CN101797365B - Preparation technology of Kaixiong Shunqi Jiaonang - Google Patents
Preparation technology of Kaixiong Shunqi Jiaonang Download PDFInfo
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Abstract
The invention discloses a Kaixiong Shunqi Jiaonang and preparation technology thereof. On the basis of the formula of the original Kaixiong Shunqi Jiaonang, repetition test, comparison, induction, screening and summarizing are carried out to obtain a new Kaixiong Shunqi Jiaonang. The technology fully considers properties and composition of all raw materials, pericarpium citri reticulatae, curcuma zedoary, rhizome sparganii and costustoot are subject to water distillation to extract volatile oil, fructus gleditsiae, areca-nut, mangnolia officinalis and semen pharbitidis are subject to ethylalcohol microwave extraction, the vast majority of active ingredients of medicinal materials are remained, extraction efficiency of medicine is improved and impurities in medicinal materials are effectively removed, pesticide effect and stability of medicine is improved, and the preparation technology is worthy of being popularized.
Description
Technical field
The present invention relates to the field of Chinese medicines and Chinese medicine manufacture field, be specifically related to a kind of Kaixiong Shunqi Jiaonang and preparation technology thereof.
Background technology
Kaixiong Shunqi Wan is a kind of classical Chinese patent medicine, and it is mainly used in removing food stagnancyization and stagnates, promoting the circulation of QI to relieve pain.Be used for stopping in the diet, the fullness and distention in the chest and hypochondrium that depression of QI causes, gastralgia, the belch vomiting and nausea, lack of appetite is indigestion and loss of appetite.The Kaixiong Shunqi Wan that Chinese Pharmacopoeia records is the watered pill, is made up of 8 flavor Chinese medicines such as Semen Arecae, Semen Pharbitidis, Pericarpium Citri Reticulatae, Radix Aucklandiae magnolia obovata.The watered pill is a kind of traditional Chinese medicine preparation form, normally Chinese crude drug is ground into to adopt behind the fine powder agitation procedure to be worth.Traditional agitation procedure production process comprises the steps: to adopt common crushing technology to be ground into fine powder medical material, and the water molding strengthens, and sieves capping then, dry, polishing repeatedly.Whole process complexity, loaded down with trivial details, labor intensity is big, be difficult to operation, the one-pass finished qualification rate is low, and ball heavily differs greatly, and also occurs molten diffusing overlong time sometimes, the nonabsorbable phenomenon of medicine has not only been brought inconvenience to production, has also influenced product quality and therapeutic effect.
In order to overcome the defective of prior art, application number is 200710170577, and publication number is CN101181572A, denomination of invention has been for disclosing a kind of preparation method of new Kaixiong Shunqi Wan in " method that prepare Kaixiong Shunqi Wan ", is about to the 8 medical material pulverize separately of distinguishing the flavor of, mixing, granulate pelleting then.Though this preparation method has solved the uneven problem of agitation procedure pill size, also improved the one-pass finished rate to a certain extent, but its technology is simple, because the raw material of Kaixiong Shunqi Wan is Chinese crude drug, composition is comparatively complicated, effective content is low, and therefore the quality of the Kaixiong Shunqi Wan product of above-mentioned prepared and curative effect are all unstable, and the impurity in the removal medical material not yet in effect.
Though Kaixiong Shunqi Wan is used for stagnation of QI due to dyspepsia disease better curative effect is arranged also, because original, the dose of dosage form is big, defective such as be difficult for swallowing, the patient is difficult for accepting.Therefore, original dosage form of change Kaixiong Shunqi Wan has very big meaning.A kind of Kaixiong Shunqi Jiaonang is disclosed in the prior art, compare with former pill, Kaixiong Shunqi Jiaonang has the active constituent content height, advantages such as dose is little, carry taking convenience, disintegrate is fast, the effective ingredient stripping is fast, stripping quantity is big, help shortening and get the effect time and better bring into play clinical efficacy, its agent changes firmly gets patient's welcome.
" CHINA JOURNAL OF CHINESE MATERIA MEDICA ", 1999 the 24th volume o. 11ths, the paper of " Kaixiong Shunqi Jiaonang Study on Preparation " discloses a kind of preparation process of Kaixiong Shunqi Jiaonang: get Pericarpium Citri Reticulatae, the Radix Aucklandiae, Rhizoma Curcumae extracting in water volatile oil, volatile oil device in addition stores for future use, and the aqueous solution after swallow is heated up in a steamer filters, and medicinal residues add decocting in water, filter, merging filtrate concentrates precipitate with ethanol, filtration, filtrate for later use; To get areca powder and be broken into fine powder. all the other Bins are thorough, Semen Pharbitidis (stir-fry), Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens), rhizoma sparganic (vinegar system), the suitable grating of Fructus Gleditsiae Abnormalis, use alcohol reflux, filter, filtrate such as filtrate and Pericarpium Citri Reticulatae merges, concentrating under reduced pressure adds the Semen Arecae fine powder, mixing, drying under reduced pressure, pulverize, sieve, granulate, drying sprays into volatile oil, mixing, the glue capsule.
The Kaixiong Shunqi Jiaonang active constituent content that above-mentioned preparation technology obtains is greatly improved, and changes also quite successfully in agent this time at that time, and becomes a kind of classical preparation technology of Kaixiong Shunqi Jiaonang gradually.But along with the research of more than ten years, people have had more scientific comprehensive understanding to each crude drug of Kaixiong Shunqi Jiaonang, and the drawback of above-mentioned technology is also by manifesting.Directly pulverize auxilliary adsorbent and the filler of making capsule particle as adopting most Semen Arecae in this preparation process, though can reduce the production cost of any and simplify the technology of medication preparation, but recent research shows, because the complicated component of Semen Arecae, it contains the not clear alkaloid of multiple fat, betel oil and various composition, exerts a certain influence without processing the stability of directly being used as medicine to capsular safety and curative effect of medication.Because Semen Arecae is a kind of of Kaixiong Shunqi Jiaonang principal agent, the most of Semen Arecae in the prescription is extracted without specific aim, and directly be used as medicine as filler, reduced its utilization rate.Add and contain some special composition in the Semen Arecae, cause the easy variable color of Semen Arecae, cause property of medicine instability, in addition, above-mentioned technology is not extracted route according to raw-material composition science design, causes extraction efficiency not good, causes the wasting of resources.Be unworthy praising highly, it is significant therefore to seek a kind of more scientific and reasonable Kaixiong Shunqi Jiaonang preparation technology.
In view of this, outstanding the present invention.
Summary of the invention
First purpose of the present invention is to provide a kind of Kaixiong Shunqi Jiaonang, and for realizing goal of the invention, the present invention adopts following technological means:
A kind of Kaixiong Shunqi Jiaonang, described Kaixiong Shunqi Jiaonang have following proportioning by weight:
Semen Arecae 24-48, Semen Pharbitidis (stir-fry) 32-64, Pericarpium Citri Reticulatae 8-16, Radix Aucklandiae 6-18, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 8-16, rhizoma sparganic (vinegar system) 8-16, Rhizoma Curcumae (vinegar system) 8-16, Fructus Gleditsiae Abnormalis 4-10;
Described Kaixiong Shunqi Jiaonang preparation technology comprises the steps:
(1) Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae are pulverized the way of distillation and extract volatile oil, volatile oil is standby;
(2) aqueous solution after the distillation filters, filtrate, the filtering residue water decocts, filter, decocting liquid, merging filtrate and decocting liquid become water extract, medicinal residues are standby;
(3) medicinal residues after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized the back and step 2 decocting is boiled mix, and use ethanol extraction, filtration, filtrate for later use;
(4) water extract in filtrate and the step 2 in the combining step 3, precipitate with ethanol is evaporated to extractum;
(5) in extractum, add acceptable accessories, stir, pulverize behind the vacuum drying, sieve, granulate drying;
(6) volatile oil is evenly sprayed into dried granule, Kaixiong Shunqi Jiaonang is made in fill.
Described Kaixiong Shunqi Jiaonang has following proportioning by weight:
Semen Arecae 32-40, Semen Pharbitidis (stir-fry) 42-56, Pericarpium Citri Reticulatae 10-15, Radix Aucklandiae 8-12, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 10-15, rhizoma sparganic (vinegar system) 10-15, Rhizoma Curcumae (vinegar system) 10-15, Fructus Gleditsiae Abnormalis 5-8; Preferably: Semen Arecae 36, Semen Pharbitidis (stir-fry) 48, Pericarpium Citri Reticulatae 12, the Radix Aucklandiae 9, Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 12, rhizoma sparganic (vinegar system) 12, Rhizoma Curcumae (vinegar system) 12, Fructus Gleditsiae Abnormalis 6.
Second purpose of the present invention is to provide a kind of preparation technology of Kaixiong Shunqi Jiaonang, and for realizing second purpose, the present invention adopts following technical scheme:
A kind of preparation technology of Kaixiong Shunqi Jiaonang as mentioned above, described Kaixiong Shunqi Jiaonang preparation technology comprises the steps:
(1) Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae are pulverized the way of distillation and extract volatile oil, volatile oil is standby;
(2) aqueous solution after the distillation filters, filtrate, the filtering residue water decocts, filter, decocting liquid, merging filtrate and decocting liquid become water extract, medicinal residues are standby;
(3) medicinal residues after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized the back and step 2 decocting is boiled mix, and use ethanol extraction, filtration, filtrate for later use;
(4) water extract in filtrate and the step 2 in the combining step 3, precipitate with ethanol is evaporated to extractum;
(5) in extractum, add acceptable accessories, stir, pulverize behind the vacuum drying, sieve, granulate drying;
(6) volatile oil is evenly sprayed into dried granule, Kaixiong Shunqi Jiaonang is made in fill.
Described step 1 is: Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 4-8 hour with the 8-12 times of medical material water yield earlier, redistillation extracted 6-8 hour, medical material adopts decoction pieces suitably to pulverize into diameter 1cm, the preferred immersion 6 hours with 10 times of medical material water yields earlier, and redistillation extracted 7 hours.
Described step 2 is: the aqueous solution after will distilling filters, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, and each 1h filters, and merges decocting liquid filtrate for later use.
Described step 3 is: after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis pretreatment, add the medicinal residues after step 2 decocting boils, as extracting solution, is 500w-800w under irradiation 10-18 minute to extract at microwave output power with the ethanol of medical material 10-18 65-85% doubly; The ethanol of preferred 12-15 70-80% doubly is as extracting solution, is under the 600-650w irradiation 12-16 minute at microwave output power; More preferably 13 times 75% ethanol is as extracting solution, is irradiation 14 minutes under the 625w at microwave output power.
Described step 4 is: the water extract in the combining step 3 in filtrate and the step 2, and adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, supersound process 20-30 minute, left standstill 24-32 hour, and filtered, filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃).
Described step 5 is: in extractum, adds acceptable accessories, stirs, pulverize behind 80 ℃ of vacuum dryings, sieve, add the alcohol granulation of 85-95%, and preferred 95%, the granulation after drying.
Described adjuvant is starch, dextrin, lactose, Carboxymethyl cellulose sodium, micropowder silica gel, stearate or Pulvis Talci.
Described pretreatment is: be ground into 50 mesh sieves after the medical material vacuum lyophilization after will cleaning.
Pericarpium Citri Reticulatae: the bitter substance of Pericarpium Citri Reticulatae is representative " limonoid " with Fructus Citri Limoniae glycosides and bitter principle, and this limonoid flavor is gentle, easily is dissolved in water, helps the digestion of food.When Pericarpium Citri Reticulatae is used for cooking dishes.Its bitterness and other tastes are in harmonious proportion mutually, can form original in style local flavor.Pericarpium Citri Reticulatae contains compositions such as volatile oil, hesperidin, vitamin B, C, and its contained volatile oil has gentle stimulation to gastrointestinal tract, but the secretion of facilitating digestion liquid is got rid of pneumatosis in the intestinal tube, stimulating appetite.Pericarpium Citri Reticulatae also is a conventional Chinese medicine simply, has spleen invigorating, the drying dampness to eliminate phlegm of ventilation, the effect of separating greasy lasting, stopping nausea and vomiting by lowering the adverse flow of QI.
The Radix Aucklandiae: mainly contain compositions such as volatile oil, lactone.
1. volatile oil 0.3%～3%.Be mainly aplotaxene, α-Zi Luolantong, β-selinene, phellandrene, costic acid, costol, α-costene, β-costene, costunolide, camphene etc.
2. lactone: contain 12 1 melonia Dehydrocostunolide lactones, different Dehydrocostunolide lactone, α-ring costunolide, β-ring costunolide, alantolactone, isoalantolactone, saussurealactone etc.
Also contain stigmasterol, stigmasterol inulin, Radix Aucklandiae alkaloid, Betula platyphylla Suk. ester alcohol, resin etc.
The Radix Aucklandiae has excitement or suppresses two-way function gastrointestinal tract, have the secretion of facilitating digestion liquid, function of gallbladder promoting, lax tracheal smooth muscle, antibacterial, diuresis, etc. effect.
Rhizoma sparganic: rhizoma sparganic contains volatile oil, and main component is phenethanol, hydroquinone, hexadecylic acid in the oil, removes stem constuslactone etc. and multiple organic acid.
Rhizoma Curcumae: the Rhizoma Curcumae rhizome contains volatile oil 1～1.5%.Main constituent is the sesquiterpene class in the oil.A sesquialter times terpene of getting from rhizome has fluffy art epoxy ketone, zedoarone, Furanodiene., curzerene, furanodienone, isofuranodienone, paulin Rhizoma Curcumae ketenes, table furanodienone, curdiono, curcolone, Rhizoma Curcumae Longae epoxy enol difficult to understand, procurcumenol, different Rhizoma Curcumae Longae epoxy enol difficult to understand, Curcumol, curcumadiol.Also contain curcumin, dehydrocurdione.Dried root starch-containing about 64%.
Semen Arecae: contain the nutrient and the benefit materials of multiple needed by human body in the Semen Arecae fruit, as compositions such as fat, betel oil, alkaloid, catechin, choline.Semen Arecae has unique imperial miasma function, is the medicine fruit that ancient Chinese medicine doctor is cured the disease, and the another name of " washing the miasma pellet " is arranged again.Because the disease of communicable subtropical diseases, generally all irregular with diet, the stagnation of QI is long-pending to have the pass, and Semen Arecae can the therapeutic method to keep the adverse QI flowing downwards, help digestion, eliminate the phlegm, so on pharmaceutical characteristic by people's extensive concern.
Semen Arecae contains alkaloid 0.3-0.6%, condensed tannin 15%, and fat 14% and areca red etc., wherein the alkaloid master is an arecoline, content 0.1-0.5%.All the other have arecaidine, demethyl arecaidine, its methyl arecoline etc.
Cortex Magnoliae Officinalis: it is about 1% that Cortex Magnoliae Officinalis contains volatile oil, mainly contains β-eucalyptol honokiol in the oil.In addition, also contain a spot of magnocurarine, magnocurarine and tannin etc.
Semen Pharbitidis: the Semen Pharbitidis master contains pharbitin (resin glycoside), fatty oil, organic acid etc.Semen Pharbitidis is the medicine of drastic purgation, and is few with logical stool then, many with then rushing down down as water, and the energy diuresis, so be mainly used in diseases such as ascites swelling, difficulty in urination and defecation and dyspepsia stagnate, constipation clinically.
Fructus Gleditsiae Abnormalis: Fructus Gleditsiae Abnormalis mainly contains polytype three-iron Saponin, also has compositions such as tannin, vinegar alcohol, stigmasterol and other biological alkali in addition.
According to the contained composition of prescription Chinese crude drug, we can be divided into it two classes.Contain the volatile ingredient medical material: Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae, owing to effective ingredient in the four Chinese medicine material in the side mostly is a volatile oil, therefore extraction process can adopt the way of distillation to extract volatile oil, medicinal residues further extract avoiding the wherein loss of fat-soluble effective ingredient by ethanol water again, thereby improve the utilization rate of medical material; Contain the unclear medical material of water soluble ingredient or composition: Semen Pharbitidis, Semen Arecae, Fructus Gleditsiae Abnormalis, Cortex Magnoliae Officinalis.According to the effective ingredient of four kinds of medical materials as can be known, adopting alcoholic acid aqueous solution that it is carried out reflux, extract, is optimal extraction way.
1, the extraction of Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae
Because Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae contain volatile effective ingredient, so select for use steam distillation to extract volatile oil, and keep the filtrate after the distillation, for fear of other composition loss, with the medicinal residues reuse ethanol extraction behind the extraction volatile oil.
(1) steam distillation extracts the preferred of volatile oil technical conditions in Pericarpium Citri Reticulatae, the Radix Aucklandiae, rhizoma sparganic, the Rhizoma Curcumae
Use steam distillation and extract operation, from prerun as can be known, the retortable extraction of contained volatile oil in the crude drug, the principal element that the volatile oil effect is extracted in influence is a distillation time, the inventor has carried out following test on the trial test basis:
To add water multiple (A), soak time (B), distillation time (C), medical material degree of fragmentation (D) four factors, the volatile oil quantities received is an index, adopts orthogonal experiment arrangement test, and the volatile oil extraction process of the best is carried out preferably.
(1) preparation of sample liquid
In the prescription ratio, accurately take by weighing totally 9 parts of Pericarpium Citri Reticulatae, the Radix Aucklandiae, rhizoma sparganic, the Rhizoma Curcumae (rhizoma sparganic is 120g) of recipe quantity, soak certain hour by the listed EXPERIMENTAL DESIGN condition of table 1, hydrodistillation distillation certain hour, collect volatile oil, placed 1 hour, precision is measured volume.
(2) result of the test: orthogonal experiments sees Table 2.
Table 1 way of distillation is extracted volatile oil and is investigated the factor level table
Table 2 orthogonal test scheme and result
Above-mentioned data are carried out variance analysis, and the inventor has carried out expansion among a small circle to each factor level on this basis and result of the test has been analyzed, and thinks that redistillation extracted 6-8 hour when adopting 8-12 times of medical material water yield to soak 4-8 hour.When medical material adopted decoction pieces suitably to pulverize into the following fragment of diameter 1cm, extraction effect was comparatively desirable.The preferred immersion 6 hours with 10 times of medical material water yields earlier, redistillation extracted 7 hours.
For the relation of four Chinese medicine material volatile oil extraction time such as further research Pericarpium Citri Reticulatae and yield, the inventor has done further test:
Other gets a collection of medical material Pericarpium Citri Reticulatae, the Radix Aucklandiae, Rhizoma Curcumae, rhizoma sparganic pulverize separately and crosses sieve No. 3, gets about 100g respectively and weighs (accurately to 0.01g), measures volatile oil content respectively distinguish the flavor of medical material volatile oil total content such as table 3 by an appendix determination of volatile oil of pharmacopeia method respectively:
Respectively the distinguish the flavor of mensuration of medical material volatile oil content of table 3
| Medical material sampling amount (g) | Volatile oil total amount (ml) | Volatile oil content % | |
| Pericarpium Citri Reticulatae | 101.8 | 1.11 | 1.10 |
| The Radix Aucklandiae | 102.1 | 0.76 | 0.75 |
| Rhizoma Curcumae | 101.6 | 0.48 | 0.48 |
| Rhizoma sparganic | 99.8 | 0.69 | 0.69 |
Annotate: material that this test is got it filled and the used medical material of orthogonal test are non-with batch medical material, and volatile oil content has difference.
Criticize medical material together with above four kinds and be broken into fragment respectively, every duplicate samples with placing the 3000ml round-bottomed flask, adds water 2400ml by every kind of medical material difference 100g, each minute, sample was respectively by following time distillating extracting oil, 2h, 4h, 6h, 8h, 10h by carrying to such an extent that the volatilization oil mass calculates rate, the results are shown in Table 4.
The result of the test of table 4 volatile oil extraction time and yield relation
| Sample number into spectrum | Medical material amount (g) | The distillation extraction time (h) | Volatile oil carry the amount (ml/g) | Medical material volatile oil is carried yield % (ml/l) | Total volatile oil extraction ratio % |
| 1 | 400g | 2 | 0.9 | 0.23 | 29.8 |
| 2 | 400g | 4 | 1.5 | 0.4 | 49.6 |
| 3 | 400g | 6 | 1.9 | 0.5 | 62.9 |
| 4 | 400g | 8 | 2.5 | 0.63 | 82.8 |
| 5 | 400g | 10 | 2.6 | 0.67 | 86.1 |
The result shows, four Chinese medicine material such as Pericarpium Citri Reticulatae extraction time, the volatile oil extraction ratio rose obviously along with time lengthening in the 2-8h scope, and extraction ratio rises not obvious behind the 8h.Therefore further specifying four flavor volatile oil extraction times such as Pericarpium Citri Reticulatae, to be decided to be 6-8h be rational.
2,4 flavor water extraction process researchs such as Pericarpium Citri Reticulatae
4 flavor medical materials such as Pericarpium Citri Reticulatae are after the way of distillation is extracted volatile oil, though water is carried 8 hours, but the reasonability to further extraction process must be investigated, we are index with hesperidin content in the high effective liquid chromatography for measuring extractum for this reason, extraction time, amount of water, extraction time are factor again with medicinal residues, each designs 2 levels and makes orthogonal test, arranges and the results are shown in Table 5,6.
Table 5 factor level
| Factor level | Extraction time A again | Amount of water B | Extraction time C |
| 1 | 1 time | 6 times | 1h |
| 2 | 2 times | 8 times | 1.5h |
Table 6 orthogonal test scheme and result
| Row hydraulic test number | 1 (A) | 2 (B) | 3 (C) | Result of the test hesperidin content % (mg/mg) |
| 1 2 3 4 | 1 1 2 2 | 1 2 1 2 | 1 1 2 2 | 2.46 2.52 2.41 2.58 |
| K1 | 4.98 | 4.87 | 4.98 | |
| K2 R | 4.99 0.01 | 5.10 0.23 | 4.99 0.01 |
After above-mentioned data are carried out variance analysis, according to result and each group test gained hesperidin content height, because four Chinese medicine is through 8 hours water extraction in the leaching process of volatile oil, therefore extraction time and extraction time are not remarkable to extraction effect again, therefore, the present invention adopts the medicinal residues after the water distillation is added 6 times of water extraction 1 time, each 1 hour again.
3, the extraction process of Cortex Magnoliae Officinalis, Semen Pharbitidis, Semen Arecae, Fructus Gleditsiae Abnormalis
Prior art discloses a kind of method of utilizing ethanol extraction Cortex Magnoliae Officinalis, Semen Pharbitidis, Semen Arecae, rhizoma sparganic, Fructus Gleditsiae Abnormalis, be specially: with above medical material with 70% alcohol reflux 2 times, the total ethanol consumption is 12 times of medical material amount, and reflux extracting time is 2.5h for the first time, and the 2nd time is 1.5 hours.In the new technology that the present invention proposes, the inventor extracts volatile oil according to the composition of rhizoma sparganic earlier with rhizoma sparganic and Pericarpium Citri Reticulatae, the Radix Aucklandiae, Rhizoma Curcumae, and the aqueous solution after the distillation filters, and in order further to extract the water soluble ingredient in the four Chinese medicine material, medicinal residues is decocted once again.The loss of other effective ingredient in the above-mentioned medical material simultaneously, medicinal residues and Cortex Magnoliae Officinalis, Semen Pharbitidis, Semen Arecae, Fructus Gleditsiae Abnormalis one after the present invention boils decocting are reinstated ethanol extraction.
Tradition ethanol reflux extraction extraction time is long, effective ingredient such as arecoline honokiol are destroyed in leaching process easily, in addition, because every medicinal ingredient has than big-difference, the thoroughly stripping of effective ingredient when adopting alcohol reflux in the lump in the part medical material causes extraction ratio low.Adopt 50% ethanol extraction 2 times as magnolol, add 10 times of amounts of alcohol for the 1st time, extract 1h, add extracting mode that 8 times of amounts of alcohol extract 1h for the 2nd time and generally can obtain high extraction, and under this extraction conditions, the extraction ratio of arecoline is quite undesirable, and the extraction effect of Semen Pharbitidis and Fructus Gleditsiae Abnormalis is also relatively poor.Employing mixes medical material after traditional ethanol refluxing process extracts can't make the four Chinese medicine material obtain the optimum extraction effect simultaneously.Therefore, in order to simplify the preparation technology of Kaixiong Shunqi Jiaonang, the present invention need seek a kind of extracting mode of suitable four Chinese medicine material co-extracted.
For a kind of more scientific and reasonable extraction scheme is provided, the inventor has done a large amount of experiments, experimental result shows no matter adopt microwave extraction to replace alcohol reflux of the prior art is in the time of extracting or aspect the extraction efficiency, all has the progress of significance.
Because microwave carries out from material molecule the heating of material, is called " internal heating " again, in Effective Components of Chinese Herb was extracted, microwave had very strong penetration power, can be inside and outside the medical material granule simultaneously evenly, and heating promptly.Simultaneously, after the Chinese crude drug cell absorbs microwave energy, the cell interior temperature rises rapidly, its cell interior aqueous water vaporization produces pressure cell membrane and cell wall is impacted, form small hole, make that the extracellular solvent is easier to be entered in the cell, accelerate dissolution also discharges effective ingredient rapidly, and cell integrity still keeps.Because microwave extraction solution in extraction does not seethe with excitement, save energy in addition, shortened extraction time greatly, improved extraction efficiency.And adopting microwave extraction to can be good at taking into account the extraction ratio of four Chinese medicine material, is preparation technology's of the present invention optimum extraction mode.
At ethanol is under the prerequisite of optimum extraction solvent, after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis pretreatment, adding the medicinal residues after step 2 decocting boils, as extracting solution, is 500w-800w under irradiation 10-18 minute to extract at microwave output power with the ethanol of medical material 10-18 65-85% doubly.The ethanol of preferred 12-15 70-80% doubly is as extracting solution, at microwave output power is to extract in irradiation 12-16 minute under the 600-650w, more preferably 13 times 75% ethanol is that irradiation extracted in 14 minutes under the 625w as extracting solution at microwave output power.The present invention can adopt any energy realization Microwave Extraction Equipment of the present invention in the prior art.
The present invention adopts the mode of microwave extraction, microwave extraction has homogeneous heating, speed is fast, heat is imitated advantages of higher, extracting through microwave heating is compared with alcohol reflux, it is characterized in that its heat results from the inside of heated material, and microwave extraction has eliminated in the heating process because air, the thermal loss that the conduction of heat of chamber wall and radiation etc. cause and be heated inhomogeneous etc.Therefore, microwave extraction can add the extraction efficiency of strong solvent, compares with ethanol refluxing process, has the extraction efficiency height, extraction ratio height, the characteristics of more effectively having preserved the effective ingredient in the medicine.
The pretreatment of medical material is the important indicator that influences the medicinal material extract rate, so the inventor has also done corresponding research at the pretreatment of medical material.Arecoline is a kind of nitrogenous heterocyclic alkalescence organic-biological alkali, the drying mode of Semen Arecae, pulverizing dynamics have a significant impact the extraction ratio of arecoline, thereby realize effective extraction of arecoline for the Semen Arecae pretreatment mode of finding out science, the inventor has done system experimentation, draw cleaned Semen Arecae adopted vacuum drying method drying after, extract after being ground into the granule of 50 mesh sieves, can obtain best extraction ratio, concrete experimental result sees Table 7,8.
Table 7 drying means is to the influence of arecoline extraction ratio (%)
As can be seen from Table 7, vacuum drying is to the minimum that influences of Semen Arecae chemical constituent, and through the Semen Arecae of vacuum lyophilization, wherein the extraction ratio of arecoline is obviously more than other two kinds of drying modes.
Table 8 grinding particle size is to the influence of arecoline extraction ratio (%)
| The order number | 30 | 40 | 50 | 60 | 80 |
| The arecoline extraction ratio | 0.35 | 0.41 | 0.44 | 0.44 | 0.44 |
Dried Semen Arecae is difficult to be pulverized, by the result of table 8 as seen, areca powder was broken into 50 orders, 60 orders and 80 mesh sieves, granularity has very big difference, but the result is constant for the arecoline assay, and, therefore, can think to be ground into the extraction ratio that 50 mesh sieves help improving arecoline apparently higher than the Semen Arecae of 30 orders and 40 mesh sieves.
The inventor has also done similar experiment to the pretreatment mode of Cortex Magnoliae Officinalis and Semen Pharbitidis, Fructus Gleditsiae Abnormalis, and the result shows, the four Chinese medicine material is peace and quiet, was ground into 50 mesh sieves and carries out microwave extraction after vacuum lyophilization, and the extraction ratio of each medical material of distinguishing the flavor of is the best.
With arecoline honokiol and honokiol content is index, and the relative prior art of the technology that the present invention protected has had the progress of significance.
Concrete outcome sees Table 10 and pharmacodynamics test research.
4, granulating process determines
The preparation of Chinese medicine granules generally is to be concentrated into the clear paste of certain density after the medicinal material extract, adds adjuvant (as dextrin, starch etc.), mixes wet method or dry granulation thoroughly.The present invention adopts the decocting liquid with medicines such as ethanol extract and Pericarpium Citri Reticulataes to merge, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stir, supersound process 20-30 minute, left standstill 24-32 hour, filter, filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃), granulates again.
Utilize ultransonic cavitation herein, also have the mechanical vibration effect, smash the effect of various ways such as effect, chemical effect, help fully disengaging of effective ingredient, further improve extraction efficiency.
Because it is consistent that the density of extractum is difficult to control, influences supplementary product consumption and method of granulating, also make in the finished product every gram granule contain the crude drug amount and differ greatly.Therefore, we add other adjuvants of pharmaceutically accepting such as an amount of filler such as starch, dextrin, lactose, Carboxymethyl cellulose sodium, micropowder silica gel, stearate or Pulvis Talci, and drying under reduced pressure become dried cream after extracting solution is concentrated, be ground into fine powder, make granule.
Adopt 85% ethanol, 95% ethanol and dehydrated alcohol to carry out wet method system granule in the test respectively as wetting agent.We have investigated the granule situation that makes of said method from granulation complexity, degree of dissolving, granularity, grain color several respects, the results are shown in Table 9.
Table 9 granulating process comparative test result
Result of the test shows that 95% ethanol system granule effect is better, so we adopt 95% ethanol system granule.
Evenly spray into volatile oil in the dried particles for preparing, the fill capsule gets final product.
Adopt technique scheme, the Kaixiong Shunqi Jiaonang with prescription in the quality of the Kaixiong Shunqi Jiaonang that the inventor is prepared with this technology and the prior art contrasts, and the present invention has obtained very good improvement effect in every respect, the results are shown in Table 10.
Wherein arecoline adopts titration measuring (with reference to 1995 editions one one of Chinese Pharmacopoeia, method is measured under the Semen Arecae medical material assay item).With tlc scanning determination magnolol and honokiol content (with reference to 1995 editions one one of Chinese Pharmacopoeia, appendix VIB thin layer chromatography scanning) composition measurement with the above-mentioned content of capsule among batch pill of medical material preparation and prior art and the present invention two be the results are shown in Table 10;
The content of arecoline and magnolol and honokiol in table 10 different dosage form
| Arecoline content mg/g | Magnolol and honokiol content mg/g | |
| Kaixiong Shunqi Jiaonang (having now) | 2.36 | 8.24 |
| The present invention | 2.79 | 9.43 |
The result shows that the preparation technology that the present invention protected can significantly improve the extraction ratio of arecoline and magnolol and honokiol, and the improvement of technology this time has the progress of significance.
Compared with prior art, the present invention is on former Kaixiong Shunqi Jiaonang prescription basis, through a kind of new Kaixiong Shunqi Jiaonang preparation technology of repetition test, contrast, conclusion, screening, summary acquisition.After adopting above-mentioned technological means, the present invention has following beneficial effect:
1, above-mentioned preparation technology is scientific and reasonable, the various raw-material property of medicine and composition have been taken into full account, by optimizing raw-material extraction process, the most active component that kept medical material, improve the extraction efficiency of medicine and effectively removed the impurity in the medical material, improved the drug effect and the stability of medicine.
2, adopting microwave-assisted to extract extracts medical material; there is not high temperature heat source; eliminated thermal gradient; thereby the extraction quality is improved greatly, effectively protect the effective ingredient in the medical material, because the penetrable formula heating of microwave; the time of extracting is saved greatly; microwave energy has extraordinary extractability, can a defecation under microwave field, simplify technological process greatly.Microwave extraction thing purity height, it is low to extract temperature, is difficult for gelatinizing, separates easily, and convenient post-treatment is saved the energy.
3, compare with the preparation technology of existing Kaixiong Shunqi Jiaonang, the purity and the curative effect of the capsule product of prepared disclosed by the invention all are improved, and this improvement has very large clinical meaning, social meaning, also has good economic benefit and application prospect simultaneously.
The specific embodiment
Embodiment 1
Take by weighing the raw material of following proportioning:
Semen Arecae 360g Semen Pharbitidis (stir-fry) 480g Pericarpium Citri Reticulatae 120g Radix Aucklandiae 90g
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 120g rhizoma sparganic (vinegar system) 120g Rhizoma Curcumae (vinegar system) 120g Fructus Gleditsiae Abnormalis 60g
Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 6 hours with 10 times of medical material water yields earlier, and redistillation extracted 7 hours.Medical material adopts decoction pieces suitably to pulverize into diameter 1cm.Aqueous solution after the distillation is filtered, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, and each 1h filters, and merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis after cleaning being ground into 50 mesh sieves after vacuum lyophilization, adding above-mentioned medicinal residues, as extracting solution, is 625w under irradiation 14 minute at microwave output power with 75% ethanol of 13 times of medical materials.
Water extract in the combining step 3 in filtrate and the step 2, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, and supersound process 25 minutes left standstill 32 hours, filtered, and filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃).
In extractum, add appropriate amount of starch, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add 95% alcohol granulation, the granulation after drying.Volatile oil is evenly sprayed into dried granule, and Kaixiong Shunqi Jiaonang is made in fill.
Embodiment 2
Take by weighing the raw material of following proportioning:
Semen Arecae 240g Semen Pharbitidis (stir-fry) 320g Pericarpium Citri Reticulatae 80g Radix Aucklandiae 60g
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 80g rhizoma sparganic (vinegar system) 80g Rhizoma Curcumae (vinegar system) 80g Fructus Gleditsiae Abnormalis 40g
Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 4 hours with 8 times of medical material water yields earlier, and redistillation extracted 6 hours, and medical material adopts decoction pieces suitably to pulverize into diameter 1cm.
Aqueous solution after the distillation is filtered, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, and each 1h filters, and merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis after cleaning were ground into 50 mesh sieves after vacuum lyophilization, add the medicinal residues after step 2 decocting boils, as extracting solution, is that 500w under irradiation 18 minute extract at microwave output power with 85% ethanol of 10 times of medical materials.
Water extract in the combining step 3 in filtrate and the step 2, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, and supersound process 20 minutes left standstill 24 hours, filtered, and filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃).
In extractum, add an amount of Pulvis Talci, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add 85% alcohol granulation, the granulation after drying.Volatile oil is evenly sprayed into dried granule, and Kaixiong Shunqi Jiaonang is made in fill.
Embodiment 3
Take by weighing the raw material of following proportioning:
Semen Arecae 320 Semen Pharbitidiss (stir-fry) 420 Pericarpium Citri Reticulataes 100 Radix Aucklandiae 80
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 100 rhizoma sparganic (vinegar system) 100 Rhizoma Curcumae (vinegar system) 100 Fructus Gleditsiae Abnormalis 50
Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 7 hours with 9 times of medical material water yields earlier, and redistillation extracted 7 hours.Medical material adopts decoction pieces suitably to pulverize into diameter 1cm.
Aqueous solution after the distillation is filtered, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, and each 1h filters, and merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
With the Fructus Gleditsiae Abnormalis after cleaning, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis after being ground into 50 mesh sieves after the vacuum lyophilization, add the medicinal residues after step 2 decocting boils, as extracting solution, is that 600w under irradiation 12 minute extract at microwave output power with 70% ethanol of 12 times of medical materials.
Water extract in the combining step 3 in filtrate and the step 2, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, and supersound process 25 minutes left standstill 28 hours, filtered, and filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃).
In extractum, add an amount of dextrin, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add 85% alcohol granulation, the granulation after drying.Volatile oil is evenly sprayed into dried granule, and Kaixiong Shunqi Jiaonang is made in fill.
Embodiment 4
Take by weighing the raw material of following proportioning:
Semen Arecae 400 Semen Pharbitidiss (stir-fry) 560 Pericarpium Citri Reticulataes 150 Radix Aucklandiae 120
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 150 rhizoma sparganic (vinegar system) 150 Rhizoma Curcumae (vinegar system) 150 Fructus Gleditsiae Abnormalis 80
Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 6 hours with 10 times of medical material water yields earlier, and redistillation extracted 7 hours.Medical material adopts decoction pieces suitably to pulverize into diameter 1cm.
Aqueous solution after the distillation is filtered, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, and each 1h filters, and merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
To clean back Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis after being ground into 50 mesh sieves after the vacuum lyophilization, and add the medicinal residues after step 2 decocting boils, as extracting solution, be 650w under irradiation 16 minute at microwave output power with 75% ethanol of 15 times of medical materials.
Water extract in the combining step 3 in filtrate and the step 2, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stir, supersound process 20-30 minute, left standstill 32 hours, filter, filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃).
In extractum, add an amount of lactose, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add 95% alcohol granulation, the granulation after drying.Volatile oil is evenly sprayed into dried granule, and Kaixiong Shunqi Jiaonang is made in fill.
Embodiment 5
Take by weighing the raw material of following proportioning:
Semen Arecae 480 Semen Pharbitidiss (stir-fry) 640 Pericarpium Citri Reticulataes 160 Radix Aucklandiae 180
Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 160 rhizoma sparganic (vinegar system) 160 Rhizoma Curcumae (vinegar system) 160 Fructus Gleditsiae Abnormalis 100
Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 8 hours with 12 times of medical material water yields earlier, and redistillation extracted 8 hours.Medical material adopts decoction pieces suitably to pulverize into diameter 1cm.
Aqueous solution after the distillation is filtered, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, and each 1h filters, and merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
With the Fructus Gleditsiae Abnormalis after cleaning, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis after being ground into 50 mesh sieves after the vacuum lyophilization, add the medicinal residues after step 2 decocting boils, as extracting solution, is that 800w under irradiation 18 minute extract at microwave output power with 85% ethanol of 15 times of medical materials.
Water extract in the combining step 3 in filtrate and the step 2, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, and supersound process 30 minutes left standstill 32 hours, filtered, and filtrate recycling ethanol also is evaporated to the extractum of 1.24-1.28 (80 ℃).
In extractum, add an amount of magnesium stearate, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add 95% alcohol granulation, the granulation after drying.Volatile oil is evenly sprayed into dried granule, and Kaixiong Shunqi Jiaonang is made in fill.
In order further to verify stability, safety and the curative effect thereof of the Kaixiong Shunqi Jiaonang that the present invention protected, the inventor has done a series of clinical research to the present invention, specifically sees pharmacodynamics test.
Test example 1
(1), testing data
Selection meets stagnation of QI due to dyspepsia card case 300 examples of Chinese medical discrimination standard, 134 examples of wherein being in hospital, outpatient service 166 examples, be divided into by single blind randomized and open EXPERIMENTAL DESIGN that 100 examples are organized in treatment, matched group 1 is that 100 examples and matched group 2 are 100 examples, wherein male 48 examples are organized in treatment, woman's 52 examples, mean age 43.6+14.1 year (20-65 year); Matched group man 53 years old, women 47 examples, mean age 44.1+13.9 year (20-65 year); Open treatment group man 51 examples, women 49 examples, mean age 46.1+14.2 year (22-66 year).Three groups age and sex there was no significant difference have comparability.
(2) diagnose and receive people's standard:
Have outside the dietary history such as eating and drinking without temperance, eating cold and uncooked food excessively or greasy, meat, following symptom still arranged:
1, fullness and distention in the chest and hypochondrium; 2, gastralgia; 3, belching and acid regurgitation; 4, indigestion and loss of appetite; 5, nausea and vomiting;
6, thick fur is greasy white or yellow; 7, stringy and rolling pulse or heavy sliding strong.
Except that the tongue arteries and veins, all medical histories that meets possess in the 1-5 item three or above person and can be diagnosed as the stagnation of QI due to dyspepsia card, and onset is no more than 2d person, can include the test case in.
(3) effect criterion
Clinical recovery: symptom, sign disappear, and integration reduces to 0;
Significantly: symptom, sign disappear substantially, and integration descends 2/3;
Effectively: symptom, sign all make moderate progress, integration descend 1/3 or more than;
Invalid: symptom, sign do not have obvious improvement, even increase the weight of.
Table 11 clinical symptoms weight grade scale
(4) method of administration
Test group: take the embodiment of the invention 1 described Kaixiong Shunqi Jiaonang, one time 3 (0.35g/ grain), 2 times on the one, 3 days is a course of treatment.
Matched group 1: existing Kaixiong Shunqi Jiaonang, one time 3 (0.35g/ bag), 2 times on the one, 3 days is a course of treatment.
Matched group 2: existing Kaixiong Shunqi Wan, a 4.5g, 2 times on the one, 3 days is a course of treatment.
All in the treatment beginning, treatment finishes to write down respectively the symptom variation situation to each group.Symptom adopts semiquantitative method, asymptomatic note (-), 0 minute, light disease note (+), 1 minute, moderate disease note (++), 2 minutes, serious symptom note (+++), 3 minutes.
(5) safety observation index: 1, general health check-up index; 2, blood, urine, routine inspection of excrement; Liver function (ALT), renal function (Cr, BUN), electrocardiogram; 4 untoward reaction.
(6) effect analysis
Get test group 30 routine cases and before and after treatment, make related experiment chamber index observing, the results are shown in Table 12.
Table 12 test group lab index observed result
| Inspection item | The example number | Before the treatment | After the treatment | The P value |
| Hb(g/L) | 30 | 129.2±9.1 | 127.3±16.9 | ＞0.05 |
| WBC(*10 7/L) | 30 | 6.71±1.98 | 6.43±1.99 | ＞0.05 |
| ALT(TU/L) | 30 | 27.5±33.5 | 23.8±27.4 | ＞0.05 |
| Cr(μm/L) | 30 | 81.6±30.89 | 81.86±32.9 | ＞0.05 |
| BUN(mmol/L) | 30 | 5.72±2.56 | 5.76±2.27 | ＞0.05 |
The comparative analysis of table 13 general effect
As can be seen from the above table, total obvious effective rate of test group is apparently higher than matched group 1,2, and up to 87%, in addition, total effective rate is also than the matched group height.As seen, Kaixiong Shunqi Jiaonang disclosed in this invention Kaixiong Shunqi Jiaonang more of the prior art or Kaixiong Shunqi Wan, its curative effect has had the significance raising, and as seen, this time preparation technology's improvement is significant.
Table 14 test group symptom and effect analysis
As can be seen from the above table, symptom and effect have notable difference, and there is the significance meaning statistical procedures P＜0.05.
(7) untoward reaction
In clinical trial, all cases of treatment group and matched group are and any untoward reaction occurs.
(8) brief summary
Take one course of treatment of the described Kaixiong Shunqi Jiaonang of the embodiment of the invention 1 by 100 routine experimenters, the result shows, Kaixiong Shunqi Jiaonang of the present invention to fullness and distention in the chest and hypochondrium, gastral cavity pain, belching and acid regurgitation, indigestion and loss of appetite, nausea and vomiting, thick fur is greasy or white or Huang etc. have remarkable result, its total obvious effective rate is up to 87%, total effective rate reaches 98%, matched group 1 existing Kaixiong Shunqi Jiaonang, its total obvious effective rate is 70%, total effective rate is 94%, matched group 2 adopts Kaixiong Shunqi Wan, its total obvious effective rate is 62%, and total effective rate is 90%.The result shows that the test group effect significantly is better than matched group and 1,2, three groups untoward reaction does not take place all, thereby illustrates that Kaixiong Shunqi Jiaonang of the present invention is a kind of safe and reliable pleasant medicine of breast of opening.
Other embodiments of the invention are also carried out identical test, obtained the result who is close with embodiment 1.
Claims (20)
1. Kaixiong Shunqi Jiaonang, described Kaixiong Shunqi Jiaonang has following proportioning by weight:
Semen Arecae 24-48 part, Semen Pharbitidis (parched) 32-64 part, Pericarpium Citri Reticulatae 8-16 part, Radix Aucklandiae 6-18 part, Sichuan Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 8-16 part, vinegar system rhizoma sparganic 8-16 part, Rhizoma Curcumae (processed with vinegar) 8-16 part, Fructus Gleditsiae Abnormalis 4-10 part;
It is characterized in that: described Kaixiong Shunqi Jiaonang preparation technology comprises the steps:
(1) Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae are pulverized the way of distillation and extract volatile oil, volatile oil is standby;
(2) aqueous solution after the distillation filters, filtrate, the filtering residue water decocts, filter, decocting liquid, merging filtrate and decocting liquid become water extract, medicinal residues are standby;
(3) Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized after, add the medicinal residues after step 2 decocting boils, as extracting solution, be to extract in irradiation 10-18 minute under the 500w-800w with the ethanol of medical material 10-18 65-85% doubly at microwave output power; Filter filtrate for later use;
(4) water extract in filtrate and the step 2 in the combining step 3, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, supersound process 20-30 minute, left standstill 24-32 hour, and filtered, filtrate recycling ethanol and when being evaporated to 80 ℃ relative density be the extractum of 1.24-1.28;
(5) in extractum, add acceptable accessories, stir, pulverize behind the vacuum drying, sieve, granulate drying;
(6) volatile oil is evenly sprayed into dried granule, Kaixiong Shunqi Jiaonang is made in fill.
2. a kind of Kaixiong Shunqi Jiaonang according to claim 1 is characterized in that: described Kaixiong Shunqi Jiaonang has following proportioning by weight:
Semen Arecae 32-40 part, Semen Pharbitidis (parched) 42-56 part, Pericarpium Citri Reticulatae 10-15 part, Radix Aucklandiae 8-12 part, Sichuan Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens) 10-15 part, vinegar system rhizoma sparganic 10-15 part, Rhizoma Curcumae (processed with vinegar) 10-15 part, Fructus Gleditsiae Abnormalis 5-8 part.
3. a kind of Kaixiong Shunqi Jiaonang according to claim 2 is characterized in that: described Kaixiong Shunqi Jiaonang has following proportioning by weight:
36 parts of Semen Arecaes, 48 parts of Semen Pharbitidis (parched), 12 parts of Pericarpium Citri Reticulataes, 9 parts of the Radix Aucklandiae, 12 parts of Sichuan Cortex Magnoliae Officinalis (processed with Rhizoma Zingiberis Recens), 12 parts of vinegar system rhizoma sparganic, 12 parts of Rhizoma Curcumae (processed with vinegar), 6 parts of Fructus Gleditsiae Abnormalis.
4. a kind of Kaixiong Shunqi Jiaonang according to claim 1, it is characterized in that: described step 1 is: Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 4-8 hour with the 8-12 times of medical material water yield earlier, redistillation extracted 6-8 hour, and medical material adopts decoction pieces suitably to pulverize into diameter 1cm.
5. a kind of Kaixiong Shunqi Jiaonang according to claim 4 is characterized in that: described step 1 is: Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 6 hours with 10 times of medical material water yields earlier, and redistillation extracted 7 hours.
6. a kind of Kaixiong Shunqi Jiaonang according to claim 1 is characterized in that: described step 2 is: the aqueous solution after will distilling filters, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, each 1h, filter, merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
7. a kind of Kaixiong Shunqi Jiaonang according to claim 1, it is characterized in that: described step 3 is: after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized, add the medicinal residues after step 2 decocting boils, as extracting solution, is 600-650w under irradiation 12-16 minute at microwave output power with the ethanol of 12-15 70-80% doubly.
8. a kind of Kaixiong Shunqi Jiaonang according to claim 7, it is characterized in that: described step 3 is: after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized, add the medicinal residues after step 2 decocting boils, as extracting solution, is 625w under irradiation 14 minute at microwave output power with 13 times 75% ethanol.
9. a kind of Kaixiong Shunqi Jiaonang according to claim 1 is characterized in that: described step 5 is: add acceptable accessories in extractum, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add the alcohol granulation of 85-95%, the granulation after drying.
10. a kind of Kaixiong Shunqi Jiaonang according to claim 1 is characterized in that: described adjuvant is starch, dextrin, lactose, Carboxymethyl cellulose sodium, micropowder silica gel, stearate or Pulvis Talci.
11. a kind of Kaixiong Shunqi Jiaonang according to claim 1 is characterized in that: described pulverizing is: be ground into 50 mesh sieves after the medical material vacuum lyophilization after will cleaning.
12. the preparation technology of a Kaixiong Shunqi Jiaonang as claimed in claim 1 is characterized in that: described Kaixiong Shunqi Jiaonang preparation technology comprises the steps:
(1) Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae are pulverized the way of distillation and extract volatile oil, volatile oil is standby;
(2) aqueous solution after the distillation filters, filtrate, the filtering residue water decocts, filter, decocting liquid, merging filtrate and decocting liquid become water extract, medicinal residues are standby;
(3) Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized after, add the medicinal residues after step 2 decocting boils, as extracting solution, be to extract in irradiation 10-18 minute under the 500w-800w with the ethanol of medical material 10-18 65-85% doubly at microwave output power; Filter filtrate for later use;
(4) water extract in filtrate and the step 2 in the combining step 3, adding ethanol in amalgamation liquid is 70% to containing the alcohol amount, fully stirs, supersound process 20-30 minute, left standstill 24-32 hour, and filtered, filtrate recycling ethanol and when being evaporated to 80 ℃ relative density be the extractum of 1.24-1.28;
(5) in extractum, add acceptable accessories, stir, pulverize behind the vacuum drying, sieve, granulate drying;
(6) volatile oil is evenly sprayed into dried granule, Kaixiong Shunqi Jiaonang is made in fill.
13. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 12, it is characterized in that: described step 1 is: Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 4-8 hour with the 8-12 times of medical material water yield earlier, redistillation extracted 6-8 hour, and medical material adopts decoction pieces suitably to pulverize into diameter 1cm.
14. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 13 is characterized in that: described step 1 is: Pericarpium Citri Reticulatae, Rhizoma Curcumae, rhizoma sparganic, the Radix Aucklandiae were soaked 6 hours with 10 times of medical material water yields earlier, and redistillation extracted 7 hours.
15. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 12 is characterized in that: described step 2 is: the aqueous solution after will distilling filters, and medicinal residues boil 1 time with the decocting of 6 times of medical material amounts, each 1h, filter, merging filtrate and decocting liquid become water extract, and medicinal residues are standby.
16. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 12, it is characterized in that: described step 3 is: after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized, add the medicinal residues after step 2 decocting boils, as extracting solution, is 600-650w under irradiation 12-16 minute at microwave output power with the ethanol of medical material 12-15 70-80% doubly.
17. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 16, it is characterized in that: described step 3 is: after Fructus Gleditsiae Abnormalis, Semen Arecae, Cortex Magnoliae Officinalis, Semen Pharbitidis are pulverized, add the medicinal residues after step 2 decocting boils, as extracting solution, is 625w under irradiation 14 minute at microwave output power with 75% ethanol of 13 times of medical materials.
18. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 12 is characterized in that: described step 5 is: add acceptable accessories in extractum, stir, pulverize behind 80 ℃ of vacuum dryings, sieve, add the alcohol granulation of 85-95%, the granulation after drying.
19. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 12 is characterized in that: described adjuvant is starch, dextrin, lactose, Carboxymethyl cellulose sodium, micropowder silica gel, stearate or Pulvis Talci.
20. the preparation technology of Kaixiong Shunqi Jiaonang according to claim 12 is characterized in that: described pulverizing is: be ground into 50 mesh sieves after the medical material vacuum lyophilization after will cleaning.
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| CN2010101520151A CN101797365B (en) | 2010-04-21 | 2010-04-21 | Preparation technology of Kaixiong Shunqi Jiaonang |
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| CN2010101520151A CN101797365B (en) | 2010-04-21 | 2010-04-21 | Preparation technology of Kaixiong Shunqi Jiaonang |
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| CN108671206A (en) * | 2018-08-09 | 2018-10-19 | 河南润弘本草制药有限公司 | Pleasant digestant Chinese medicine |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1363311A (en) * | 2001-01-10 | 2002-08-14 | 杨孟君 | Nano medicine 'Kaixiong Shunqi' and its preparing process |
| CN101181572A (en) * | 2007-11-19 | 2008-05-21 | 上海复星临西药业有限公司 | Method for preparing kaixiong shunqi wan |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1363311A (en) * | 2001-01-10 | 2002-08-14 | 杨孟君 | Nano medicine 'Kaixiong Shunqi' and its preparing process |
| CN101181572A (en) * | 2007-11-19 | 2008-05-21 | 上海复星临西药业有限公司 | Method for preparing kaixiong shunqi wan |
Non-Patent Citations (4)
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| ***等.槟榔活性成分及其功能作用的研究进展.《中国食物与营养》.2008,(第06期),第50-53页. * |
| 徐韧柳等.开胸顺气丸(大蜜丸)质量标准研究.《中国实验方剂学杂志》.2005,第11卷(第02期),第24-27页. * |
| 董学等.中药三棱的化学成分及药理研究进展.《齐鲁药事》.2005,第24卷(第10期),第612-614页. * |
| 高家鉴等.开胸顺气胶囊制备工艺研究.《中国中药杂志》.1999,第24卷(第11期),第668-670页. * |
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