CN103494928A - Preparation method for compound houttuynia cordata preparation - Google Patents
Preparation method for compound houttuynia cordata preparation Download PDFInfo
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Abstract
The invention discloses a preparation method for a compound houttuynia cordata preparation. The preparation method comprises the following steps: (1) extracting volatile oil from houttuynia cordata and fructus forsythiae; (2) extracting medicine drugs of the houttuynia cordata and fructus forsythiae which are extracted to obtain the volatile oil, isatis tinctoria and lonicera japonica by water; filtering an extracting solution and concentrating the filtering solution until the relative density is 1.10-1.30 (at 60 DEG C); adding ethanol until the alcohol content is up to 60%-85%; standing and filtering; recycling the ethanol and concentrating to form a fluid extract; (3) extracting scutellaria baicalensis by using water and filtering an extracting solution; adjusting the pH (Potential of Hydrogen) value of the filtering solution to be 1.0-3.0; keeping the heat at 60-95 DEG C for 0.5-2.5 hours; standing and filtering; washing sediments by sequentially using 30%-95% of the ethanol and the water until the pH value is 4-6 to obtain a scutellaria baicalensis extract; and (4) combining the volatile oil, the fluid extract and the scutellaria baicalensis extract and mixing uniformly by adopting a mechanical grinding method; and then preparing a mixture into pills to obtain the product.
Description
Technical field
The present invention relates to the field of Chinese medicines, particularly a kind of preparation method of heat-clearing and detoxifying herb preparation.
Background technology
Pharyngitis, tonsillitis are the common symptoms of upper respiratory tract infection, and the traditional Chinese medical science belongs to throat moth, the sore throat category of larynx section, is that affection due to external wind and heat causes.Doctor trained in Western medicine is thought, pharyngitis, tonsillitis are pharyngolaryngeal mucosa and adenoid inflammation thereof, the cause of disease is mainly the stimulations such as antibacterial, viral infection, chemical factors dust, tobacco and wine, also can be secondary to the symptom in early stage of systemic disease or other diseases, treatment adopts antibiotics to be aided with the methods such as buccal tablets agent mostly, but curative effect is often undesirable, though having, symptom alleviates, but the swelling and ache of throat, the dry disease such as itch often delay difficult more, be difficult for eradicating, some several months do not heal, thereby have caused abuse of antibiotics.
The way that the traditional Chinese medical science uses that organic conception and dialectical opinion control that external wind heat causes has sore throat, acute pharyngitis, tonsillitis often adopt heat-clearing and toxic substances removing.The clinical Chinese medicine for heat-clearing and toxic substances removing is more, take the Chinese medicine agent as many.The conventional dosage forms production technology is relatively backward, and active constituent content is lower, and bioavailability is lower, and curative effect has much room for improvement.Record the effect that has heat-clearing and toxic substances removing in the FUFANG YUXINGCAO PIAN of the Pharmacopoeia of the People's Republic of China, what for affection due to external wind and heat, cause has sore throat; Acute pharyngitis, tonsillitis have the wind heat patient.
The Herba Houttuyniae suffering, be slightly cold, and returns lung meridian, has heat-clearing and toxic substances removing, an effect of pain evacuation of pus, the inducing diuresis for treating stranguria syndrome that disappear.Modern pharmacological research shows, that Herba Houttuyniae has is antibiotic, antiviral, immunomodulating, diuresis.Clinical have a report that it is treated to 24 kinds of active chronic inflammations of 109 examples, proves that it has definite curative effect.
The Radix Scutellariae hardship, cold, return lung, gallbladder, spleen, large intestine, small intestine meridian, there is heat clearing and damp drying, eliminating fire and detoxication, hemostasis, antiabortive effect.The pharmacology report: it has antimicrobial effect, antiinflammatory and anti-allergy action.The low dosage baicalin can obviously promote the mice spleen lymphocytes proliferation reaction that con A (ConA) is induced, high dose significantly suppresses, and reduces blood pressure and diuresis, effect for reducing blood fat, the gathering of anti-blood plate and anticoagulation, antioxidation, the central nervous system had to remarkable sedation.Clinical report treatment children with acute respiratory infection 51 examples, anxious chronic bronchitis tracheitis 11 examples, acute tonsillitis 1 example, control rear body temperature and be down to normally, transference cure person 51 examples, invalid 12 examples.
Radix Isatidis is bitter, cold, and GUIXIN, stomach warp, have the effect of heat-clearing and toxic substances removing, removing heat from blood sore-throat relieving.The pharmacology report, Radix Isatidis has antibacterium, antiviral effect, and anti-endotoxin effect, antitumaous effect, have regulating action to immunity, the clinical child virus upper respiratory tract infection that is used for the treatment of, injection 182 examples, produce effects 60 examples, effective 12 examples, granule 50 examples, produce effects 20 examples, effective 16 examples.
The Fructus Forsythiae hardship, be slightly cold, and returns lung, the heart, small intestine meridian.Effect with heat-clearing and toxic substances removing, dispersing swelling and dissipating binds.Pharmacological research shows, Fructus Forsythiae is the effective antimicrobial medicine of a kind of wide spectrum, and in vitro tests has inhibitory action to many kinds of antibacterials.
The applicant, in order to improve the curative effect of FUFANG YUXINGCAO PIAN prescription, conducts in-depth research it, and applied for patent of invention in 2007 " preparation method of FUFANG YUXINGCAO DIWAN (publication number: CN101040950A) ".
Summary of the invention
The object of the present invention is to provide a kind of preparation method of compound houttuynin preparation, preparation method of the present invention is more scientific and reasonable, and the curative effect of medication prepared is more excellent.
The compound houttuynin preparation the present invention relates to is to be prepared from by following weight proportion crude drug: Herba Houttuyniae 1000-1300 part, Radix Scutellariae 250-350 part, Radix Isatidis 250-350 part, 100-150 parts of Fructus Forsythiaes, 100-150 parts of Flos Loniceraes.
Preparation method provided by the invention comprises the steps:
(1) Herba Houttuyniae, Fructus Forsythiae extract volatile oil, standby;
(2) Herba Houttuyniae, the Fructus Forsythiae medicinal residues extracting in water together with Radix Isatidis, Flos Lonicerae after step (1) extraction volatile oil, extracting liquid filtering, it is 1.10～1.30 that filtrate is concentrated into relative density in the time of 60 ℃, adding ethanol makes to reach 60%-85% containing the alcohol amount, standing, filter, filtrate recycling ethanol also is condensed into fluid extract, standby;
(3) Radix Scutellariae water extraction, extracting liquid filtering, filtrate is adjusted ℃-95 ℃, PH to 1.0～3.0,60 insulation 0.5-2.5 hours, standing, filters, and precipitate is used successively 30%-95% ethanol and is washed to pH value is 4～6, obtains Radix Scutellariae extract, standby;
(4) above-mentioned volatile oil, fluid extract and Radix Scutellariae extract are merged, and adopt mechanical lapping to make its mix homogeneously, obtain active constituents of medicine, then make drop pill, obtain.
The present invention extracts Herba Houttuyniae, Forsythia volatile oil can adopt to close and carry, and also can adopt independent extraction; Extracting mode can adopt vapor distillation or supercritical extraction.
The present invention, for Radix Scutellariae extract can be scattered in fluid extract uniformly, has adopted the method for mechanical lapping, and equipment used is colloid mill.
Compound houttuynin preparation of the present invention is drop pill, and its preparation adopts the preparation of galenic pharmacy routine techniques, comprises the step that active constituents of medicine is mixed with substrate, and the weight ratio of active constituents of medicine and substrate is 1: 1-6.Described substrate is selected from one or more in fat-soluble substrate and water-soluble base, and wherein fat-soluble substrate is selected from: stearic acid, glyceryl monostearate, insect wax, Cera Flava, paraffin, hydrogenated vegetable oil, semi-synthetic fatty acid ester; Water-soluble base is selected from Polyethylene Glycol, polyoxyethylene monostearate, poloxamer, sodium stearate, glycerin gelatine etc.; Xylitol and composites of starch, erythritol.The preferred substrate of the present invention is polyethylene glycol 6000 and the Macrogol 4000 mixture that weight ratio is 3: 1, and active constituents of medicine and substrate weight ratio are 1: 3.
Innovation of the present invention is:
Below by some experimental examples, the invention will be further described.
Experimental example 1 Herba Houttuyniae, Radix Isatidis, Fructus Forsythiae and Flos Lonicerae four Chinese medicine material Study on extraction
1, Extraction Process of Volatile Oil relatively
Weight by table 1 design takes each test group medical material, adds respectively 12 times of water gagings, soaks 5 hours, extracts volatile oil.
Each test group medical material of table 1 forms and the weight situation
| Title | Herba Houttuyniae | Radix Isatidis | Flos Lonicerae | Fructus Forsythiae |
| Group 1 | 583g | — | — | 58g |
| Group 2 | 583g | — | 58g | 58g |
| Group 3 | 583g | 150g | 58g | 58g |
Each test group extraction time and the volatilization oil mass collected are in Table 2:
Each test group extraction time of table 2 and the volatilization oil mass situation of collecting
| Extraction time (minute) | Group 1 volatilization oil mass (ml) | Group 2 volatilization oil masses (ml) | Group 3 volatilization oil masses (ml) |
| 30 | 0.31 | 0.29 | 0.28 |
| 60 | 0.50 | 0.44 | 0.42 |
| 90 | 0.62 | 0.53 | 0.51 |
| 120 | 0.69 | 0.60 | 0.56 |
| 150 | 0.70 | 0.64 | 0.60 |
| 180 | 0.70 | 0.66 | 0.62 |
| 240 | 0.70 | 0.66 | 0.62 |
As shown in Table 2, test group 1 is extracted 120 minutes volatile oil and is substantially extracted fully, and the volatilization oil mass of collecting is than test group 2 and test group more than 3.
2, the impact of extraction time on the Chlorogenic Acid of Flos Lonicerae extracted amount
3 parts of extracting honeysuckles, every part of 100g, add 12 times of water gagings and decoct, and decocting time is respectively 2h, 2.5h and 3h, measures the content of decoction liquor Content of Chlorogenic Acid, calculates its extracted amount, the results are shown in Table 3:
Table 3 chlorogenic acid extracted amount situation of different extraction time
| Tested number | Extraction time (h) | Chlorogenic acid extracted amount (mg/g) |
| 1 | 2 | 23.4 |
| 2 | 2.5 | 22.3 |
| 3 | 3 | 21.1 |
As shown in Table 3, Flos Lonicerae extraction time is unsuitable long, otherwise the chlorogenic acid extracted amount can reduce, and this may be subject to thermally labile relevant in aqueous solution with chlorogenic acid.In conjunction with the Extraction Process of Volatile Oil result of study, Herba Houttuyniae, Radix Isatidis, Fructus Forsythiae and the preferred extraction process of Flos Lonicerae four Chinese medicine material are that Herba Houttuyniae and Fructus Forsythiae first extract volatile oil, then adopt water extraction together with Radix Isatidis, Flos Lonicerae.
Experimental example 2 Radix Scutellariae extracts and all the other medicinal substances extracts mix method research
1, test specimen: embodiment 1 drop pill and Comparative Examples 1 drop pill
2, content determination of Baicalin
According to high performance liquid chromatography (appendix VID of Pharmacopoeia of People's Republic of China version in 2000), measure.
Chromatographic condition and system suitability octadecylsilane chemically bonded silica are filler; Methanol-water-phosphoric acid (47: 53: 0.2) mobile phase; The detection wavelength is 280nm.Number of theoretical plate is pressed the baicalin peak and is calculated, and should be not less than 2500.
The preparation precision of reference substance solution takes and adds in right amount 50% methanol at 60 ℃ of drying under reduced pressure baicalin of 4 hours and make every 1ml containing the solution of 30ug, obtains.
Drop pill 2.5g is got in the preparation of need testing solution, grinds, and gets 0.5g, accurately weighed, add the heat of solution of 10ml water temperature, add the 1.5ml6mol/L hydrochloric acid solution, shake up, 80 ℃ are incubated 1 hour, placement is spent the night, centrifugal, the supernatant that inclines, and precipitation adds 70% ethanol ultrasonic dissolution, be transferred in the 50ml measuring bottle, add 70% ethanol to scale, shake up, filter, discard just filtrate, the accurate subsequent filtrate 2ml that draws, water bath method, add 50% ethanol gradation and dissolve, and be transferred in the 10ml measuring bottle, add 50% ethanol to scale, shake up, obtain; Embodiment 1 drop pill and Comparative Examples 1 drop pill respectively prepare 6 parts.
Algoscopy is accurate reference substance solution and each 20ul of need testing solution of drawing respectively, and the injection liquid chromatography, measure and get final product.
Result: embodiment 1 drop pill is on average containing baicalin (C
21h
18o
11) be that 2.53%, RSD value is 1.58%; Comparative Examples 1 drop pill is on average containing baicalin (C
21h
18o
11) be that 2.16%, RSD value is 1.64%.As can be seen here, the content of baicalin that adopts colloid mill to be mixed in the drop pill made extract is high.
Experimental example 3 drop pill Study on Forming
1, the selection of substrate: substrate commonly used has: Polyethylene Glycol (PEG4000, PEG6000), glycerin gelatine, stearic acid, insect wax, hydrogenated vegetable wet goods.Select in this test that fusing point is low has dispersion force and than the PEG-4000 of imperial palace collection power with carry out design and the screening of molding formula for the PEG-6000 that adjusts drop pill hardness, thermostability and mobility simultaneously.
2, determining of condensing agent: water-soluble base will select fat-soluble coolant.Selecting respectively liquid Paraffin, dimethicone, Oleum Arachidis hypogaeae semen is condensing agent: take medicine: substrate PEG-6000 as 1: 2 and 1: 3; With the water dropper bore (inside/outside, mm) 2.0/5.0,70 ℃ of fluid temperature, condensing agent temperature-5 ℃ are experiment condition: take sedimentation velocity, hardness, roundness is observation index.Result shows, drop pill sedimentation velocity in liquid paraffin is moderate, and roundness is good, and hardness is good, therefore the selection liquid Paraffin is condensing agent.
3, molding formula screening: first the PEG-4000 of different proportionings and PEG-6000 substrate prescription are made to substrate, melting, then the active constituents of medicine of mix homogeneously is joined respectively in the substrate of melting. and continuous agitating heating. make it mix homogeneously.Remain under uniform temperature (8O ℃).The liquid Paraffin of take carries out dripping as condensing agent.Take and form prescription PEG-6000:PEG-4000=3: 1 drop pill of making for the substrate situation that bonds is better, and roundness, hardness can meet the requirement of drop pill.
4, the drop pill molding technological condition is preferred: in the preparation technology of drop pill, the mixed proportion of matrix species, Chinese medicine extract and substrate, dripping temperature, water dropper bore, coolant temperature etc. are the key factors of drop pill molding, on the basis of single Factor Selection, take PEG-6000:PEG-4000=3: 1 is substrate, liquid Paraffin is condensing agent, (inside/outside mm) is decided to be 2.0/5.0 to the water dropper bore.Be evaluation index with weight differential, dissolve scattered time limit, presentation quality (hardness, the color and luster uniformity, roundness, sticky ball, hangover), the factors such as medicine and substrate ratio, dripping temperature, coolant temperature carried out to orthogonal test preferred.Result shows: the best moulding process of drop pill is: the dripping temperature is 75 ℃, and coolant temperature is-5 ℃, Chinese medicine extract: substrate=1:3 (g/g).Drop pill ratio of briquetting average out to 95.83%.
Experimental example 4 pharmacodynamics comparative studies
1, antiinflammatory test
Get 30 of mices, be divided at random 3 groups, 10 every group, i.e. blank group (isometric(al)), embodiment 1 FUFANG YUXINGCAO DIWAN group (2gkg
-1), Comparative Examples 1 FUFANG YUXINGCAO DIWAN group (2gkg
-1).The Ig administration, continuous 7d, 1h after the last administration, at left ear two flour of mice, with 100% dimethylbenzene, auris dextra, for contrast, is put to death mice after 4h, decoct down two ears along ear corridor baseline, prepare the mice auricle with 6mm diameter card punch, with electronic scale, claim weight in wet base, using the difference of two ear weight as swelling (inflammation index).The results are shown in Table 4.
The impact of the mice ear that table 4 compound houttuynin preparation xylol is induced
| Group | Dosage (gkg-1) | Ear swelling degree (△ mg) |
| The blank group | — | 9.44±1.76 |
| Embodiment 1 FUFANG YUXINGCAO DIWAN group | 2 | 5.22±2.04** |
| Comparative Examples 1 FUFANG YUXINGCAO DIWAN group | 2 | 7.69±2.19* |
Compare * * P<0.01 with the blank group; * P<0.05.
The impact of 2, mice spleen lymphocytes proliferation being reacted
2.1 the preparation of splenocyte
Get 40 of mices, be divided at random 4 groups, 10 every group, i.e. blank group (isometric(al)), pathological model group, embodiment 1 FUFANG YUXINGCAO DIWAN group (2gkg
-1), Comparative Examples 1 FUFANG YUXINGCAO DIWAN group (2gkg
-1).The ig administration, continuous 7d, from medication 3d, except the blank group, each organizes the equal SC cyclophosphamide of mice 80mgkg
-1once, 1h after the last administration, put to death each group mice dislocation, put 75% alcohol-pickled 5min, under aseptic condition, take out spleen, remove tunicle, use Hank ' s liquid to wash 2 times, shred, piece of tissue is put into to micro glass homogenizer, repeatedly grind, make splenocyte suspension, with 200 order net filtration splenocytes, then carry out cell counting, be made into 5 * 10
6ml
-1stand-by.
2.2 the breeder reaction of splenocyte
Undertaken by the Mosmann method, the cell suspension of adjusting is joined in 96 porocyte culture plates, every hole 200 μ l(5 * 10
6ml
-1), then to every hole, add final concentration 10 μ gml
-1conA or 20 μ gml
-1lPS, put 37 ℃ of %CO
2incubator is cultivated 66 hours, takes out culture plate, and every hole adds 5mgml
-1mTT20 μ l, continue to cultivate 4～6 hours.Take out Sptting plate, centrifugal 3000rmin
-110min, inhale and abandon supernatant, and every hole adds acidify isopropyl alcohol 150 μ l, in agitator, vibrates for 3 seconds, fully mixes, and reads the A value at microplate reader 570nm place after 10 minutes, in Table 5.
The impact of table 5 compound houttuynin preparation on the mouse lymphocyte transformation function
With the blank group, compare,
△ △p<0.01; Compare * * P<0.01, * P<0.05 with the pathological model group.
3, mouse antibodies is formed the impact of cell
3.1 prepare the immune mouse spleen cell suspension
Grouping and medication are with 2, and from medication 3d, except the blank group, each organizes the equal SC cyclophosphamide of mice 80mgkg
-1once; From medication 3d, each SRBC0.2ml that organizes the equal ip10% of mice only
-1, 1h after time administration organizes mice dislocation and puts to death each, takes out spleen and prepares individual cells, with containing Ca
2+, Mg
2+the PBS furnishing 1 * 10 of ion
7individual ml
-1.
3.2 measure the antibody forming cell
The extracting spleen cell suspension, the PBS of PH7.2 of take is medium, in small test tube, adds above-mentioned splenocyte suspension 1ml, adds 0.2%SRBC1ml and fresh guinea pig serum (1:20) dilution 1ml, fully mixes, and puts 37 ℃ of incubation 1h.The experimental port cumulative volume is 3ml.Establish cell negative control, complement control, SRBC contrast and PBS blank (zeroing is used) simultaneously.Centrifugal (2000rmin
-1, 10min), get supernatant 2ml, put visible spectrophotometer and measure its light absorption value (A), detect wavelength 413nm, the results are shown in Table 6.
Table 6 compound houttuynin preparation antagonist forms the impact of cell
| Group | Dosage/gkg-1 | A value (413nm) |
| The blank group | — | 0.957±0.027 |
| The pathological model group | — | 0.716±0.076 △△ |
| Embodiment 1 FUFANG YUXINGCAO DIWAN group | 2 | 1.423±0.069** |
| Comparative Examples 1 FUFANG YUXINGCAO DIWAN group | 2 | 1.098±0.240** |
With the adjuvant group, compare,
△ △p<0.01; Compare * * P<0.01 with the pathological model group.
4, on the impact of phagocytic activity of leukocytes
4.1 bacterium solution preparation
The Staphylococcus albus of biological 24h (staphylococcus epidermidis) is scraped on the solid agar culture medium, wash 2 times with PH7.2PBS, by turbidimetry, bacterium is adjusted to 5 * 10
7individual ml-
1 bacteriumliquid, 100 ℃ of 15min sterilization, put 4 ℃ standby.
4.2 phagocytic activity of leukocytes is measured
Grouping and medication be with 2,1h after the last administration, and each is organized eyeball of mouse and gets blood (anticoagulant heparin), anticoagulation 3 is dripped to 3 of Staphylococcus albus liquid and mix, lain against in the wet box of lid, put 37 ℃ of 30min jogs 1 time, put slide one auspicious, push jack, methanol is fixed, Wright-Giemsa dyeing.Under the oil mirror, 200 neutrophil cells of counting, write down the cell number that the cell number of engulfing antibacterial and each neutrophilic granulocyte are swallowed, and is calculated as follows:
The cell number of cytophagy rate (%)=engulf antibacterial/200 * 100%;
Phagocytic index=200 neutrophilic granulocyte is engulfed total number of bacteria/200.
The results are shown in Table 7.
The impact of table 7 compound houttuynin preparation on mice phagocytic rate and phagocytic index
| Group | Dosage/gkg-1 | Phagocytic rate | Phagocytic index |
| The blank group | — | 55.3±11.90 | 0.814±0.122 |
| The pathological model group | — | 44.8±9.95△ | 0.523±0.053△△ |
| Embodiment 1 FUFANG YUXINGCAO DIWAN group | 2 | 66.55±9.32** | 0.761±0.122** |
| Comparative Examples 1 FUFANG YUXINGCAO DIWAN group | 2 | 54.90±11.89 | 0.654±0.186* |
With the blank group, compare,
△p<0.05;
△ △p<0.01; Compare * * P<0.01, * P<0.05 with the pathological model group.
In sum, experimental example 1 drop pill drug effect is better than Comparative Examples 1 drop pill.
The specific embodiment
Following embodiment is used for the present invention is described, but is not used for limiting the scope of the invention.
Embodiment 1 drop pill
Herba Houttuyniae 1166g Radix Scutellariae 300g Radix Isatidis 300g
Fructus Forsythiae 116g Flos Lonicerae 116g
Above-mentioned medical material is made the 1000g drop pill as follows:
Above-mentioned five tastes medical material, Herba Houttuyniae, Fructus Forsythiae two flavor medical materials add 12 times of water gagings, and distillating extracting oil 2 hours, collect volatile oil standby; Filter, the another device of filtrate is collected standby; Medicinal residues add 12 times of water gagings again and decoct 2 times together with Radix Isatidis, Flos Lonicerae, and each 2 hours, filter, collect filtrate, merge three times filtrate, be concentrated into relative density and be about 1.15 (60 ℃), add ethanol and make to reach 70% containing the alcohol amount, placed liquid, and filtered, filtrate recycling ethanol also is condensed into fluid extract.Radix Scutellariae adds 10 times of water gagings and decocts 2 times, and each 1 hour, merging filtrate, adjust PH1.5～2,80 ℃ insulation 1 hour, standing 24 hours with dilute hydrochloric acid, filter, PH5～6 are washed, are washed to precipitation with ethanol, adds in fluid extract, and add volatile oil, and with colloid mill, mix, with the polyethylene glycol 6000 of melting-Macrogol 4000 mixture, mix homogeneously, from top to bottom, splash in liquid Paraffin, liquid Paraffin is use up and wiped to the drop pill drop of molding, 1000g processed, obtain.
Embodiment 2 drop pills
Herba Houttuyniae 1166g Radix Scutellariae 300g Radix Isatidis 300g
Fructus Forsythiae 116g Flos Lonicerae 116g
Above-mentioned medical material is made the 1000g drop pill as follows:
Above-mentioned five tastes medical material, Herba Houttuyniae, Fructus Forsythiae two flavor medical materials add 12 times of water gagings, and distillating extracting oil 2 hours, collect volatile oil standby; Filter, the another device of filtrate is collected standby; Medicinal residues add 10 times of water gagings again and decoct 3 times together with Radix Isatidis, Flos Lonicerae, and each 1 hour, filter, collect filtrate, merge three times filtrate, be concentrated into relative density and be about 1.15 (60 ℃), add ethanol and make to reach 70% containing the alcohol amount, placed liquid, and filtered, filtrate recycling ethanol also is condensed into fluid extract.Radix Scutellariae adds 10 times of water gagings and decocts 2 times, and each 2 hours, merging filtrate, adjust PH1.5～2,80 ℃ insulation 1 hour, standing 24 hours with dilute hydrochloric acid, filter, PH5～6 are washed, are washed to precipitation with 30% ethanol, adds in fluid extract, and add volatile oil, and with colloid mill, mix, with the polyethylene glycol 6000 of melting, mix homogeneously, from top to bottom, splash in liquid Paraffin, liquid Paraffin is use up and wiped to the drop pill drop of molding, 1000g processed, obtain.
Comparative Examples 1 drop pill
Herba Houttuyniae 1166g Radix Scutellariae 300g Radix Isatidis 300g
Fructus Forsythiae 116g Flos Lonicerae 116g
Above-mentioned medical material is made the 1000g drop pill as follows:
Above-mentioned five tastes medical material, Herba Houttuyniae, Fructus Forsythiae, Flos Lonicerae three flavor medical materials add 12 times of water gagings, and distillating extracting oil 2 hours, collect volatile oil standby; Filter, the another device of filtrate is collected standby; Medicinal residues add 12 times of water gagings again and decoct 2 times together with Radix Isatidis, and each 2 hours, filter, collect filtrate, merge three times filtrate, be concentrated into relative density and be about 1.15 (60 ℃), add ethanol and make to reach 70% containing the alcohol amount, placed liquid, and filtered, filtrate recycling ethanol also is condensed into clear paste.Radix Scutellariae adds 10 times of water gagings and decocts 2 times, each 1 hour, merging filtrate, adjusted PH1.5～2 with dilute hydrochloric acid, 80 ℃ are incubated 1 hour, standing 24 hours, to filter, PH5～6 are washed, are washed to precipitation with ethanol, vacuum drying, pulverize, obtain the Radix Scutellariae extract powder, add in clear paste to mix to be condensed into fluid extract, add volatile oil, mix, mix homogeneously with the polyethylene glycol 6000 of melting-Macrogol 4000 mixture, from top to bottom, splash in liquid Paraffin, liquid Paraffin is use up and wiped to the drop pill drop of molding, and 1000g processed, obtain.
Claims (7)
1. the preparation method of a compound houttuynin preparation, described compound houttuynin preparation is prepared from by following weight proportion crude drug: Herba Houttuyniae 1000-1300 part, Radix Scutellariae 250-350 part, Radix Isatidis 250-350 part, 100-150 parts of Fructus Forsythiaes, 100-150 parts of Flos Loniceraes is characterized in that preparation method is as follows:
(1) Herba Houttuyniae, Fructus Forsythiae extract volatile oil, standby;
(2) Herba Houttuyniae, the Fructus Forsythiae medicinal residues extracting in water together with Radix Isatidis, Flos Lonicerae after step (1) extraction volatile oil, extracting liquid filtering, it is 1.10～1.30 that filtrate is concentrated into relative density in the time of 60 ℃, adding ethanol makes to reach 60%-85% containing the alcohol amount, standing, filter, filtrate recycling ethanol also is condensed into fluid extract, standby;
(3) Radix Scutellariae water extraction, extracting liquid filtering, filtrate is adjusted ℃-95 ℃, PH to 1.0～3.0,60 insulation 0.5-2.5 hours, standing, filters, and precipitate is used successively 30%-95% ethanol and is washed to pH value is 4～6, obtains Radix Scutellariae extract, standby;
(4) above-mentioned volatile oil, fluid extract and Radix Scutellariae extract are merged, and adopt mechanical lapping to make its mix homogeneously, obtain active constituents of medicine, then make drop pill, obtain.
2. preparation method according to claim 1, is characterized in that it is steam distillation that step (1) is extracted the method for volatile oil.
3. preparation method according to claim 1, is characterized in that the described machinery of step (4) is colloid mill.
4. according to the arbitrary described preparation method of claim 1-3, it is characterized in that step (4) drop pill processed substrate used is selected from one or more in fat-soluble substrate and water-soluble base, wherein fat-soluble substrate is selected from: stearic acid, glyceryl monostearate, insect wax, Cera Flava, paraffin, hydrogenated vegetable oil, semi-synthetic fatty acid ester; Water-soluble base is selected from Polyethylene Glycol, polyoxyethylene monostearate, poloxamer, sodium stearate, glycerin gelatine; Xylitol and composites of starch, erythritol.
5. preparation method according to claim 4, is characterized in that the weight ratio of step (4) drop pill active constituents of medicine processed and substrate is 1: 1-6.
6. preparation method according to claim 5, is characterized in that step (4) drop pill active constituents of medicine processed and substrate weight ratio are 1: 3.
7. preparation method according to claim 6, is characterized in that described substrate is the weight ratio polyethylene glycol 6000-Macrogol 4000 mixture that is 3: 1.
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| CN107496576A (en) * | 2017-09-28 | 2017-12-22 | 南京正宽医药科技有限公司 | A kind of compound houttuynin soft capsule and preparation method and purposes |
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| CN104435113B (en) * | 2014-12-16 | 2018-06-19 | 江西天施康中药股份有限公司 | It is used to prepare the preparation method of the Baical Skullcap root P.E of Ynxingchao dropping pills compound |
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| CN108935868A (en) * | 2017-05-18 | 2018-12-07 | 云南天士力帝泊洱生物茶集团有限公司 | A method of extracting aromatic substance from plant product |
| CN108935868B (en) * | 2017-05-18 | 2023-10-03 | 云南天士力帝泊洱生物茶集团有限公司 | Method for extracting aromatic substances from plant products |
| CN107496576A (en) * | 2017-09-28 | 2017-12-22 | 南京正宽医药科技有限公司 | A kind of compound houttuynin soft capsule and preparation method and purposes |
| CN111973515A (en) * | 2020-08-28 | 2020-11-24 | 科丝美诗(中国)化妆品有限公司 | Bacteriostatic restoration plant extraction composition, preparation method and application thereof |
| CN111973515B (en) * | 2020-08-28 | 2022-09-20 | 科丝美诗(中国)化妆品有限公司 | Bacteriostatic restoration plant extraction composition, preparation method and application thereof |
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