kg and citric acid 0.096kg, stir and make dissolving; It is an amount of to take by weighing cane sugar powder 5.832kg and dextrin, fully behind the mixing, adds the thick paste mixture, mix homogeneously makes the ointment-like medicine for oral or plastering use homodisperse, adds an amount of 95% ethanol and regulates the soft material humidity, granulate with squash type comminutor 16 mesh sieves, granule is in 75～80 ℃ of dryings, and control moisture is below 3%; Dried granule sieves coarse granule and fine powder respectively with 10 orders and 60 mesh sieves after sieving with 14 mesh sieves are whole; Qualified granule is sub-packed in the complex pocket, every packed 6g, per 6 bags with adorning box behind the plastic bag sealing, make 12.0kg infantile heat-clearing and antitussive granule (6g * 2000 bag)
3, the three batches of pilot scale data (the every batch of inventory be 2000 bags * 6g)
| Lot number | Thick paste amount (kg) | Relative density (70 ℃) | Moisture content (%) | Cane sugar powder (kg) | Sodium cyclamate (kg) | Citric acid (kg) | Dextrin (kg) |
| 01 | 2.92 | 1.37 | 24.0 | 5.84 | 0.096 | 0.096 | 3.70 |
| 02 | 3.00 | 1.37 | 24.2 | 6.00 | 0.096 | 0.096 | 3.49 |
| 03 | 3.14 | 1.36 | 24.5 | 6.28 | 0.096 | 0.096 | 3.11 |
| Lot number | Qualified granule (kg) | Coarse granule (kg) | Fine powder (kg) | Pellet moisture (%) | Granule yield (%) | Number of package (box) | Yield rate (%) |
| 01 | 10.80 | 0.60 | 0.40 | 1.5 | 90.0 | 300 | 90.0 |
| 02 | 10.62 | 0.72 | 0.63 | 1.7 | 88.5 | 293 | 87.9 |
| 03 | 10.70 | 0.57 | 0.58 | 1.7 | 89.2 | 295 | 88.5 |
Embodiment three:
Get Herba Ephedrae 180g, Gypsum Fibrosum 430g decocts with water half an hour, adds Semen Armeniacae Amarum (stir-fry) 220g, Radix Glycyrrhizae 130g, Radix Scutellariae 320g, Radix Isatidis 280g and Rhizoma Menispermi 160g again, decoct with water twice, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate decompression is concentrated into the thick paste that relative density is 1.35-1.38 (60 ℃), adds sodium cyclamate 9g, citric acid 7g, the an amount of mixing of sucrose 470g and dextrin, make granule 1000g, dry (80 ℃), promptly.(concrete technology is identical with embodiment one)
Embodiment four:
Get Herba Ephedrae 130g, Gypsum Fibrosum 470g decocts with water half an hour, adds Semen Armeniacae Amarum (stir-fry) 180g, Radix Glycyrrhizae 180g, Radix Scutellariae 280g, Radix Isatidis 240g and Rhizoma Menispermi 140g again, decoct with water twice, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, filtrate decompression is concentrated into the thick paste that relative density is 1.35-1.38 (60 ℃), adds sodium cyclamate 7g, citric acid 10g, the an amount of mixing of sucrose 500g and dextrin, make granule 1000g, dry (80 ℃), promptly.This product is faint yellow to brown yellow granule, and it is sweet to distinguish the flavor of, little hardship.Usage and dosage is: boiled water is taken after mixing it with water.One-year-oldly once obeyed 2-3g to two years old, once obeyed 3-6g, once obeyed 6-9g, 3 times on the one in six years old to 14 years old in three years old to five years old.(concrete technology is identical with embodiment one)
Claims (1)
1. the particulate preparation method of infantile heat-clearing and antitussive is characterized in that, it comprises the steps: (1) extraction: get Herba Ephedrae 150g and Gypsum Fibrosum coarse powder 450g, add the water of 8 times of amounts, heated and boiled 30 minutes; Radix Glycyrrhizae 150g, Radix Scutellariae 300g, Radix Isatidis 300g, Semen Armeniacae Amarum (parched) 200g, Rhizoma Menispermi 150g are added, add and drink make a living 4 times of amounts of medicine of the water yield, boiled 2 hours; Decocting liquid is emitted through piping filter; For the second time add 3 times of amounts that water is crude drug, boiled 1 hour; Decocting liquid is emitted through piping filter; Merge decocting liquid twice, be evaporated to 1/3 amount of fried liquid, emit standing over night; Draw supernatant, filter, filtrate continuation is concentrated under 60 ℃ of conditions heat, and to survey relative density be 1.35～1.38, and thick paste is measured water content and accurately metering; (2) preparation, granulation: get thick paste, add sodium cyclamate 8g, citric acid 8g stirs and makes dissolving; It is an amount of to take by weighing cane sugar powder 486g and dextrin, fully behind the mixing, adds the thick paste mixture, and mixing adds an amount of 95% ethanol and regulates the soft material humidity, and 16 mesh sieves are granulated, and granule finally makes infantile heat-clearing and antitussive granule 1000g in 75～80 ℃ of dryings.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102038775B (en) * | 2009-10-09 | 2012-10-31 | 北京亚东生物制药有限公司 | Preparation method of traditional Chinese medicine composition for treating cold in children |
| CN102579632A (en) * | 2012-04-09 | 2012-07-18 | 河南百年康鑫药业有限公司 | Preparation method of concentrated heat-clearing and cough-relieving oral solution for children |
| CN107773593A (en) * | 2016-08-30 | 2018-03-09 | 北京盈科瑞创新医药股份有限公司 | A kind of infantile heat-clearing and antitussive Neulized inhalation pharmaceutical solutions and preparation method thereof |
| CN107468951A (en) * | 2017-06-30 | 2017-12-15 | 成都恒凌科技有限公司 | A kind of anti-cough granules |
| CN112263551A (en) * | 2020-10-30 | 2021-01-26 | 重庆希尔安药业有限公司 | Spleen-tonifying and digestion-improving composition granules with excellent taste and preparation method thereof |
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|---|---|---|---|---|
| CN1660260A (en) * | 2004-12-09 | 2005-08-31 | 贵阳高新瑞得科技开发有限公司 | Effervescence grains of reducing fever and relieving a cough for infant and preparation method |
| CN1895398A (en) * | 2006-06-15 | 2007-01-17 | 贵州太和制药有限公司 | Preparation of infantie heating-clearing and antitussive effervescent particles |
| CN1939449A (en) * | 2005-09-30 | 2007-04-04 | 江西本草天工科技有限责任公司 | Infantile heat-clearing and antitussive dispersing tablets |
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|---|---|---|---|---|
| CN1660260A (en) * | 2004-12-09 | 2005-08-31 | 贵阳高新瑞得科技开发有限公司 | Effervescence grains of reducing fever and relieving a cough for infant and preparation method |
| CN1939449A (en) * | 2005-09-30 | 2007-04-04 | 江西本草天工科技有限责任公司 | Infantile heat-clearing and antitussive dispersing tablets |
| CN1895398A (en) * | 2006-06-15 | 2007-01-17 | 贵州太和制药有限公司 | Preparation of infantie heating-clearing and antitussive effervescent particles |
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