CN105079564A - Preparation method of fructus forsythiae antidotal tablet - Google Patents
Preparation method of fructus forsythiae antidotal tablet Download PDFInfo
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Abstract
The invention relates to a fructus forsythiae antidotal tablet and a preparation method of the fructus forsythiae antidotal tablet. The fructus forsythiae antidotal tablet is prepared through the preparation method which comprises the following steps: honeysuckle, fructus forsythia and fermented soybean are soaked with an appropriate volume of 50% ethanol, leachate is extracted, volatile oil in dregs of mint, herba schizonepetae, honeysuckle and fructus forsythia is extracted by a supercritical CO2 extraction method, wherein ethanol is used as a cosolvent, and after refining, the volatile oil is covered with beta-cyclodextrin; and lophatherum gracile, liquorice and great burdock achene are extracted through a continuous dynamic multiple extraction method, and residual dregs and liquor of the volatile oil are extracted; and the leachate and the extraction liquid are merged and concentrated, an auxiliary material is added in the concentrate to prepare a soft material, and platycodon grandiflorum powder and the volatile oil covered with beta-cyclodextrin are mixed in the soft material to prepare the fructus forsythiae antidotal tablet, wherein the weight of each tablet is 1.02 g. In the fructus forsythiae antidotal tablet, the contents of effective components with different solubility properties are all improved, the stability is enhanced, and besides, the exertion of the drug properties of the compatibility of the herbal pairs of monarch drugs is considered to the greatest degree in the preparation process of Chinese patent medicines. The fructus forsythiae antidotal tablet, disclosed by the invention, can exert the effects of expelling wind to resolve the exterior and clearing away heat and toxic materials, relieves corresponding cold symptoms, is low in irritation to stomach and intestine, is low in side effects, and has a good effect.
Description
Technical field:
The present invention relates to a kind of YINQIAO JIEDU PIAN with and preparation method thereof
Technical background:
The traditional Chinese medical science is thought, anemopyretic cold is the sign caused by heresy experiencing wind heat, is more common in summer and autumn." General Treatise on the Cause and Symptoms of Diseases wind heat time ": " wind heat patient, the gas of wind heat first enter lung also from fur.Lung is the five internal organs upper cover, and wait the fur of body, if the skin natural fibre line of meat is empty, then the gas of wind heat, first hinders fur, is into lung also.Its shape makes people's aversion to wind shiver with cold, and order is for de-, and tears saliva goes out.Control suitable relieving the exterior syndrome with drugs of pungent in flavor and cool in nature, disperse wind heat.Square Lonicerae and Forsythiae Powder, SANGJU YIN, Radix Platycodonis decoction, supernatant are loose, chrysanthemum powder forimproving etc." wherein Lonicerae and Forsythiae Powder be the main formula for anemopyretic cold, function cures mainly: dispelling wind to relieve the exterior syndrome, heat-clearing and toxic substances removing, disease see fever and headache, cough mouthfeel, have sore throat.
Li Shizhen (1518-1593 A.D.) just has following guidance for the preparation of Chinese medicine in Compendium of Materia Medica: " taking decoction though all makes thing specially smart, repairs and renovate as method, and decocts crude and rash hurried, and extreme misery is bad, duration and degree of heating mistake degree, then loss of drug potency." due to the transformation of modern life demand and progressing greatly of pharmaceutical technology, Chinese patent medicine become the main existence form of general side, ancient prescription accept by extensive patients, so preparation technology's choice and optimization of Chinese patent medicine is the key link ensureing drug effect.Lonicerae and Forsythiae Powder, as the representative of the ancient prescription medicine that induces sweat, method for making is also emphasized " fragrance goes out greatly, namely gets clothes, does not over-cook ", and being afraid of that " fragrance " runs off is exactly that volatile oil plays an important role inducing sweat in effect to the reservation of volatile oil effective ingredient.But the effective ingredient of Chinese crude drug is not merely volatile oil part, if Lonicerae and Forsythiae Powder Content of Chlorogenic Acid is organic acid, also have the effective ingredient such as flavonoid, lignanoids, triterpenes, alkaloids, inorganic elements; The chemical composition of Fructus Forsythiae is mainly lignanoid, oleanolic acid, ursolic acid and the triterpene acids such as volatile oil, phillyrin, phillyrin.Be not limited to the pharmacological model of certain chemical composition or applicable pure chemistry composition, but consider the effect of comprehensive composition.In spice leaching process, some composition may interact, and generates new compound, considers from drug metabolism processes, may be the compound action played in body in drug effect process.The composition that some independent medical materials do not have can be produced in the compatibility process that medicine is right.If but apply the mode of medical material compatibility decoction in present large-scale production, the extraction efficiency of effective ingredient is low and stability is also low in aqueous, and in order to the extraction ratio of pursuing principle active component and recall rate, independent extraction medicine, or untreated powder is used as medicine, just lose effect that medicine is right.
In comparison, Chinese Pharmacopoeia discloses prescription and the preparation method of YINQIAO JIEDU PIAN: Flos Lonicerae 200g, Fructus Forsythiae 200g, Herba Menthae 120g, Herba Schizonepetae 80g, Semen Sojae Preparatum 100g, Fructus Arctii (stir-fry) 120g, Radix Platycodonis 120g, Herba Lophatheri 80g, Radix Glycyrrhizae 100g.Above nine tastes, Flos Lonicerae, Radix Platycodonis are ground into fine powder respectively, sieve; Herba Menthae, Herba Schizonepetae extract volatile oil, and the another device of the aqueous solution after distillation is collected; Medicinal residues and Fructus Forsythiae, Fructus Arctii, Herba Lophatheri, Radix Glycyrrhizae decoct with water twice, each 2 hours, filter, merging filtrate; After Semen Sojae Preparatum adds water boil, in 80 DEG C of warm macerating secondaries, each 2 hours, merge leachate, filter.Merged with last medicinal liquid, be condensed into thick paste, add Flos Lonicerae, Radix Platycodonis fine powder and magnesium stearate 3g, to add starch or Pulvis Talci appropriate, mixing, makes granule, dry, lets cool, and spray adds Herba Menthae, Herba Schizonepetae volatile oil, and mixing, tabletted, or film coating, to obtain final product.Although this mode continues to use the mode that ancient prescription twice decoction merges medicinal liquid as much as possible, in modern production process, simple mode also greatly reduces the yield of effective ingredient, and drug effect is affected.
Chinese patent 201210516928.6 provides new a kind of refined lonicera-forsythia alexipharmic preparation and preparation method thereof, Herba Schizonepetae oil and Mentholum is made the preparation that alcoholic solution mixes with decoction medicinal liquid again.
Chinese patent 201310580207.6 provides a kind of preparation method of YINQIAO granule, joins by number material of getting it filled, and decocting mixing medical material is obtained granule finally.
Chinese patent 201410786635.9 provides a kind of preparation method of YINQIAO preparation, adopts Flos Lonicerae directly to pulverize to be used as medicine, mode that Fructus Forsythiae decocts separately, improves the content of effective main component.
In prior art, the preparation method of the medicinal liquids such as Herba Lophatheri, Semen Sojae Preparatum, Radix Glycyrrhizae, adopts decocting method more, and the present invention adopts continuously dynamically decoction medicinal liquid extracting method.
Therefore in this research, random choose is material in 3 wherein, measures the effective ingredient of the medicine that distinct methods extracts and compares.
(1) for the content of Radix Glycyrrhizae acid ammonium, the extraction efficiency of more each preparation method effective ingredient.Assay method is high performance liquid chromatography.
Chromatographic condition: with the strong silica gel that closes of octadecylsilane for filler; Acetonitrile-0.1% acetic acid (20:80) is mobile phase, and determined wavelength is 250nm, column temperature 40 DEG C.Number of theoretical plate should be not less than 3000, calculates by ammonium glycyrrhizinate peak.
Solution preparation:
The preparation of reference substance solution: extracting liquorice acid ammonium reference substance is appropriate, adds mobile phase and makes the solution of every 1ml containing 40 μ g, to obtain final product.
The preparation of need testing solution: extracting liquorice extract 0.1g, accurately weighed, put in 10ml measuring bottle, add the appropriate ultrasonic dissolution of mobile phase, and be diluted to scale, shake up, then get in the measuring bottle of 1ml to 10ml, add mobile phase to scale, shake up, to obtain final product.
Algoscopy: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, in injection liquid chromatography, measure and result of calculation.
Measurement result is rear as shown in table 5 as calculated.
The comparison of ammonium glycyrrhizinate content under the different extracting mode of table 3
| Tested number | Extracting method | Ammonium glycyrrhizinate content (mg/g) |
| Embodiment 1 | Continuous dynamic extraction method | 78.07 |
| Comparative example 1 and comparative example 3 | Decocting method | 61.93 |
(2) for Semen Sojae Preparatum polyoses content in Semen Sojae Preparatum, the extraction efficiency of extracting method to effective ingredient is compared.
The purification of Semen Sojae Preparatum polysaccharide: take the medicinal liquid in step (2) in embodiment 1 respectively, the medicinal liquid of step (2) in comparative example 1,2, the pepsin adding 3% (mass fraction) respectively removes foreign protein.Enzymatic hydrolysis condition PH=7, water bath with thermostatic control 60 DEG C, enzymolysis 1h, is then warming up to 90 DEG C, 6min enzymolysis reaction.Add 1.5% activated carbon adsorption small molecular weight impurity and desolventing technology, filter to obtain Semen Sojae Preparatum polysaccharide.
Then use dehydrated alcohol, acetone single extraction, 4000r/min high speed centrifugation 10min, precipitation is dried.Distilled water stalks 3 days, and precipitate with ethanol 12h, is settled to same volume, obtains determinand polysaccharide.
Get the polysaccharide solution sample 2ml purified respectively, Phenol-sulphate acid method develops the color, and surveys polysaccharide sample concentration at 490nm wavelength place, calculates content.
Polyoses content (g/g)=(sample concentration × reaction volume × extension rate/20g) × 100%
Measurement result is in table 6.
The detection of table 4 polyoses content
| Numbering | Extracting method | Semen Sojae Preparatum polyoses content (%) |
| Embodiment 1 | Alcohol reflux | 0.17 |
| Comparative example 1 and 2 | Decocting method | 0.08 |
Conclusion: in this product, the preparation method of the medicinal liquid such as Herba Lophatheri, Semen Sojae Preparatum, Radix Glycyrrhizae can effectively improve respective components content.
(3) for Folium Bambosae flavone content in Herba Lophatheri, the extraction efficiency of extracting method to effective ingredient is compared.
With C18ODS chromatographic column, with methanol: water=50:50 is mobile phase, take 360nm as determined wavelength, with red careless glycosides, Saponaretin for standard substance, measure the medicinal liquid in embodiment 1 step (3), and the content of Folium Bambosae flavone in medicinal liquid in comparative example 1 and 2 step (2), its result is as shown in table 7.
Table 5 Herba Lophatheri assay
| Numbering | Extracting method | Content (%) |
| Embodiment 1 | Alcohol reflux | 2.5 |
| Comparative example 1 and 3 | Decocting method | 1.72 |
Conclusion: in this product, the preparation method of the medicinal liquid such as Herba Lophatheri, Semen Sojae Preparatum, Radix Glycyrrhizae can effectively improve respective components content.
By the investigation to the preparation method of step (3) in embodiment 1, the predominant amount of 3 medicines in random mensuration admixing medical solutions, proves that the extracting method of preparation method step (3) herb liquid of the present invention and traditional decocting method have obvious superiority.
1.3.1 the medicinal liquid such as this product Herba Lophatheri, Semen Sojae Preparatum, Radix Glycyrrhizae extracts Study on influencing factors.
Adopt the medicinal liquid extracting method such as this product preparation process (3) middle Herba Lophatheri, Semen Sojae Preparatum, Radix Glycyrrhizae, the influence factor such as concentration of alcohol, soak time is investigated, and detects according to the detection method in 1.2.Its experimental result is as following table 8
The research of 1.4 Fructus Arctii extracting solution
In preparation method step (3) of the present invention, utilize the effective ingredient in ethanol extraction Fructus Arctii, thus decrease the extraction time in the independent extractive technique of Fructus Arctii.To this, the effective ingredient arctiin in this study tour step (3) extraction process in extracting solution carries out dynamic monitoring, to determine the optimum extraction time.
In step of the present invention (3), the assay method of arctiin is as follows:
(1) measuring condition:
Reference substance solution: it is appropriate that precision measures arctiin reference substance, adds the reference substance solution that methanol makes 0.05g/L.
Chromatographic condition C18 chromatographic column (4.6mm × 250mm, 5 μm), determined wavelength 280nm, column temperature 35 DEG C, flow velocity 1mL/min, mobile phase acetonitrile-water (20:80).
(2) detection method:
When first time extracts in step (3), measure extracting solution 3ml every 20min, cooling, supplies the ethanol of 60% of same volume at every turn; Second time measures 3ml extracting solution every 15min when extracting, and supplies the ethanol of 60% simultaneously.
After first time extracting solution cooling, measure supernatant 1ml, be placed in the measuring bottle of 10ml, add methanol constant volume to scale, filter through 0.45 μm of microporous filter membrane, and measure.
After the cooling of second time extracting solution, measure in supernatant 1ml to 5ml measuring bottle, add methanol constant volume to scale, filter through 0.45 μm of microporous filter membrane, and measure.Experimental result is as shown in following table 7 and 8.
The peak area rate of change of arctiin in table 6 first time extraction
| Time (min) | Peak area rate of change (%) |
| 0 | —————————————— |
| 20 | 256.31 |
| 40 | 98.13 |
| 60 | 61.45 |
| 80 | 27.85 |
| 100 | 42.78 |
| 120 | 5.31 |
| 140 | 4.87 |
| 160 | 2.44 |
| 180 | 1.15 |
| 200 | 0.77 |
| 220 | 0.81 |
The rate of change of arctiin peak area in the extraction of table 7 second time
| Time (min) | Peak area rate of change (%) |
| 0 | ———————————— |
| 15 | 32.89 |
| 30 | 11.19 |
| 45 | 5.11 |
| 60 | 1.45 |
| 75 | 1.31 |
| 90 | 1.22 |
Conclusion: first time is extracted in the basic < 4% of rate of change of peak area after 180min; Second time is extracted in the basic < 5% of rate of change of peak area after 60min, and therefore in the present invention, Fructus Arctii extracting solution primary extraction time is 180min, and the time that second time is extracted is 60min.
The research of the continuous dynamic extraction liquid of 1.5 monarch drug
In preparation method step (3) of the present invention, utilize the effective ingredient in continuous dynamic extraction monarch drug, to this, the special effective ingredient in this study tour step (3) extraction process in extracting solution carries out dynamic monitoring, to determine that medicine is to effectively.
Table 8 continuously dynamic extraction FAXIA monarch drug compares with the special of comparative example 4
Conclusion: this product monarch drug medicine can effectively improve respective components content to pair principle and compound recipe preparation method.
Summary of the invention:
An object of the present invention is to provide a kind of YINQIAO JIEDU PIAN;
Another object of the present invention is to provide a kind of preparation method of YINQIAO JIEDU PIAN.
In order to realize object of the present invention, technical scheme of the present invention is as follows:
The prescription of YINQIAO JIEDU PIAN: Flos Lonicerae 200g, Fructus Forsythiae 200g, Herba Menthae 120g, Herba Schizonepetae 80g, Semen Sojae Preparatum 100g, Fructus Arctii (stir-fry) 120g, Radix Platycodonis 120g, Herba Lophatheri 80g, Radix Glycyrrhizae 100g
One or both in the optional magnesium stearate of its adjuvant, hydroxypropyl emthylcellulose.
The present invention realizes by the following method, and its preparation method is
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae of recipe quantity, Fructus Forsythiae and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid;
(2) supercritical carbon dioxide fluid extraction volatile oil
Connect with the Flos Lonicerae of (1) after the Herba Menthae of recipe quantity, Herba Schizonepetae are pulverized 20 mesh sieves, stick up medicinal residues and mix and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100-250ml volumetric concentration be 95% ethanol do entrainer;
To extraction kettle, separating still separating still I, separating still II heats, and when extraction temperature is 25-45 DEG C, when separating still I temperature is 20-35 DEG C, opens CO
2gas cylinder, until extraction kettle pressure is 28-38MPa, when separating still I pressure is 5-8MPa, starts cycling extraction, regulates CO
2flow be 15 ~ 30kg/h, constant temperature and pressure extract, after 90-360min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Microwave after the crude drug mixing such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii is pulverized, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, heating temperatures to 60 ~ 75 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, and two pressure extracting storehouse can independently control, and alcohol concentration can independently be monitored.Add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 0.5 ~ 5%/min, reaction 1h-2.5h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 60 ~ 75 DEG C, adds water in extraction storehouse 1, regulates water velocity to make concentration of alcohol rate of change be 0.5 ~ 5%/min, and reaction 1h-2.5h is 10% to alcohol concentration.Extracting solution is filtered to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 2, regulate water velocity to make concentration of alcohol rate of change be 0.5 ~ 5%/min, reaction 1h-2.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir;
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
(1) (3) concentration of liquid medicine being dried to density is 1.05-1.15 (55 DEG C), and spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised the magnesium stearate mixing of volatile oil and recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, (4) 500, and every sheet weight is at 1.02g.
Beneficial effect of the present invention is: the Compatibility Law utilizing Flos Lonicerae, Fructus Forsythiae medicine right obtains, and drug effect is good and have the YINQIAO JIEDU PIAN of compatibility special nature.
Detailed description of the invention
Embodiment 1. YINQIAO JIEDU PIAN
Prescription: Flos Lonicerae 200g Herba Menthae 120g Semen Sojae Preparatum 100g Fructus Arctii (stir-fry) 120g Radix Platycodonis 120g Herba Lophatheri 80g Radix Glycyrrhizae 100g
Adjuvant: magnesium stearate and powder-beta-dextrin
Make: 500 1.02g
Preparation method:
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae Fructus Forsythiae of recipe quantity and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid,
(2) supercritical carbon dioxide fluid extraction volatile oil
Connect with the Flos Lonicerae of (1) after the Herba Menthae of recipe quantity, Herba Schizonepetae are pulverized 20 mesh sieves, stick up medicinal residues and mix and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100l volumetric concentration be 95% ethanol do entrainer;
To extraction kettle, separating still separating still I, separating still II heats, and when extraction temperature is 25 DEG C, when separating still I temperature is 20, opens CO
2gas cylinder, until extraction kettle pressure is 28MPa, when separating still I pressure is 5, starts cycling extraction, regulates CO
2flow be 15kg/h, constant temperature and pressure extract, after 100min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Microwave after the crude drug mixing such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii is pulverized, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, the heating temperatures to 60 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, and two pressure extracting storehouse can independently control, and alcohol concentration can independently be monitored.Add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 0.35%/min, reaction 2.5h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 60 DEG C, adds water in extraction storehouse 1, regulates water velocity to make concentration of alcohol rate of change be 0.35%/min, and reaction 2.5h is 10% to alcohol concentration.Extracting solution is filtered to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 3%/min, reaction 2.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir.
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
(1) (2) (3) concentration of liquid medicine being dried to density is 1.10-1.12 (60 DEG C), and spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised the magnesium stearate mixing of volatile oil and recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, (4) 500, and every sheet weight is at 1.02g.
Embodiment 2
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae Fructus Forsythiae of recipe quantity and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid,
(2) supercritical carbon dioxide fluid extraction volatile oil
Connect with the Flos Lonicerae of (1) after the Herba Menthae of recipe quantity, Herba Schizonepetae are pulverized 20 mesh sieves, stick up medicinal residues and mix and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100l volumetric concentration be 95% ethanol do entrainer;
To extraction kettle, separating still separating still I, separating still II heats, and when extraction temperature is 25 DEG C, when separating still I temperature is 20, opens CO
2gas cylinder, until extraction kettle pressure is 28MPa, when separating still I pressure is 5, starts cycling extraction, regulates CO
2flow be 15kg/h, constant temperature and pressure extract, after 100min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Most coarse powder will be ground into after the mixing of the crude drug such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, the heating temperatures to 70 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, and two pressure extracting storehouse can independently control, and alcohol concentration can independently be monitored.Add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 0.5%/min, reaction 1.5h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 70 DEG C, adds water in extraction storehouse 1, regulates water velocity to make concentration of alcohol rate of change be 0.5%/min, and reaction 1.5h is 10% to alcohol concentration.Extracting solution is filtered to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 2, regulate water velocity to make concentration of alcohol rate of change be 3%/min, reaction 1.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir.
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
(1) (2) (3) concentration of liquid medicine being dried to density is 1.10-1.12 (60 DEG C), and spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised the magnesium stearate mixing of volatile oil and recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, (4) 500, and every sheet weight is at 1.02g.
Embodiment 3
Prescription: Flos Lonicerae 200g Herba Menthae 120g Semen Sojae Preparatum 100g Fructus Arctii (stir-fry) 120g Radix Platycodonis 120g Herba Lophatheri 80g Radix Glycyrrhizae 100g
Adjuvant: magnesium stearate and powder-beta-dextrin
Make: 500 1.02g
Preparation method:
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae Fructus Forsythiae of recipe quantity and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid,
(2) supercritical carbon dioxide fluid extraction volatile oil
Connect with the Flos Lonicerae of (1) after the Herba Menthae of recipe quantity, Herba Schizonepetae are pulverized 20 mesh sieves, stick up medicinal residues and mix and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100l volumetric concentration be 95% ethanol do entrainer;
To extraction kettle, separating still separating still I, separating still II heats, and when extraction temperature is 25 DEG C, when separating still I temperature is 20, opens CO
2gas cylinder, until extraction kettle pressure is 28MPa, when separating still I pressure is 5, starts cycling extraction, regulates CO
2flow be 15kg/h, constant temperature and pressure extract, after 100min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Microwave after the crude drug mixing such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii is pulverized, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, the heating temperatures to 75 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, and two pressure extracting storehouse can independently control, and alcohol concentration can independently be monitored.Add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 4%/min, reaction 1h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 75 DEG C, adds water in extraction storehouse 1, regulates water velocity to make concentration of alcohol rate of change be 4%/min, and reaction 1h is 10% to alcohol concentration.Extracting solution is filtered to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 5%/min, reaction 1h is 10% to alcohol concentration, filters extracting solution to fluid reservoir.
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
(1) (3) concentration of liquid medicine being dried to density is 1.10-1.12 (60 DEG C), and spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised the magnesium stearate mixing of volatile oil and recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, (4) 500, and every sheet weight is at 1.02g.
Comparative example 1
Prescription: Flos Lonicerae 200g Herba Menthae 120g Semen Sojae Preparatum 100g Fructus Arctii (stir-fry) 120g Radix Platycodonis 120g Herba Lophatheri 80g Radix Glycyrrhizae 100g Fructus Forsythiae 200g
Adjuvant: magnesium stearate and starch
Make: 500 1.02g
Preparation method:
(1) Flos Lonicerae, the preparation of Radix Platycodonis fine powder
Flos Lonicerae in prescription, Radix Platycodonis are ground into respectively 20 object fine powders, sieve.
(2) way of distillation extracts volatile oil
Herba Menthae in prescription, Herba Schizonepetae are placed in the volatile oil extractor of steam distillation, add the water of 5 times amount, extract 4 hours, layering after condensation, collect aqueous solution and obtain volatile oil, medicinal residues are for subsequent use.
(3) compound recipe decoction liquor preparation
The medicinal residues of (2) and Fructus Forsythiae, Fructus Arctii, Herba Lophatheri, Radix Glycyrrhizae are decocted with water twice, each 2 hours, filter, merging filtrate.
(4) preparation of Semen Sojae Preparatum leachate
After Semen Sojae Preparatum adds water boil, in 80 DEG C of warm macerating secondaries, each 2 hours, merge leachate, filter.
(5) thick paste preparation
Merge the above each medicinal liquid of (2) (3) (4) step, be condensed into thick paste,
(6) preparation of YINQIAO JIEDU PIAN
Add Flos Lonicerae, Radix Platycodonis fine powder and magnesium stearate 3g, add starch in right amount, mixing, makes granule, dry, lets cool, and spray adds Herba Menthae, Herba Schizonepetae volatile oil, mixing, tabletted.
Comparative example 2
Prescription: Flos Lonicerae 200g Mentholum 0.6g Semen Sojae Preparatum 100g Fructus Arctii (stir-fry) 120g Radix Platycodonis 120g Herba Lophatheri 80g Radix Glycyrrhizae 100g Fructus Forsythiae 210g Herba Schizonepetae 80g
Adjuvant: magnesium stearate and starch
Make: 500 1.02g
Preparation method:
(1) Radix Platycodonis is pulverized
The acetaminophen of formula ratio and Radix Platycodonis are ground into fine powder respectively;
(2) Herba Schizonepetae oil is extracted
The Herba Schizonepetae of formula ratio was pulverized 10 orders, with 10 times amount water soaking 35min, discards water, directly logical Steam Heating, collects Aromatic water, carries to taste most, namely obtains Herba Schizonepetae oil after Aromatic water is refining;
(3) Herba Schizonepetae oil and Mentholum is dissolved
The Herba Schizonepetae oil of above-mentioned (2) and formula ratio and Mentholum are used 3 times of 90% dissolve with ethanol respectively, obtains Herba Schizonepetae oil dissolve with ethanol liquid and Mentholum alcoholic solution;
(4) all the other medicines are extracted
By Fructus Forsythiae, Semen Sojae Preparatum, Radix Glycyrrhizae, Herba Lophatheri, Flos Lonicerae, Fructus Arctii, drop in extraction pot in prescription ratio, first time adds 8 times amount drinking waters, soaks 3h, decocts and extracts 2h, filters; Second time adds 5 times amount drinking waters, and decoct and extract 2h, filtrate reduced in volume to proportion is 1.30g/ml (60 DEG C of surveys), goes out cream; Control temperature 70 ~ 80 DEG C, vacuum-0.05MPa ~-0.09MPa, drying under reduced pressure, by broken for dried cream powder mistake 80 order, obtains mixture dried cream powder;
(5) preparation is made
In the mixture dried cream powder of above-mentioned (4) step, add the Radix Platycodonis fine powder of (1) step, add the starch of 0.05g/ sheet, mixing, add the obtained suitable soft material of 85% ethanol, 16 mesh sieves are granulated, 60 ~ 70 DEG C of dryings, 16 mesh sieve granulate; Add Herba Schizonepetae oil alcoholic solution and the Mentholum alcoholic solution of above-mentioned (3) step again, add the micropowder silica gel of 1% and the magnesium stearate of 0.5%, mixing, inspection acetaminophen content, tabletting, to obtain final product.
Comparative example 3
Prescription: Flos Lonicerae 200g Herba Menthae 120g Semen Sojae Preparatum 100g Fructus Arctii (stir-fry) 120g Radix Platycodonis 120g Herba Lophatheri 80g Radix Glycyrrhizae 100g Fructus Forsythiae 200g Herba Schizonepetae 80g
Adjuvant: magnesium stearate and starch
Make: 0.5g/ sheet
Preparation method:
Flos Lonicerae, Radix Platycodonis are ground into fine powder respectively, sieve for subsequent use; Herba Menthae Herba Schizonepetae vapor distillation extracts volatile oil, and the another device of the aqueous solution after distillation is collected, for subsequent use; Medicinal residues and Fructus Arctii, Herba Lophatheri, Radix Glycyrrhizae add 10 times amount soak by water secondaries, each 2 hours, collecting decoction, filter; After Semen Sojae Preparatum adds water boil, in 80 DEG C of warm macerating secondaries, each 2 hours, merge leachate, filter; Merge above-mentioned medicinal liquid, be condensed into thick paste; Fructus Forsythiae adds 10 times amount soak by water secondaries, each 2 hours, collecting decoction, filters, is being condensed into thick paste; Add the starch of Flos Lonicerae and Radix Platycodonis fine powder and the amount of making 10%, mixing, makes granule, dry, lets cool, and spray adds Herba Menthae, Herba Schizonepetae volatile oil, mixing, tabletted.
Comparative example 4
Prescription: Flos Lonicerae 180g Fructus Forsythiae 180g
Steam distillation extracts volatile oil respectively, extracts 6h.Again with distilled water decocting herbs twice respectively, each 1.5 hours.Collecting decoction, filters.
Experimental example: the 1. research of preparation technology in each step of this product
1.1 monarch drug active substance content detection
The high effective liquid chromatography for measuring step below listing 2010 editions pharmacopoeial requirements detection Chlorogenic Acid of Flos Loniceraes and Phillyrin in Forsythia suspensa is played, and other organic acid substances are analyzed and content detection foundation 2010 editions pharmacopeia or conventional high-performance liquid chromatography equally.
Chromatographic condition and system suitability
Chromatographic condition and system suitability take octadecylsilane chemically bonded silica as filler; With acetonitrile-0.3% phosphoric acid solution (10:90) for mobile phase; Determined wavelength is 327nm.Number of theoretical plate is pressed chlorogenic acid peak and must not calculate lower than 3000.
The preparation of reference substance solution gets chlorogenic acid reference substance in right amount, accurately weighed, puts in brown measuring bottle, adds 50% methanol and make the solution not having 1ml to contain 30 μ g, to obtain final product.
This product 10 is got in the preparation of need testing solution, Film coated tablets removing coating, accurately weighed, porphyrize, get about 0.3g, accurately weighed, put in tool plug conical flask, precision adds 50% methanol 50ml, close plug, weighed weight, supersound process (power 250W, frequency 35kHz) 20 minutes, lets cool, weighed weight again, supplies the weight of less loss, shakes up with methanol, filter, get subsequent filtrate, to obtain final product.
Algoscopy is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
The every sheet of this product contains Flos Lonicerae with chlorogenic acid (C
16h
18o
9) meter, must not 2.7mg. be less than
Fructus Forsythiae is according to high effective liquid chromatography for measuring
Chromatographic condition and system suitability take octadecylsilane chemically bonded silica as filler; With acetonitrile-water (19:81) for mobile phase; Determined wavelength is 230nm.Number of theoretical plate is pressed phillyrin peak and must not calculate lower than 3000.
The preparation of reference substance solution gets phillyrin reference substance in right amount, accurately weighed, adds methanol and makes the solution not having 1ml to contain 25 μ g, to obtain final product.
This product 10 is got in the preparation of need testing solution, Film coated tablets removing coating, accurately weighed, porphyrize, get about 2g, accurately weighed, put in tool plug conical flask, precision adds 50% methanol 50ml, close plug, weighed weight, supersound process (power 250W, frequency 35kHz) 30 minutes, let cool, weighed weight again, the weight of less loss is supplied with methanol, shake up, filter, steam near dry, add central alumina 0.5g to mix thoroughly, be added in central alumina post (100 ~ 200 orders, 1g, internal diameter is 1 ~ 1.5cm) on, with 70% ethanol 80ml eluting, collect eluent, be concentrated into dry, residue adds 50% methanol makes dissolving in right amount, be transferred in 10ml measuring bottle, and be diluted to scale, shake up, filter, get subsequent filtrate, obtain.
Algoscopy is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
The every sheet of this product contains Fructus Forsythiae with phillyrin (C
27h
34o
11) meter, must not 0.50% be less than.
The extraction efficiency research at different conditions of table 1 Flos Lonicerae Fructus Forsythiae of the present invention leachate
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | |
| Chlorogenic acid peak area | 8567.2 | 8472.3 | 8698.6 | 7458.7 | 7314.6 | 7681.1 | 7416.5 |
| Chlorogenic acid content % | 4.01 | 3.61 | 4.23 | 5.97 | 5.82 | 6.11 | 5.79 |
| Caffeic acid peak area | 4124.3 | 4386.5 | 4076.3 | 5693.3 | 5628.4 | 5736..1 | 5578.2 |
| Caffeic acid content | 2.17 | 2.56 | 2.71 | 1.14 | 1.23 | 1.10 | 1.06 |
| Fructus Forsythiae ester glycoside peak area | 7459.6 | 7402.8 | 7318.6 | 5460.7 | 4738.1 | 5943.9 | 5261.3 |
| Fructus Forsythiae ester glycoside content % | 4.03 | 3.76 | 3.69 | 2.19 | 1.94 | 3.32 | 2.02 |
| Phillyrin peak area | 8327.6 | 8365.5 | 8419.3 | 5756.3 | 6315.9 | 6016.5 | 6120.4 |
| Determination of forsythin % | 5.68 | 5.73 | 5.81 | 3.39 | 3.76 | 3.43 | 3.54 |
The research of 1.2 Extraction Process of Volatile Oils
About the supercritical fluid extraction method of volatile oil in this product preparation process, all report in existing document.
About concentration and the relation proposing composition of entrainer ethanol, point out in prior art, when concentration >=90% of ethanol, be applicable to extracting volatile oil material, the concentration of alcohol that therefore this product adopts in volatile oil is drawn is generally 95%.
The present invention is carrying out supercritical CO to mixed material
2during extraction, extracting pressure, extraction temperature separating pressure, separation temperature, disengaging time carries out utilizing GC-MS analysis and investigation, and compares with existing document, obtains different results.Investigation of the present invention the results are shown in Table 1 and table 2.
The oil yield research of table 2 monarch drug
Conclusion: from table 1 and table 2, in Extraction Process of Volatile Oil of the present invention, under different condition, extract volatile oil component is large different with fuel-displaced effect; And adopt extracting method and the condition of volatile oil in the embodiment of the present invention 1, the volatile oil of desired substance can be obtained.
The 1.3 dynamic preparation method researchs decocting medicinal liquid continuously
Embodiment 2 zoopery
The 2.1 pairs of adenoviruss, coronavirus, human parainfluenza viruses, influenza A H1N1 influenza virus etc. therapeutical effect, and the change to mouse temperature
Body weight is suitable, and age in week is consistent, and the mice of sex random choose often organizes 10, and with the fatal dose lumbar injection infecting mouse of 85%, each group mice gastric infusion respectively, observes the therapeutical effect of this medicine to infected mice.In Table 11-14.
First group: adenovirus experimental group
Table 9
Second group: coronavirus experimental group
Table 10
3rd group: human parainfluenza viruses
Table 11
4th group: influenza A H1N1 influenza virus
Table 12
| Group | Often organize number of elements | Institute's drug | Mice survival rate (%) |
| 1 | 10 | According to tablet prepared by embodiment 1 | 88 |
| 2 | 10 | According to tablet prepared by embodiment 2 | 84 |
| 3 | 10 | According to tablet prepared by embodiment 3 | 87 |
| 4 | 10 | Prepared by Chinese Pharmacopoeia method | 65 |
| 5 | 10 | Normal saline | 25 |
Result shows: medicine of the present invention is to above virus inhibited (p<0.01)
3.2 medicines of the present invention are to the variable effect of body temperature
With escherichia coli endotoxin to after rabbit auricular vein injection pyrogenicity, observe the present invention to the impact of Temperature changing; With yeast be pyrogen to after rat skin lower injection, gastric infusion, observe the present invention to the effect of pyrogenicity rat temperature.
Rabbit group:
Table 13
Mice group:
Table 14
Result shows: medicine of the present invention can be good at body temperature rising (p<0.05) reduced and improve because viral infection etc. causes, and has stronger effect of bringing down a fever.
Claims (4)
1. a YINQIAO JIEDU PIAN, it is characterized in that, its main component comprises Flos Lonicerae 200g, Fructus Forsythiae 200g, Herba Menthae 120g, Herba Schizonepetae 80g, Semen Sojae Preparatum 100g, Fructus Arctii (stir-fry) 120g, Radix Platycodonis 120g, Herba Lophatheri 80g, Radix Glycyrrhizae 100g, adjuvant is one or more in starch, dextrin, magnesium stearate, and its preparation method is:
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae of recipe quantity, Fructus Forsythiae and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid;
(2) supercritical carbon dioxide fluid extraction volatile oil
Mixed with the Flos Lonicerae of (1), Fructus Forsythiae medicinal residues after the Herba Menthae of recipe quantity, Herba Schizonepetae were pulverized 20 mesh sieves and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100-250ml volumetric concentration be 95% ethanol do entrainer;
Extraction kettle, separating still I, separating still II are heated, when extraction temperature is 25-45 DEG C, when separating still I temperature is 20-35 DEG C, opens CO
2gas cylinder, until extraction kettle pressure is 28-38MPa, when separating still I pressure is 5-8MPa, starts cycling extraction, regulates CO
2flow be 15 ~ 30kg/h, constant temperature and pressure extract, after 90-360min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Microwave after the crude drug mixing such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii is pulverized, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, heating temperatures to 60 ~ 75 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, two pressure extracting storehouse can independently control, alcohol concentration can independently be monitored, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 0.5 ~ 5%/min, reaction 1h-2.5h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 60 ~ 75 DEG C, adds water in extraction storehouse 1, water velocity is regulated to make concentration of alcohol rate of change be 0.5 ~ 5%/min, reaction 1h-2.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 2, regulate water velocity to make concentration of alcohol rate of change be 0.5 ~ 5%/min, reaction 1h-2.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir;
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
It is 1.05-1.15(55 DEG C that (1) (3) concentration of liquid medicine is dried to density), spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised volatile oil, the Radix Platycodonis fine powder of (4) and the magnesium stearate mixing of recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, 500, and every sheet weight is at 1.02g.
2. YINQIAO JIEDU PIAN according to claim 1, is characterized in that: its adjuvant is magnesium stearate, beta-schardinger dextrin-.
3. YINQIAO sheet according to claim 1, is characterized in that, its preparation method is
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae Fructus Forsythiae of recipe quantity and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid;
(2) supercritical carbon dioxide fluid extraction volatile oil
Connect with the Flos Lonicerae of (1) after the Herba Menthae of recipe quantity, Herba Schizonepetae are pulverized 20 mesh sieves, stick up medicinal residues and mix and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100ml volumetric concentration be 95% ethanol do entrainer;
To extraction kettle, separating still I, separating still II heats, and when extraction temperature is 25 DEG C, when separating still I temperature is 20, opens CO
2gas cylinder, until extraction kettle pressure is 28MPa, when separating still I pressure is 5MPa, starts cycling extraction, regulates CO
2flow be 15kg/h, constant temperature and pressure extract, after 100min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Microwave after the crude drug mixing such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii is pulverized, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, the heating temperatures to 60 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, two pressure extracting storehouse can independently control, alcohol concentration can independently be monitored, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 0.35%/min, reaction 2.5h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 60 DEG C, adds water in extraction storehouse 1, regulates water velocity to make concentration of alcohol rate of change be 0.35%/min, and reaction 2.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 3%/min, reaction 2.5h is 10% to alcohol concentration, filters extracting solution to fluid reservoir;
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
It is 1.10-1.12(60 DEG C that (1) (3) concentration of liquid medicine is dried to density), spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised volatile oil, the Radix Platycodonis fine powder of (4) and the magnesium stearate mixing of recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, 500, and every sheet weight is at 1.02g.
4. YINQIAO sheet according to claim 1, is characterized in that, its preparation method is
(1) Flos Lonicerae Fructus Forsythiae, Semen Sojae Preparatum leachate extract:
By the Flos Lonicerae Fructus Forsythiae of recipe quantity and Semen Sojae Preparatum respectively with 50% of 2 times of volumes soak with ethanol and fully stir, mixing speed 180rpm/min, 2 hours first times, second time 2 hours, filter, merge two-stage leaching liquid;
(2) supercritical carbon dioxide fluid extraction volatile oil
Connect with the Flos Lonicerae of (1) after the Herba Menthae of recipe quantity, Herba Schizonepetae are pulverized 20 mesh sieves, stick up medicinal residues and mix and drop into supercritical CO
2in the extraction kettle of extractor, and add in extraction kettle 100ml volumetric concentration be 95% ethanol do entrainer;
To extraction kettle, separating still separating still I, separating still II heats, and when extraction temperature is 25 DEG C, when separating still I temperature is 20, opens CO
2gas cylinder, until extraction kettle pressure is 28MPa, when separating still I pressure is 5MPa, starts cycling extraction, regulates CO
2flow be 15kg/h, constant temperature and pressure extract, after 100min, collect volatile oil slightly oily; Above-mentioned volatile oil residue is collected for subsequent use, and by mixed volatile oil anhydrous alcohol solution sucking filtration 2 times, removing residue, Rotary Evaporators reclaims ethanol, calculates oil-collecting ratio and comprises volatile oil with beta-schardinger dextrin-after collecting;
(3) preparation of the medicinal liquid such as Herba Lophatheri, Radix Glycyrrhizae, Fructus Arctii
Microwave after the crude drug mixing such as the Herba Lophatheri of recipe quantity, Radix Glycyrrhizae, Fructus Arctii is pulverized, drop in the extraction storehouse 1 of continuous extractor, 95% ethanol adding 3 times of volumes is that stirring solvent soaks 30min, the heating temperatures to 75 DEG C in storehouse 1 and temperature controlled water tank will be extracted, water tank can add water respectively to extraction storehouse 1,2, flow can adjust in good time, two pressure extracting storehouse can independently control, alcohol concentration can independently be monitored, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 4%/min, reaction 1h is 50% to alcohol concentration; Passed into by first set reaction extracting solution and extract storehouse 2, medicinal residues are still stayed and are extracted storehouse 1; 50% ethanol adding 3 times of volumes in extraction storehouse 1 is stirring solvent, is heated to 75 DEG C, adds water in extraction storehouse 1, regulates water velocity to make concentration of alcohol rate of change be 4%/min, and reaction 1h is 10% to alcohol concentration, filters extracting solution to fluid reservoir; Dropped into by (2) medicinal residues and extract storehouse 2, add water in extraction storehouse 1, regulate water velocity to make concentration of alcohol rate of change be 5%/min, reaction 1h is 10% to alcohol concentration, filters extracting solution to fluid reservoir;
(4) Radix Platycodonis fine powder preparation
The Radix Platycodonis of recipe quantity is pulverized and sieved rear mixing, for subsequent use;
(5) preparation of thick paste:
It is 1.10-1.12(60 DEG C that (1) (3) concentration of liquid medicine is dried to density), spraying dry, obtains dry extract;
(6) preparation of YINQIAO JIEDU PIAN
The beta-schardinger dextrin-that dry extract, (2) obtain is comprised volatile oil, the Radix Platycodonis fine powder of (4) and the magnesium stearate mixing of recipe quantity, tabletting, film coating makes YINQIAO JIEDU PIAN, 500, and every sheet weight is at 1.02g.
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Cited By (4)
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| CN105748980A (en) * | 2016-02-26 | 2016-07-13 | 南京正亮医药科技有限公司 | Preparation method and application of Yinqiao detoxification granules |
| CN106641846A (en) * | 2016-12-30 | 2017-05-10 | 郭子颖 | Spirit refreshing LED reading lamp |
| WO2021213059A1 (en) * | 2020-04-23 | 2021-10-28 | 江苏康缘药业股份有限公司 | Use of traditional chinese medicine composition in preparation of drug for treating or preventing coronavirus infection |
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