CN101134056B - A Chinese medicinal composition for preventing and treating influenza, and its preparation method - Google Patents
A Chinese medicinal composition for preventing and treating influenza, and its preparation method Download PDFInfo
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Abstract
本发明公开了一种用于预防和治疗流行性感冒的中药组合物及制备方法，其特征在于该中药组合物是由紫锥菊和板蓝根二味中药材组成。本发明首先用乙醇溶液提取紫锥菊中的有效成分，提取后的药渣再与板蓝根一起提取，充分将紫锥菊与板蓝根中的有效成分提取出来得到主药，将主药中加入药剂学上可以接受的药用辅料，用常规制药工艺制备成制剂。本发明中药组合物质量稳定，环境污染小，适于大工业生产。药理试验表明，本发明组合物对流感病毒有较强的抑制作用，并可增强免疫机能。The invention discloses a traditional Chinese medicine composition for preventing and treating influenza and a preparation method, which is characterized in that the traditional Chinese medicine composition is composed of echinacea purpurea and Radix isatidis. In the present invention, the active ingredients in Echinacea purpurea are firstly extracted with ethanol solution, and the extracted dregs are extracted together with Radix Radix, and the active ingredients in Echinacea Purpurea and Radix Radix are fully extracted to obtain the main drug, and pharmaceutically acceptable ingredients are added to the main drug. Pharmaceutical excipients are prepared into preparations by conventional pharmaceutical techniques. The traditional Chinese medicine composition of the invention has stable quality, less environmental pollution and is suitable for large-scale industrial production. Pharmacological tests show that the composition of the invention has strong inhibitory effect on influenza virus and can enhance immune function.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicine pharmacy, be specifically related to a kind of grippal Chinese medicine composition and preparation method thereof that is used for preventing and treating.
Background technology
Influenza is the common acute respiratory infectious disease that is caused by virus, and transmissibility is strong, and it is popular often to be endemicity, and mainly by three viroids: first type, B-mode and influenza virus C cause.Be used for prevention at present and treat grippal kind a lot, especially based on Western medicine, but the Western medicine side effect is big, and virus also produces drug resistance to it easily, tackles novel variant virus poor effect.And Chinese medicine has certain characteristic in the treatment influenza, and " pestilence " repeatedly in history all embodies unique curative effect of Chinese medicine.
Echinacea (Echinaceapurpurea Moench) comes from each state of Northeastern United States to southern Texas one band, used by American Indian the earliest, be used for various types of infection, have antiviral, anti-inflammation, antitumor, preventing cold, improve the effect of immunity, become the North America first preventing cold medication.Studies show that, Echinacea contains plurality of active ingredients such as polysaccharide, caffeic acid derivant, volatile oil, alkylamide and flavonoid, wherein polysaccharide, caffeic acid derivant and alkylamide compound have stronger physiologically active, are the main component of antiinflammatory, antiviral, immunostimulant.The ethanol extraction of Echinacea root has certain facilitation to granulocytic phagocytic function.Echinacea crude polysaccharides (EPS) but 100ug obvious stimulation macrophage kills and wounds the activity of P815 oncocyte, its intensity is similar to 0.1667umol/s (10U) macrophage activating factor (MAF).The genus echinacea plant is used in North America and the traditional anti-inflammatory drug of European Ceng Zuowei.The polyunsaturated isobutyl group phthalein amine that the root of this platymiscium and aerial parts are contained has immunoregulatory function, and the inflammation that can stop pathogen to cause has stronger anti-inflammatory activity, can be used for bacterial infection.
Radix Isatidis (Radix Isatidis) is the dry root of cruciferae isatis Isatis indigotica Fort..Use Radix Isatidis injection to do the antiviral experiment, proving has the infection of inhibition and the inhibition proliferation function is arranged influenza A virus, encephalitis b virus, mumps virus, influenza virus.Utilize chick embryo amnoitic sac half intracorporal method to carry out the anti-influenza virus activity experiment, the effective site of screening Radix Isatidis resisiting influenza virus, experimental result shows that active site is in conjunction with aminoacid.Investigate the inhibitory action of the Radix Isatidis of 15 germplasms to influenza A virus with chick embryo method, the experiment of blood clotting titre shows that the water extract-alcohol precipitation liquid of Radix Isatidis is respectively 100%, 60%, 70% to direct effect, therapeutical effect, the preventive effect effective percentage of virus.Lumbar injection Radix Isatidis polysaccharide 50mg/kg can significantly promote immune function of mice.Can increase obviously that the normal mouse spleen is heavy, total white blood cells and lymphocyte number, the reduction that immunologic function due to the hydrocortisone is suppressed mouse spleen index, total white blood cells and lymphocyte number has obvious antagonism; Significantly strengthen the delayed hypersensitivity of normal and caused by cyclophosphamide immunosuppressed mice; Strengthen normal mouse peripheral blood lymphocyte ANAF positive percentage, and obviously resist the immunosuppressive action due to the HC; Promote the mononuclear phagocyte system function, obviously strengthen antibody forming cell's function; Increase the quiet notes carbon clearance of mice speed.
Summary of the invention
Research worker of the present invention is through great deal of experimental, Echinacea and Radix Isatidis two flavor Chinese medicines are concerned prescription according to a certain ratio, at first with the effective ingredient in the alcoholic solution extraction Echinacea, medicinal residues after the extraction extract with Radix Isatidis again, fully the extracts active ingredients in Echinacea and the Radix Isatidis is come out to obtain principal agent, with adding acceptable pharmaceutic adjuvant on the pharmaceutics in the principal agent, be prepared into preparation with conventional pharmaceutical technology.Chinese medicine composition steady quality of the present invention, environmental pollution is little, is suitable for big commercial production.Pharmacological testing shows that the present composition has stronger inhibitory action to influenza virus, but and enhance immunity function.
The purpose of this invention is to provide a kind of determined curative effect, little being used for prevention and treating grippal Chinese medicine composition of untoward reaction.
Another object of the present invention provides a kind of preparation method of preventing and treating grippal Chinese medicine composition.
The present invention is achieved through the following technical solutions:
One, process recipes
(1) prescription raw material medicines in portions by weight proportioning:
Echinacea 20-180, Radix Isatidis 20-180;
(2) get the Echinacea medical material, pulverize, add alcohol reflux 1-3 time that 8-12 doubly measures 70%-95%, each 1-2 hour, filter, merging filtrate, 55 ± 5 ℃ of concentrating under reduced pressure, 60 ± 5 ℃ of vacuum dryings must extract I;
(3) get the Radix Isatidis medical material, pulverize, mix with filtering residue after Echinacea extracts, 6-10 doubly measures alcohol reflux 1-3 time of 15%-60%, each 1-2 hour, filter, merging filtrate, 60 ± 5 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, add the ethanol of 15%-25% in the extractum, amount of alcohol added is 2-3ml in every gram extractum, and dissolving refluxes, room temperature cools, 4 ± 2 ℃ of refrigerators were placed 12-36 hour, filtered and obtained supernatant, and it is stand-by to collect insoluble matter, it is 1.1-1.5 that supernatant continues to be evaporated to relative density of medicine liquid, the ethanol that adds 80%-95% transfers determining alcohol to carry out precipitate with ethanol, makes it contain the alcohol amount and is 35%-75%, and room temperature left standstill 16-32 hour, filter, 60 ± 5 ℃ of concentrating under reduced pressure of supernatant, 55 ± 10 ℃ of vacuum dryings get extract II;
(4) above-mentioned insoluble matter is dissolved in water goes up column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 60 ± 5 ℃ of concentrating under reduced pressure, 55 ± 10 ℃ of vacuum dryings get extract II I;
(5) united extraction thing I, II, III, pulverize the back mixing, be principal agent,, be prepared into capsule, tablet, granule, oral liquid, syrup, pill, drop pill, sustained-release preparation with conventional pharmaceutical technology with adding acceptable pharmaceutic adjuvant on the pharmaceutics in the principal agent.
The proportioning of Echinacea and Radix Isatidis is 1-9: 1-9 in the Chinese medicine composition of the present invention.
Pharmaceutical preparation of the present invention, its preparation can contain excipient commonly used, such as binding agent, diluent, disintegrating agent, wetting agent, filler, lubricant, correctives, can carry out coating to tablet in case of necessity.Binding agent can be polyvidone, starch slurry, cellulose etc.; Diluent can be starch, dextrin, Icing Sugar, lactose etc.; Disintegrating agent can be dry starch, sodium carboxymethyl cellulose, low-substituted hydroxypropyl cellulose; Wetting agent can be water or ethanol; Filler can be starch, microcrystalline Cellulose, pregelatinized Starch; Lubricant can be Pulvis Talci, stearic acid, calcium stearate magnesium, calcium stearate; Correctives can be that sucrose, A Siba are sweet, steviosin, fructose etc.
Column chromatography described in the process recipes of the present invention be macroporous adsorbent resin column chromatography, polyamide column chromatography, siliceous earth column chromatography, cellulose chromatography, activated carbon column chromatography, alumina column chromatography.
Column chromatography described in the process recipes of the present invention can be used alone, but also also mix together.
Medicine of the present invention has the function of heat-clearing and toxic substances removing, removing heat from blood sore-throat relieving, antibiotic, antiviral, enhance immunity, and influenza virus is had stronger inhibitory action, is used for prevention and treatment influenza.
Two, pharmacology embodiment
Reagent: preparation group of the present invention (, providing), Radix Isatidis granule (commercially available product) by Beijing XingHao JiaYu Pharmaceutical Technology Co., Ltd's Chinese medicine laboratory by preparation technology's preparation of the present invention;
Animal: Kunming kind white mice, body weight 13-15g;
1. antipyretic and antidote functions
Get 40 of Kunming white mice, body weight 13-15g, the male and female dual-purpose is divided into four groups at random, 10 every group.One group of negative matched group wherein, the abdominal cavity gives 0.9% normal saline; One group of positive matched group, the abdominal cavity gives Radix Isatidis granule; Two groups are Chinese medicine composition group of the present invention, intraperitoneal administration in addition.With the escherichia coli endotoxin modeling.Write down the body temperature after 1 hour, 2 hours, 4 hours, 6 hours, the results are shown in Table 1
The effect of fervescence due to the table 1 Chinese medicine composition escherichia coli endotoxin of the present invention
As seen from the above table, Chinese medicine composition low dosage of the present invention and high dose group all have certain reduction effect to the fervescence that is caused by escherichia coli endotoxin, can keep action time 4 hours.
2. antivirus action
(1) to the influence of Influenza A1 virus FM1 strain infecting mouse mortality rate
Seed culture of viruses: Influenza A1 virus FM1 Mus lung adapted strain (identifies that by the Chinese biological goods institute provides, and after mice strengthens virulence, goes down to posterity 2 times in the Embryo Gallus domesticus blister cavities, and measures its median lethal dose(LD 50) LD
50).
Getting seed culture of viruses before the experiment is diluted to every 0.05mL with physiological saline solution and contains 8 LD
50, put in the frozen water and preserve.Get the Kunming white mice, body weight 13-15g, male and female half and half are pressed grouping shown in the table 2.Under the slight anesthesia of ether, with titration influenza virus drop nose infection, 4 of every Mus, about 0.05mL.The administration group all begins gastric infusion according to dosage in viral infection the previous day, and the virus control group gives the equal-volume distilled water, every day 1 time, continuous 12 days.Day by day observe animal disease symptom and death toll, observed altogether 15 days.The result shows that mean survival time, the survival rate of two dosage groups of Chinese medicine composition of the present invention mice all are higher than the virus control group, and with the corresponding increase of increase mean survival time, survival rate of dosage, observed result sees Table 2.
(2) to the influence of Influenza A1 virus FM1 strain infecting mouse lung weight
Grouping, modeling, administration are the same, every day 1 time, continuous 4 days.Infected back 4 days, cut open mice extremely, fasting was prohibited water more than 24 hours before cuing open extremely, claimed the mice body weight, put to death mice, take out the Mus lung, write down lesion degree, lung is placed in the flat butterfly that fills 0.9% physiology basin water washs secondary, blot surface moisture with absorbent paper, claim lung heavy, calculate lung exponential sum lung index suppression ratio.The result shows that the lung index of two dosage groups of Chinese medicine composition of the present invention all is lower than the virus control group, the results are shown in Table 3.
Table 2 Chinese medicine composition of the present invention is to the influence of Influenza A1 virus FM1 strain infecting mouse mortality rate
Compare with matched group:
*P＜0.05,
*P＜0.01
Table 3 Chinese medicine composition of the present invention is to the influence of Influenza A1 virus FM1 strain infecting mouse lung weight
Compare with matched group:
*P＜0.05,
*P＜0.01
Pharmacological testing shows that Chinese medicine composition of the present invention has significant antivirus action.
3. to the regulating action of immunologic function
The medicinal liquid preparation: Radix Isatidis granule is made into the solution of 4mg/mL
Chinese medicine composition of the present invention is made into the solution of 4mg/mL, 2mg/mL
40 of Kunming white mice are got in animal grouping and processing. be divided into 4 groups at random.Experimental group difference each Chinese medicine ingredients of lumbar injection every 0.2mL/ days.Every 0.2mL/ of matched group intraperitoneal injection of saline days, continuous 7 days.Back 24 hours of last injection, every mouse peritoneal is injected 8% peptone solution 2ml.Every eye socket blood sampling in 24 hours, heparin (500IU/mL) anticoagulant added in the equivalent D-Hank ' s liquid, is used to measure peripheral blood lymphocyte propagation again.Draw dead mice immediately, lumbar injection sterilization D-Hank ' s liquid 8mL collects the abdominal cavity washing liquid and is used to measure the peritoneal macrophage activity; The aseptic spleen of taking is made single splenocyte suspension simultaneously, is used to measure spleen lymphocyte propagation.
Lymphopoiesis is measured and is used the MTT colorimetry.Get above-mentioned anticoagulation and single splenocyte suspension and add the lymphocyte separation medium isolated lymphocytes.Cell number is adjusted to 5x10
6/ mL is inoculated on 96 well culture plates, every hole 200uL.Experimental port adds ConA (con A, final concentration 5ug/mL) or LPS (lipopolysaccharide, final concentration 20ug/mL), all repeats 4 holes, establishes acellular hole simultaneously as the zeroing hole.At 37 ℃, 5%CO
2Cultivated 72 hours in the incubator.Cultivate and finish preceding 4 hours every hole adding MTT (5mg/mL) 10uL, cultivate and finish to add DMSO 100uL dissolved cell.Measure each hole A with microplate reader in the 10min
570Value is as judging lymphopoietic index.The result is with the A of each group
570Meansigma methods is represented (getting n=4), the results are shown in Table 4.
The peritoneal macrophage determination of activity: get above-mentioned abdominal cavity washing liquid in the centrifugal 10min of 1000r/min, resuspended with 3mLD-Hank ' s liquid, centrifuge washing is 1 time again; Resuspended with 1640 complete culture solutions, carry out cell counting (1x10
6/ mL).Every group of cell suspension 100uL repeats 4 holes, put cultivate 2h in 37 ℃, 5%C02 incubator after, renew bright RPMI-1640.After continuing to hatch 2 hours, each hole adds 10uL MTT, jog 1min, and incubation 4 hours adds DMSO, and concussion 30s surveys A
570Value.The result is with the A of each group
570Meansigma methods is represented (getting n=4), the results are shown in Table 4.
Table 4 Chinese medicine composition of the present invention is to the influence (A of mouse lymphocyte increment, Turnover of Mouse Peritoneal Macrophages
570)
Compare with matched group:
*P＜0.05,
*P0.01
Pharmacological tests shows that Chinese medicine composition of the present invention has the effect that improves immunologic function.
Last table result shows that Chinese medicine composition high dose group of the present invention has extremely significant potentiation to by in the inductive mice peripheral blood lymphocyte of ConA, the spleen lymphocyte increment reaction, and Radix Isatidis group and low dose group have significant potentiation; In the inductive reaction that spleen lymphocyte is rised in value by LPS, the high dose group effect is extremely remarkable, and Radix Isatidis and low dosage Chinese medicine composition group of the present invention has significant effect.Compare with matched group, but the Chinese medicine composition high dose group utmost point of the present invention improves the activity of Turnover of Mouse Peritoneal Macrophages significantly, low dose group can improve the Turnover of Mouse Peritoneal Macrophages activity significantly, and the effect of Radix Isatidis group is not remarkable.
Three, preparation embodiment
Embodiment 1
(1) get Echinacea 500g medical material, pulverize, add the alcohol reflux 1 time of 8 times of amounts 70%, 2 hours extraction times, filter, merging filtrate, 50 ℃ of concentrating under reduced pressure, 55 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis 500g medical material, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 6 times of amounts 15% 1 time, filters at 2 hours extraction times, merging filtrate, 55 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 15% in the extractum, amount of alcohol added is 2ml in every gram extractum, dissolving refluxes, room temperature cools, 2 ℃ of refrigerators were placed 12 hours, filtered and obtained supernatant, and it is stand-by to collect insoluble matter, it is 1.1 that supernatant continues to be evaporated to relative density of medicine liquid, add 80% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 35%, and room temperature left standstill 16 hours, filter, 55 ℃ of concentrating under reduced pressure of supernatant, 45 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up macroporous adsorbent resin column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 55 ℃ of concentrating under reduced pressure, 45 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, and principal agent is packed in the snap fit capsule, promptly get capsule.
Embodiment 2
(1) get Echinacea medical material 100g, pulverize, add the alcohol reflux 3 times of 12 times of amounts 95%, each 2 hours, filter, merging filtrate, 65 ℃ of concentrating under reduced pressure, 65 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis medical material 900g, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 10 times of amounts 60% 3 times each 2 hours, filters, merging filtrate, 65 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 25% in the extractum, amount of alcohol added is 3ml in every gram extractum, dissolving refluxes, room temperature cools, 6 ℃ of refrigerators were placed 36 hours, filtered and obtained supernatant, and it is stand-by to collect insoluble matter, it is 1.5 that supernatant continues to be evaporated to relative density of medicine liquid, add 95% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 75%, and room temperature left standstill 32 hours, filter, 65 ℃ of concentrating under reduced pressure of supernatant, 65 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up polyamide column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 65 ℃ of concentrating under reduced pressure, 65 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, add ethanol at principal agent and do binding agent, add starch and do filler, make granule.
Embodiment 3
(1) get Echinacea medical material 900g, pulverize, add the alcohol reflux 2 times of 9 times of amounts 75%, each 1.2 hours, filter, merging filtrate, 55 ℃ of concentrating under reduced pressure, 58 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis medical material 100g, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 7 times of amounts 25% 2 times each 1.2 hours, filters, merging filtrate, 58 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 17% in the extractum, amount of alcohol added is 2.2ml in every gram extractum, dissolving refluxes, room temperature cools, 3 ℃ of refrigerators were placed 16 hours, filtered and obtained supernatant, and it is stand-by to collect insoluble matter, it is 1.2 that supernatant continues to be evaporated to relative density of medicine liquid, add 85% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 45%, and room temperature left standstill 20 hours, filter, 58 ℃ of concentrating under reduced pressure of supernatant, 50 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up the siliceous earth column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 58 ℃ of concentrating under reduced pressure, 50 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, add adjuvant, wetting agent, make granule, and drying is sieved, granulate, and compacting is in flakes.
Embodiment 4
(1) get Echinacea medical material 300g, pulverize, add the alcohol reflux 3 times of 10 times of amounts 80%, each 1.4 hours, filter, merging filtrate, 58 ℃ of concentrating under reduced pressure, 60 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis medical material 700g, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 8 times of amounts 35% 3 times each 1.4 hours, filters, merging filtrate, 60 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 20% in the extractum, amount of alcohol added is 2.4ml in every gram extractum, dissolving refluxes, room temperature cools, 4 ℃ of refrigerators were placed 20 hours, filtered and obtained supernatant, and it is stand-by to collect insoluble matter, it is 1.3 that supernatant continues to be evaporated to relative density of medicine liquid, add 90% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 55%, and room temperature left standstill 22 hours, filter, 60 ℃ of concentrating under reduced pressure of supernatant, 55 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up cellulose chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 60 ℃ of concentrating under reduced pressure, 55 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, and principal agent is joined in the molten matrix, and mixing is made drop pill.
Embodiment 5
(1) get Echinacea medical material 400g, pulverize, add the alcohol reflux 2 times of 11 times of amounts 85%, each 1.6 hours, filter, merging filtrate, 60 ℃ of concentrating under reduced pressure, 62 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis medical material 600g, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 9 times of amounts 50% 2 times each 1.6 hours, filters, merging filtrate, 62 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 22% in the extractum, amount of alcohol added is 2.6ml in every gram extractum, dissolving refluxes, room temperature cools, 5 ℃ of refrigerators were placed 24 hours, filtered and obtained supernatant, and it is stand-by to collect insoluble matter, it is 1.4 that supernatant continues to be evaporated to relative density of medicine liquid, add 90% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 60%, and room temperature left standstill 24 hours, filter, 62 ℃ of concentrating under reduced pressure of supernatant, 60 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up activated carbon column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 62 ℃ of concentrating under reduced pressure, 60 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, and principal agent is dissolved in water, and stirs evenly; Other gets sucrose and makes syrup, merges with above-mentioned medicinal liquid, stirs evenly, and filters, and oral liquid is made in fill.
Embodiment 6
(1) get Echinacea medical material 600g, pulverize, add the alcohol reflux 3 times of 10 times of amounts 90%, each 1.8 hours, filter, merging filtrate, 62 ℃ of concentrating under reduced pressure, 64 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis medical material 400g, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 10 times of amounts 55% 3 times each 1.8 hours, filters, merging filtrate, 64 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 24% in the extractum, amount of alcohol added is 2.8ml in every gram extractum, dissolving refluxes, room temperature cools, 4.5 ℃ refrigerator was placed 30 hours, filtered to obtain supernatant, it is stand-by to collect insoluble matter, it is 1.25 that supernatant continues to be evaporated to relative density of medicine liquid, add 92% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 65%, and room temperature left standstill 26 hours, filter, 64 ℃ of concentrating under reduced pressure of supernatant, 62 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up alumina column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 64 ℃ of concentrating under reduced pressure, 62 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, and principal agent is dissolved in water, and stirs evenly, and adds simple syrup and sodium benzoate, stirs evenly, and filters, and promptly gets syrup.
Embodiment 7
(1) get Echinacea medical material 700g, pulverize, add the alcohol reflux 2 times of 11 times of amounts 92%, each 1.5 hours, filter, merging filtrate, 64 ℃ of concentrating under reduced pressure, 59 ℃ of vacuum dryings, extract I;
(2) get Radix Isatidis medical material 300g, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 10 times of amounts 58% 2 times each 1.5 hours, filters, merging filtrate, 59 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 19% in the extractum, amount of alcohol added is 2.5ml in every gram extractum, dissolving refluxes, room temperature cools, 3.5 ℃ refrigerator was placed 32 hours, filtered to obtain supernatant, it is stand-by to collect insoluble matter, it is 1.15 that supernatant continues to be evaporated to relative density of medicine liquid, add 94% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 70%, and room temperature left standstill 30 hours, filter, 59 ℃ of concentrating under reduced pressure of supernatant, 59 ℃ of vacuum dryings get extract II;
(3) above-mentioned insoluble matter is dissolved in water goes up polyamide and kieselguhr mixed column chromatography, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 59 ℃ of concentrating under reduced pressure, 59 ℃ of vacuum dryings get extract II I;
(4) united extraction thing I, II, III pulverize the back mixing, are principal agent, and medicated powder is done the general ball of making of wetting agent with water, drying, and polishing, sugar coating promptly gets pill.
Embodiment 8
(2) get Echinacea medical material 200g, pulverize, add the alcohol reflux 3 times of 9 times of amounts 88%, each 1.4 hours, filter, merging filtrate, 51 ℃ of concentrating under reduced pressure, 56 ℃ of vacuum dryings, extract I;
(3) get Radix Isatidis medical material 800, pulverize, mix with filtering residue after Echinacea extracts, the alcohol reflux of 10 times of amounts 50% 3 times each 1.5 hours, filters, merging filtrate, 60 ℃ of reclaim under reduced pressure concentrate, to the extractum shape, the ethanol of adding 20% in the extractum, amount of alcohol added is 2.1ml in every gram extractum, dissolving refluxes, room temperature cools, 5.5 ℃ refrigerator was placed 34 hours, filtered to obtain supernatant, it is stand-by to collect insoluble matter, it is 1.25 that supernatant continues to be evaporated to relative density of medicine liquid, add 94% ethanol and transfer determining alcohol to carry out precipitate with ethanol, making it contain the alcohol amount is 60%, and room temperature left standstill 29 hours, filter, 64 ℃ of concentrating under reduced pressure of supernatant, 57 ℃ of vacuum dryings get extract II;
(4) above-mentioned insoluble matter is dissolved in water goes up macroporous resin column, the water eluting is removed washing and is muddy stream part, begin when clear to collect to water, the washing amount shows negative for making sugar colour developing reflection, merges and washes part, 64 ℃ of concentrating under reduced pressure, 58 ℃ of vacuum dryings get extract II I;
(5) united extraction thing I, II, III pulverize the back mixing, are principal agent, add hydroxypropyl cellulose in principal agent, do wetting agent with ethanol, make granule, drying, and granulate, tabletting promptly gets slow releasing tablet.
Claims (2)
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