CN1923263A - Traditional Chinese medicine composition, its preparing method and quality controlling means - Google Patents
Traditional Chinese medicine composition, its preparing method and quality controlling means Download PDFInfo
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Abstract
The invention discloses a medicinal composition, which is prepared from poria cocos, peach kernels, fragrant solomonseal rhizome, schisandra fruit, corktree bark, ledebouriella root, notopterygium root, tetrandra root, Clematis chinensis, excrementum bombycis, rhizoma dioscoreae hypoglaueae, Japanese yam, cassia twig, Chinese angelica root, safflower, ginseng, orienavine, levisticum through conventional preparing process. The composition can be prepared into dosage forms of tablets, capsules, granules and pills. The The invention also discloses the method for preparing the medicinal composition and its quality control method.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition, especially a kind of Chinese medicine composition that is used for the treatment of rheumatic arthritis and rheumatoid arthritis belongs to the field of Chinese medicines; The preparation method and the method for quality control that also relate to this medicine simultaneously.
Background technology
Rheumatic arthritis is the modal a kind of clinical manifestation of rheumatic fever, and is relevant with the allergy that A group hemolytic streptococcal infection causes.The morbidity of this disease is more anxious, and the joint of getting involved is based on big joint, begins to invade and the joint of the lower extremity person accounts for 85%, and knee joint and ankle joint are the most common, secondly be that shoulder, elbow and wrist, hands and sufficient little joint are rare.Arthropathy is multiple and migration, and the local joint inflammation is obvious, that performance has is red, swollen, hot, bitterly, tenderness and limitation of activity.In arthritis patients during acute stage can occur together heat, pharyngalgia, nervous, erythrocyte sedimentation rate speeds and the C-reactive protein such as increases at performance.Rheumatic arthritis patient is during acute pain, because long-term bed, perhaps take hormone overlong time etc., it is low to cause patient's body's immunity, some complication appear, comprise pneumonia, urinary system infection, hypercortisolism, oral ulcer etc., and, also be more vulnerable to infection than the normal person for epidemic infectious diseases.For this sick cause, academia does not still have final conclusion, does not have way in full force and effect in treatment yet, and based on chemical medicine treatment, effect is not satisfactory at present.
Rheumatoid arthritis is a kind of systemic autoimmune disease of the non-infectious inflammation based on joint and joint surrounding tissue, its pathological characteristic is the chronic inflammatory disease of synovium of joint, cellular infiltration, and the synovial membrane nebula forms, the invasion and attack of cartilage and osseous tissue, the destruction that causes articulation structure.Final joint deformity, dysfunction or forfeiture, in addition maimed, the forfeiture viability.Primary disease disability rate height has become one of universally acknowledged refractory disease, and modern medicine does not still have specific short to it.
In recent years, Chinese medicine has been obtained certain progress in the research of treatment rheumatic and rheumatoid arthritis, and the inventor is in conjunction with oneself clinical experience for many years, formulated we, and made Chinese patent medicine, through clinical verification through modern pharmaceutical technology, expelling wind and removing dampness, the channels sootheing and network vessel quickening relieving pain.
The object of the invention is intended to overcome the deficiency of existing treatment means and medicine, and a kind of Chinese medicine composition of effectively controlling inflammation is provided; The object of the invention also is to provide the preparation method and the method for quality control of this Chinese medicine composition.
Summary of the invention
The present invention seeks to be achieved through the following technical solutions:
Medicine of the present invention is to be made by the crude drug of following component:
150～250 parts of Rhizoma Smilacis Glabraes, 10～20 parts in Semen Persicae, 10～20 parts of Rhizoma Polygonati Odorati, 10～20 parts of Fructus Schisandrae Chinensis, 10～20 parts of Cortex Phellodendris, 10～20 parts of Radix Saposhnikoviaes, 10～20 parts of Rhizoma Et Radix Notopterygiis, 10～20 parts of Radixs Stephaniae Tetrandrae, 10～20 parts of Radix Clematidis, 10～20 parts of silkworm excrements, 10～20 parts of Dioscorea septemloba Thunb. , 10～20 parts of Rhizoma Dioscoreae Nipponicae, 10～20 parts of Ramulus Cinnamomi, 10～30 parts of Radix Angelicae Sinensis, 5～15 parts on Flos Carthami, 10～20 parts of Radix Ginsengs, 10～20 parts of Caulis Sinomeniis, 10～20 parts of Radix Angelicae Pubescentiss.
Crude drug ratio after preferred is:
180～220 parts of Rhizoma Smilacis Glabraes, 12～18 parts in Semen Persicae, 12～18 parts of Rhizoma Polygonati Odorati, 12～18 parts of Fructus Schisandrae Chinensis, 12～18 parts of Cortex Phellodendris, 12～18 parts of Radix Saposhnikoviaes, 12～18 parts of Rhizoma Et Radix Notopterygiis, 12～18 parts of Radixs Stephaniae Tetrandrae, 12～18 parts of Radix Clematidis, 12～18 parts of silkworm excrements, 12～18 parts of Dioscorea septemloba Thunb. , 12～18 parts of Rhizoma Dioscoreae Nipponicae, 12～18 parts of Ramulus Cinnamomi, 15～25 parts of Radix Angelicae Sinensis, 8～12 parts on Flos Carthami, 12～18 parts of Radix Ginsengs, 12～18 parts of Caulis Sinomeniis, 12～18 parts of Radix Angelicae Pubescentiss.
Through test further preferred after, optimal proportion is really:
200 parts of Rhizoma Smilacis Glabraes, 15 parts in Semen Persicae, 15 parts of Rhizoma Polygonati Odorati, 15 parts of Fructus Schisandrae Chinensis, 15 parts of Cortex Phellodendris, 15 parts of Radix Saposhnikoviaes, 15 parts of Rhizoma Et Radix Notopterygiis, 15 parts of Radixs Stephaniae Tetrandrae, 15 parts of Radix Clematidis, 15 parts of silkworm excrements, 15 parts of Dioscorea septemloba Thunb. , 15 parts of Rhizoma Dioscoreae Nipponicae, 15 parts of Ramulus Cinnamomi, 20 parts of Radix Angelicae Sinensis, 10 parts on Flos Carthami, 15 parts of Radix Ginsengs, 15 parts of Caulis Sinomeniis, 15 parts of Radix Angelicae Pubescentiss.
Clinical use for convenience, the inventor has done further research at this crude drug, to formulate its extraction and preparation technique, is made into various dosage forms clinical or that pharmacy is required, as granule, tablet, capsule, soft capsule, pill etc.Research process is as follows:
1, ginseng crude drug's disintegrating process is investigated:
(1) grinding particle size is investigated and to be got ginseng crude drug 100g, respectively gets three parts, and pulverize separately is crossed 80 mesh sieves, 100 mesh sieves, 120 mesh sieves, investigate each powder character and the powder rate.The results are shown in following table.
Ginseng crude drug's grinding particle size is investigated
| Pulverize the order number | Characters powder | Get powder rate (%) |
| 80 orders | Powder is thicker, and fine particle is arranged | 98.6％ |
| 100 orders | Powder is thinner | 96.8％ |
| 120 orders | Powder is thinner | 91.5％ |
According to above-mentioned result of the test, when Radix Ginseng was pulverized 100 mesh sieves, pulverulence was better, and granularity is little, is easy to molding, and it is higher to pulverize yield, so this product is determined the Radix Ginseng powder is broken into 100 order fine powders.
(2) the investigation Radix Ginseng of sterilizing methods directly is used as medicine after pulverizing, and is up to specification for the microbial limit that guarantees finished product, needs it is carried out sterilization treatment.Through overtesting, cobalt 60 sterilizations and steam sterilization all have satisfied effect.
2, the volatile oil extraction process is preferred
The inventor thinks that the main medicinal ingredient in Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, the Radix Angelicae Sinensis is volatile oil, thereby the inventor studies in great detail the extracting parameter of volatile oil, focuses on extraction time.
Test method is got Radix Saposhnikoviae 100g, Rhizoma Et Radix Notopterygii 100g, Radix Angelicae Pubescentis 100g, Radix Angelicae Sinensis 134, gets three parts altogether, adds 5 times of water gagings respectively, flood after 1 hour, distillation extraction is 4 hours, 5 hours, 6 hours respectively, divides to get to slip out liquid, with Petroleum ether extraction three times, each 10ml merges petroleum ether liquid, filter with anhydrous sodium sulfate, and, merge petroleum ether liquid with petroleum ether 10ml washing, volatilize naturally, the weight that volatile oil decided in title the results are shown in following table.
Extract the volatile oil engineer testing
| Distill attached | 4 hours | 5 hours | 6 hours |
| Volatilization oil mass (g) | 0.6574 | 0.8269 | 0.8305 |
Result of the test shows that the volatilization oil mass of distilling 4 hours is less, and extraction ratio is lower, distilled 5 hours and the extraction effect of 6 hours volatile oil suitable, extraction ratio is all higher.For saving time, when extracting volatile oil, this product selects distillation extraction 5 hours.
3, water extraction process is investigated
Test method fetch earth Poria 200g, Semen Persicae 15g, Rhizoma Polygonati Odorati 15g, Fructus Schisandrae Chinensis 15g, Cortex Phellodendri 15g, Radix Stephaniae Tetrandrae 15g, Radix Clematidis 15g, silkworm excrement 15g, Dioscorea septemloba Thunb. 15g, Rhizoma Dioscoreae Nipponicae 15g, Ramulus Cinnamomi 15g, Flos Carthami 10g, Caulis Sinomenii 15g, respectively get three parts, adding 8 times of amounts, 10 times of amounts, 12 times of water gagings respectively extracts 3 times, be followed successively by 3,2,1 hours, filter, merging filtrate, standby.
Berberine hydrochloride in the selection selection Cortex Phellodendri of index composition carries out optimal process as testing index, and assay method is:
According to high effective liquid chromatography for measuring
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; The acetonitrile of 25: 75 ratios-0.1% phosphoric acid solution is a mobile phase, detects wavelength 265nm, flow velocity 1.0ml/min, and 25 ℃ of column temperatures, number of theoretical plate calculate by the berberine hydrochloride peak should be not less than 3000.
It is an amount of that the reference substance solution precision takes by weighing the berberine hydrochloride reference substance, adds the mutual-assistance dissolving of flowing, and makes the solution that every 1ml contains 5 μ g, promptly.
Need testing solution is got 1/1000 amount of extracting solution, water bath method, residue add the small amount of methanol dissolving, quantitatively are added on the neutral alumina post, with methanol 50ml eluting, collect eluent, evaporate to dryness, residue add the mobile phase dissolving and quantitatively are transferred in the 10ml measuring bottle, add mobile phase to scale, shake up, filter with microporous filter membrane, promptly.
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Result of the test is extracted by above process, and the content of above method mensuration berberine hydrochloride, calculates the content of amounting in total extracting solution, the results are shown in following table.
Water extraction process is investigated test
| Adding water doubly measures | 8 times of amounts | 10 times of amounts | 12 times of amounts |
| Berberine hydrochloride amount (mg) | 35.8 | 48.2 | 48.5 |
According to above result of the test, the extraction effect that adds 8 times of amounts of water is relatively poor, and 10 times in water is measured and the extraction effect of 12 times of amounts is all higher and add, and extraction ratio is suitable.Be energy savings, this product is determined to add 10 times of water gagings and is decocted 3 times, is followed successively by 3,2,1 hours.
4, concentration technology is investigated
According to producing practical situation, adopt normal pressure to concentrate and two kinds of methods of concentrating under reduced pressure when concentrating, but because the spissated temperature of normal pressure is higher, the time of recovery is longer, causes loss of active ingredients easily; The loss that the employing concentrating under reduced pressure then can reduce above factor as far as possible to be caused is so this preparation is selected concentrating under reduced pressure.Through overtesting, reach in vacuum-situation about 0.08MPa under, when temperature reached 65～70 ℃, recovery speed was very fast, effect is better.So this product determines to adopt concentrating under reduced pressure, 65～70 ℃ of temperature, vacuum-0.08MPa, relative density is 1.30～1.35 thick paste when being concentrated into 60 ℃.
5, drying process is preferred
Above concentrated solution, the Radix Ginseng fine powder of adding respective amount carries out the research of drying process.Drying process commonly used in industry has constant pressure and dry and drying under reduced pressure.This technology is to dry rerum natura shape, the drying time of different drying means gained comparing preferably more excellent drying means.Result of the test sees the following form.
Drying means preferred
| Drying means | Condition | State | Drying time |
| Constant pressure and dry | 70～80℃ | Color and luster is dark, and is harder | Time is longer |
| Drying under reduced pressure | 70～75℃，-0.08MPa | Color and luster is darker, and is loose | Time is shorter |
| Drying under reduced pressure | 65～70℃，-0.08MPa | Lighter color is loose | Time is shorter |
Above result of the test shows that the dry thing of constant pressure and dry is harder, and color and luster is dark; And the effect of drying under reduced pressure is better, and dry thing is all more loose, pulverizes easily; When drying under reduced pressure condition temperature is 65～70 ℃, vacuum is-and during the 0.08MPa left and right sides, the dry thing of gained is loose, and lighter color so this product is determined drying condition is: adopt drying under reduced pressure, control vacuum and reach-0.08MPa 65～70 ℃ of temperature.
The preparation method of tablet that the inventor is finally preferred: get Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, Radix Angelicae Sinensis extraction volatile oil, distillate is standby in addition; Radix Ginseng is pulverized, and crosses 100 mesh sieves, and is standby; 13 flavors such as Rhizoma Smilacis Glabrae add 10 times of water gagings respectively and decoct 3 times, are followed successively by 3,2,1 hours, filter, and merging filtrate and distillate, relative density is 1.30～1.35 thick paste when being evaporated to 60 ℃; Add the Radix Ginseng fine powder at thick paste, mixing, drying under reduced pressure, dry extract is pulverized, and crosses 100 mesh sieves, and add volatile oil and stir, and add starch and be adjusted to suitable dispersion in right amount, mixing, with 70% alcohol granulation, cold drying is pressed into tablet.
In the research technical process, and after making product, the inventor has also formulated the method for quality control of product, to guarantee the quality of this drug regimen.This method of quality control comprises assay and qualitative identification two parts, is described below respectively.
(1) assay:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 25: 75 acetonitrile-0.1% phosphoric acid is mobile phase, detects wavelength 265nm, flow velocity 1.0ml/min, and 25 ℃ of column temperatures, number of theoretical plate calculate by the berberine hydrochloride peak should be not less than 3000;
It is an amount of that the reference substance solution precision takes by weighing the berberine hydrochloride reference substance, adds the mutual-assistance dissolving of flowing, and makes the solution that every 1ml contains 5 μ g, promptly;
Need testing solution is got drug combination preparation 5～15g of the present invention, and porphyrize takes by weighing 1g, and accurate the title decides, precision adds methanol 50ml, claims to decide weight, supersound process 30 minutes, room temperature to be chilled to, claim to decide weight, supply the weight that subtracts mistake with methanol, filter, precision is measured subsequent filtrate 10ml, quantitatively be added on the neutral alumina post,, collect eluent with methanol 50ml eluting, evaporate to dryness, residue add the mobile phase dissolving and quantitatively are transferred in the 25ml measuring bottle, add mobile phase to scale, shake up, filter with microporous filter membrane, promptly;
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
(2) qualitative identification:
1) get preparation 3～10g of the present invention, porphyrize adds methanol eddy and extracted 1 hour, put coldly, filter the filtrate evaporate to dryness, residue adds the 0.05mol/L sodium hydroxide solution makes dissolving, puts in the separatory funnel, with the chloroform extraction secondary, discard chloroform solution, water liquid adds water-saturated n-butanol and extracts secondary, merges n-butyl alcohol liquid, wash with the n-butyl alcohol saturation water, n-butyl alcohol liquid evaporate to dryness, residue adds methanol makes dissolving, as need testing solution; Other gets Radix Ginseng control medicinal material 1g, shines medical material solution in pairs with legal system; Also can get ginsenoside Re, Rg1 reference substance again, add methanol and make the mixed solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds or three kinds of each 2 μ l of solution, put respectively on same silica gel g thin-layer plate, with 15: 40: 22: chloroform-ethyl acetate of 10-methanol-water mixture was developing solvent at lower floor's solution of placing below 10 ℃, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings several minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of four same colors at least; Or with the corresponding position of reference substance chromatograph on, show identical aubergine speckle;
2) get preparation 3～10g of the present invention, porphyrize added the methanol supersound process 30 minutes, filtered, filtrate evaporate to dryness, residue add water makes dissolving, adds strong aqua ammonia and regulates pH9～10, with chloroform extraction three times, combined chloroform liquid, water bath method, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.5g, shines medical material solution in pairs with legal system; Also can get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution, control medicinal material solution and/or reference substance solution, put respectively on same silica gel g thin-layer plate, with 6: 3: 1.5: the mixed liquor of toluene-ethyl acetate-methanol of 1.5: 0.5-isopropyl alcohol-strong ammonia solution was developing solvent, put interior expansion of expansion cylinder of ammonia saturated with vapor, took out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material, the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle;
3) get the sinomenine reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw the need testing solution under reference substance solution and " differentiate 2) ", put respectively on same silica gel g thin-layer plate, with 2: 4: 2: the upper solution of the mixed liquor of toluene-ethyl acetate-methanol-water of 1 after placing below 10 ℃ was developing solvent, put interior expansion of expansion cylinder of ammonia saturated with vapor, take out, dry, spray successively with bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical punctation.
Prove that through the inventor above method of quality control can be applied to the various dosage forms that technical solution of the present invention can be made.
For rheumatic and rheumatoid arthritis the obvious treatment effect be arranged by the invention pharmaceutical composition, the result with clinical experiment illustrates beneficial effect of the present invention below: (used in the experiment " the numbness sheet relaxes " is the tablet of making by optimum prescription of the present invention and technology)
One, easypro numbness sheet is for the therapeutical effect of rheumatic arthritis
1, data and method
1.1 physical data is observed 40 examples altogether, male 26 examples, women 14 examples, 18～50 years old age, average 27.58 ± 4.25 years old, the course of disease 2 months～5 years, average 1.2 ± 0.5 years.
1.2 diagnostic criteria diagnosis basis ACC up-to-date revision Jones standard in 1992.Chinese medical discrimination and diagnostic criteria are with reference to " the clinical research guideline of new Chinese medicine treatment numbness disease ".
1.3 Therapeutic Method is taken the numbness sheet that relaxes, each 3, every day 3 times, one after each meal, 3 months courses of treatment.
1.4 observation index cardinal symptom, sign (arthralgia, joint function disturbance, arthroncus, both hands grip, 15 meters are apart from travel time), its grade scale is with reference to Ministry of Health of the People's Republic of China " treatment rheumatism medicine research guideline Clinical Researches of New Drugs guideline (1993) ", index calculation method is: remember 0 fen for 0 grade, counted 1 fen for 1 grade, counted 2 fens for 2 grades, remember 3 fens for 3 grades, counted 4 fens for 4 grades that its index is all joints score sums.Physical and chemical index (ESR, ASQ, IgG, IgM).
1.5 curative effect determinate standard is with reference to " the clinical research guideline of new Chinese medicine treatment numbness disease ", clinical cure: symptom all disappears, and functional activity is normal, and main physical and chemical index is normal.Produce effects: symptomatology disappears or cardinal symptom is eliminated, and joint function recovery can be participated in operate as normal and work, and physical and chemical index is normal substantially.Effectively: cardinal symptom is eliminated substantially, and main function of joint is recovered substantially, and can't take care of oneself to transfer to can take care of oneself, and perhaps loses the job and work capacity transfers the work or physical labor ability to and recovers to some extent, and main physical and chemical index improves.Invalid: and compare before the treatment, each side does not all have progress.
1.6 all measurement datas of statistical procedures are all represented enumeration data X with mean ± standard deviation
2Check, P＜0.01 has statistical significance.
2 results
2.1 changing, cardinal symptom, sign see Table 1
2.2 improving, blood biochemistry index sees Table 2.
Symptom, sign change relatively before and after the table 1 rheumatic arthritis patient
| Group | The arthralgia index | The dysfunction index | Joint swelling index | Both hands grip (mmHg) | 15 meters apart from travel time (s) |
| Before the treatment | 21.25±6.52 | 2.36±0.41 | 2.73±0.52 | 91.87±9.27 | 51.36±3.42 |
| After the treatment | 6.67±0.87 | 0.75±0.22 | 0.6±0.32 | 190.67±15.46 | 16.08±3.71 |
The improvement of table 2 blood index
| Group | ESR (min/h) | ASO (IU/L) | IgG (g/L) | IgA (mg/L) |
| Before the treatment | 47.53±3.5 | 402.36±128.76 | 22.19±4.45 | 3918±1296 |
| After the treatment | 16.4±5.7 | 236.41±69.57 | 12.67±3.3 | 1564±1232 |
2.3 efficacy determination clinical cure 15 examples (37.5%), produce effects 19 examples (47.5%), effective 6 examples (15%), invalid 0 example, total effective rate 100%.
Two, easypro numbness sheet is for the therapeutical effect of rheumatoid arthritis
1 physical data
Observe 60 cases altogether, wherein male 33 examples, women 27 examples; At 18～60 years old age, the course of disease did not wait in 2 months～10 years.All patient's clinical manifestation, iconography, lab testing etc. all meet U.S. ARA, the diagnostic criteria of the 5th ARR meeting revision June in 1987.
2 Therapeutic Method: take the numbness sheet that relaxes, each 4, every day 3 times, one after each meal, 3 months courses of treatment.
3 results
3.1 curative effect determinate standard
Produce effects: the arthralgia of getting involved disappears, and function of joint is recovered normally substantially, and it is normal that ESR recovers.Effectively: the arthralgia of getting involved is clearly better, and function of joint is partly improved, and the RF titre reduces, and ESR is slack-off, but does not reach normal value.Invalid: sings and symptoms does not have change substantially.
Carry out therapeutic evaluation after six months 3.2 therapeutic outcome is taken: produce effects 35 examples account for 58.3%; Effective 21 examples account for 35%; Invalid 4 examples account for 6.7%.Total effective rate is 93.3%.
Describe technical scheme of the present invention by the following examples in detail:
Embodiment 1:
Prescription: Rhizoma Smilacis Glabrae 200g Semen Persicae 15g Rhizoma Polygonati Odorati 15g
Fructus Schisandrae Chinensis 15g Cortex Phellodendri 15g Radix Saposhnikoviae 15g
Rhizoma Et Radix Notopterygii 15g Radix Stephaniae Tetrandrae 15g Radix Clematidis 15g
Silkworm excrement 15g Dioscorea septemloba Thunb. 15g Rhizoma Dioscoreae Nipponicae 15g
Ramulus Cinnamomi 15g Radix Angelicae Sinensis 20g flower 10g
Radix Ginseng 15g Caulis Sinomenii 15g Radix Angelicae Pubescentis 15g
Method for making: above 18 flavors, it is standby that Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, Radix Angelicae Sinensis are extracted volatile oil, it is standby that the Radix Ginseng powder is broken into fine powder, four flavors such as Radix Saposhnikoviae behind 13 flavors such as Rhizoma Smilacis Glabrae and the extraction volatile oil add 15 times of water gagings and decoct 3 times (3,2,1 hours), gradation filters, and merging filtrate is concentrated into the thick paste shape, adding Radix Ginseng fine powder, volatile oil stir, and add dextrin 300g again and make granule.
Instructions of taking: each 5g, three times on the one.
Embodiment 2:
Prescription: Rhizoma Smilacis Glabrae 500g Semen Persicae 40g Rhizoma Polygonati Odorati 20g
Fructus Schisandrae Chinensis 40g Cortex Phellodendri 20g Radix Saposhnikoviae 30g
Rhizoma Et Radix Notopterygii 20g Radix Stephaniae Tetrandrae 40g Radix Clematidis 40g
Silkworm excrement 30g Dioscorea septemloba Thunb. 20g Rhizoma Dioscoreae Nipponicae 40g
Ramulus Cinnamomi 25g Radix Angelicae Sinensis 60g Flos Carthami 20g
Radix Ginseng 40g Caulis Sinomenii 20g Radix Angelicae Pubescentis 40g
Method for making: 1. above 18 flavors, Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, Radix Angelicae Sinensis extract volatile oil, and distillate is standby in addition;
2. Radix Ginseng is pulverized, and crosses 100 mesh sieves, and is standby;
3. 13 flavors such as Rhizoma Smilacis Glabrae add 10 times of water gagings respectively and decoct 3 times, are followed successively by 3,2,1 hours, filter, and merging filtrate and distillate, concentrating under reduced pressure (65～70 ℃ ,-0.08MPa) to relative density the thick paste of 1.30～1.35 (60 ℃);
4. the thick paste in 3 is added the Radix Ginseng fine powder, mixing, drying under reduced pressure (65～70 ℃ ,-0.08MPa), dry extract is pulverized, cross 100 mesh sieves, add volatile oil and stir, and add starch to total amount 300g, mixing, with 70% alcohol granulation, cold drying is pressed into 1000, promptly.
Instructions of taking: each 3～4, three times on the one.
Embodiment 3:
Prescription: Rhizoma Smilacis Glabrae 300g Semen Persicae 20g Rhizoma Polygonati Odorati 40g
Fructus Schisandrae Chinensis 20g Cortex Phellodendri 40g Radix Saposhnikoviae 40g
Rhizoma Et Radix Notopterygii 40g Radix Stephaniae Tetrandrae 20g Radix Clematidis 20g
Silkworm excrement 20g Dioscorea septemloba Thunb. 40g Rhizoma Dioscoreae Nipponicae 20g
Ramulus Cinnamomi 20g Radix Angelicae Sinensis 20g Flos Carthami 40g
Radix Ginseng 20g Caulis Sinomenii 40g Radix Angelicae Pubescentis 20g
Method for making: above 18 flavors, Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, Radix Angelicae Sinensis extract volatile oil, and distillate is standby in addition; It is standby that the Radix Ginseng powder is broken into fine powder; 13 flavors such as Rhizoma Smilacis Glabrae add 10 times of water gagings respectively and decoct 3 times, be followed successively by 3,2,1 hours, and filtered merging filtrate and distillate, being evaporated to relative density is the thick paste of 1.30～1.35 (60 ℃), add Radix Ginseng fine powder mixing, drying under reduced pressure, dry extract is pulverized, adding volatile oil stirs, make granule, load 1000 of capsules, promptly.
Character: this product is a capsule, and content is the granule of brown or pitchy; Mildly bitter flavor.
Instructions of taking: each 4, every day secondary.
Differentiate: (1) gets this product content 4g, and porphyrize adds methanol 25ml, reflux, extract, 1 hour, put coldly, filter the filtrate evaporate to dryness, residue adds 0.05mol/L sodium hydroxide solution 20ml makes dissolving, puts in the separatory funnel, with the chloroform extraction secondary, each 20ml discards chloroform solution, and water liquid adds water-saturated n-butanol and extracts secondary, each 15ml merges n-butyl alcohol liquid, washs with n-butyl alcohol saturation water 30ml, n-butyl alcohol liquid evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Radix Ginseng control medicinal material 1g, shines medical material solution in pairs with legal system.Get ginsenoside Re, Rg1 reference substance again, add methanol and make the mixed solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, (15: 40: 22: 10) lower floor's solution of placing below 10 ℃ was developing solvent with chloroform-ethyl acetate-methanol-water, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings several minutes.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of four same colors at least; With the corresponding position of reference substance chromatograph on, show identical aubergine speckle.
(2) get this product content 6g, porphyrize adds methanol 30ml, supersound process 30 minutes filters the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, add strong aqua ammonia and regulate pH9～10, with chloroform extraction three times, each 15ml, combined chloroform liquid, water bath method, residue add methanol 1ml makes dissolving, as need testing solution.Other gets Cortex Phellodendri control medicinal material 0.5g, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw need testing solution 4 μ l, control medicinal material solution, each 1 μ l of reference substance solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution (6: 3: 1.5: 1.5: 0.5) is developing solvent, puts interior expansion of expansion cylinder of ammonia saturated with vapor, takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material, the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle.
(3) get the sinomenine reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw each the 5 μ l of need testing solution under reference substance solution and " differentiating (2) " item, respectively on the same silica gel g thin-layer plate of idea, (2: 4: 2: 1) upper solution of placing below 10 ℃ was developing solvent with toluene-ethyl acetate-methanol-water, put interior expansion of expansion cylinder of ammonia saturated with vapor, take out, dry, spray successively with bismuth potassium iodide test solution and sodium nitrite ethanol test solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical punctation.
Assay: according to high effective liquid chromatography for measuring.
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-0.1% phosphoric acid (25: 75) is mobile phase, detects wavelength 265nm, flow velocity 1.0ml/min, and 25 ℃ of column temperatures, number of theoretical plate calculate by the berberine hydrochloride peak should be not less than 3000.
It is an amount of that the reference substance solution precision takes by weighing the berberine hydrochloride reference substance, adds the mutual-assistance dissolving of flowing, and makes the solution that every 1ml contains 5 μ g, promptly.
Need testing solution is got this product content under the content uniformity item, and porphyrize takes by weighing 1g, the accurate title, decide, and precision adds methanol 50ml, claims to decide weight, supersound process (power 250W, frequency 50kHz) 30 minutes, room temperature to be chilled to, claim to decide weight, supply the weight that subtracts mistake, filter with methanol, precision is measured subsequent filtrate 10ml, quantitatively be added in the neutral alumina post (120～200 orders, 3g is on the internal diameter 1～1.5cm), with methanol 50ml eluting, collect eluent, evaporate to dryness, residue add the mobile phase dissolving and quantitatively are transferred in the 25ml measuring bottle, add mobile phase to scale, shake up, filter with microporous filter membrane (0.45 μ m), promptly.
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Cortex Phellodendri with berberine hydrochloride (C
20H
18ClNO
4HCl) meter must not be less than 0.12mg.
Claims (9)
1. pharmaceutical composition, it is characterized in that it is to be made by the crude drug of following part by weight: 150～250 parts of Rhizoma Smilacis Glabraes, 10～20 parts in Semen Persicae, 10～20 parts of Rhizoma Polygonati Odorati, 10～20 parts of Fructus Schisandrae Chinensis, 10～20 parts of Cortex Phellodendris, 10～20 parts of Radix Saposhnikoviaes, 10～20 parts of Rhizoma Et Radix Notopterygiis, 10～20 parts of Radixs Stephaniae Tetrandrae, 10～20 parts of Radix Clematidis, 10～20 parts of silkworm excrements, 10～20 parts of Dioscorea septemloba Thunb. , 10～20 parts of Rhizoma Dioscoreae Nipponicae, 10～20 parts of Ramulus Cinnamomi, 10～30 parts of Radix Angelicae Sinensis, 5～15 parts on Flos Carthami, 10～20 parts of Radix Ginsengs, 10～20 parts of Caulis Sinomeniis, 10～20 parts of Radix Angelicae Pubescentiss.
2. pharmaceutical composition according to claim 1, the preferred weight proportioning that it is characterized in that each crude drug is: 180～220 parts of Rhizoma Smilacis Glabraes, 12～18 parts in Semen Persicae, 12～18 parts of Rhizoma Polygonati Odorati, 12～18 parts of Fructus Schisandrae Chinensis, 12～18 parts of Cortex Phellodendris, 12～18 parts of Radix Saposhnikoviaes, 12～18 parts of Rhizoma Et Radix Notopterygiis, 12～18 parts of Radixs Stephaniae Tetrandrae, 12～18 parts of Radix Clematidis, 12～18 parts of silkworm excrements, 12～18 parts of Dioscorea septemloba Thunb. , 12～18 parts of Rhizoma Dioscoreae Nipponicae, 12～18 parts of Ramulus Cinnamomi, 15～25 parts of Radix Angelicae Sinensis, 8～12 parts on Flos Carthami, 12～18 parts of Radix Ginsengs, 12～18 parts of Caulis Sinomeniis, 12～18 parts of Radix Angelicae Pubescentiss.
3. pharmaceutical composition according to claim 2 is characterized in that the optimum weight proportioning of each crude drug is: 200 parts of Rhizoma Smilacis Glabraes, 15 parts in Semen Persicae, 15 parts of Rhizoma Polygonati Odorati, 15 parts of Fructus Schisandrae Chinensis, 15 parts of Cortex Phellodendris, 15 parts of Radix Saposhnikoviaes, 15 parts of Rhizoma Et Radix Notopterygiis, 15 parts of Radixs Stephaniae Tetrandrae, 15 parts of Radix Clematidis, 15 parts of silkworm excrements, 15 parts of Dioscorea septemloba Thunb. , 15 parts of Rhizoma Dioscoreae Nipponicae, 15 parts of Ramulus Cinnamomi, 20 parts of Radix Angelicae Sinensis, 10 parts on Flos Carthami, 15 parts of Radix Ginsengs, 15 parts of Caulis Sinomeniis, 15 parts of Radix Angelicae Pubescentiss.
4. according to the pharmaceutical composition described in the claim 1,2 or 3, it is characterized in that said composition can be made into clinically or pharmaceutically acceptable various dosage form, comprise granule, tablet, capsule, soft capsule, pill etc.
5. according to the described preparation of drug combination method of claim 4, it is characterized in that this method comprises following technical process: it is standby that Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, Radix Angelicae Sinensis are extracted volatile oil, it is standby that the Radix Ginseng powder is broken into fine powder, four flavors such as Radix Saposhnikoviae behind 13 flavors such as Rhizoma Smilacis Glabrae and the extraction volatile oil decoct with water 3 times, gradation filters, and merging filtrate is concentrated into the thick paste shape, add Radix Ginseng fine powder and volatile oil and stir, get medicated powder; Add proper auxiliary materials again, make required dosage form, promptly.
6. as preparation of drug combination method as described in the claim 5, it is characterized in that the preparation method of tablet is as follows: get Radix Saposhnikoviae, Rhizoma Et Radix Notopterygii, Radix Angelicae Pubescentis, Radix Angelicae Sinensis and extract volatile oil, distillate is standby in addition; Radix Ginseng is pulverized, and crosses 100 mesh sieves, and is standby; 13 flavors such as Rhizoma Smilacis Glabrae add 10 times of water gagings respectively and decoct 3 times, are followed successively by 3,2,1 hours, filter, and merging filtrate and distillate, relative density is 1.30～1.35 thick paste when being evaporated to 60 ℃; Add the Radix Ginseng fine powder at thick paste, mixing, drying under reduced pressure, dry extract is pulverized, and crosses 100 mesh sieves, and add volatile oil and stir, and add starch and be adjusted to suitable dispersion in right amount, mixing, with 70% alcohol granulation, cold drying is pressed into tablet.
7. according to the method for quality control of the described pharmaceutical composition of claim 4, comprise assay and qualitative identification two parts, it is characterized in that content assaying method wherein is as follows:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 25: 75 acetonitrile-0.1% phosphoric acid is mobile phase, detects wavelength 265nm, flow velocity 1.0ml/min, and 25 ℃ of column temperatures, number of theoretical plate calculate by the berberine hydrochloride peak should be not less than 3000;
It is an amount of that the reference substance solution precision takes by weighing the berberine hydrochloride reference substance, adds the mutual-assistance dissolving of flowing, and makes the solution that every 1ml contains 5 μ g, promptly;
Need testing solution is got drug combination preparation 5～15g of the present invention, and porphyrize takes by weighing 1g, the accurate title, decide, precision adds methanol 50ml, claims to decide weight, supersound process 30 minutes, room temperature to be chilled to, claim to decide weight, supply the weight that subtracts mistake, filter with methanol, precision is measured subsequent filtrate 10ml, quantitatively be added on the neutral alumina post,, collect eluent with methanol 50ml eluting, evaporate to dryness, residue adds the mobile phase dissolving and quantitatively is transferred in the 25ml measuring bottle, adds mobile phase to scale, shakes up, filter with microporous filter membrane, promptly;
Accurate reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
8. according to the method for quality control of the described pharmaceutical composition of claim 7, it is characterized in that wherein qualitative identification method can be following one or more:
1) get preparation 3～10g of the present invention, porphyrize adds methanol eddy and extracted 1 hour, put coldly, filter the filtrate evaporate to dryness, residue adds the 0.05mol/L sodium hydroxide solution makes dissolving, puts in the separatory funnel, with the chloroform extraction secondary, discard chloroform solution, water liquid adds water-saturated n-butanol and extracts secondary, merges n-butyl alcohol liquid, wash with the n-butyl alcohol saturation water, n-butyl alcohol liquid evaporate to dryness, residue adds methanol makes dissolving, as need testing solution; Other gets Radix Ginseng control medicinal material 1g, shines medical material solution in pairs with legal system; Also can get ginsenoside Re, Rg1 reference substance again, add methanol and make the mixed solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography, draw above-mentioned two kinds or three kinds of each 2 μ l of solution, put respectively on same silica gel g thin-layer plate, with 15: 40: 22: chloroform-ethyl acetate of 10-methanol-water mixture was developing solvent at lower floor's solution of placing below 10 ℃, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings several minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of four same colors at least; Or with the corresponding position of reference substance chromatograph on, show identical aubergine speckle;
2) get preparation 3～10g of the present invention, porphyrize added the methanol supersound process 30 minutes, filtered, filtrate evaporate to dryness, residue add water makes dissolving, adds strong aqua ammonia and regulates pH9～10, with chloroform extraction three times, combined chloroform liquid, water bath method, residue add methanol 1ml makes dissolving, as need testing solution; Other gets Cortex Phellodendri control medicinal material 0.5g, shines medical material solution in pairs with legal system; Also can get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw need testing solution, control medicinal material solution and/or reference substance solution, put respectively on same silica gel g thin-layer plate, with 6: 3: 1.5: the mixed liquor of toluene-ethyl acetate-methanol of 1.5: 0.5-isopropyl alcohol-strong ammonia solution was developing solvent, put interior expansion of expansion cylinder of ammonia saturated with vapor, took out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material, the corresponding position of reference substance chromatograph on, show identical yellow fluorescence speckle;
3) get the sinomenine reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw the need testing solution under reference substance solution and " differentiate 2) ", put respectively on same silica gel g thin-layer plate, with 2: 4: 2: the upper solution of the mixed liquor of toluene-ethyl acetate-methanol-water of 1 after placing below 10 ℃ was developing solvent, put interior expansion of expansion cylinder of ammonia saturated with vapor, take out, dry, spray successively with bismuth potassium iodide test solution and sodium nitrite ethanol test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical punctation.
9. be used for the treatment of application in the medicine of rheumatic arthritis and rheumatoid arthritis according to claim 1,2 or 3 described pharmaceutical compositions in preparation.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430077A (en) * | 2011-11-29 | 2012-05-02 | 尹涓 | A Chinese medicinal composition for treating rheumatic arthritis and rheumatoid arthritis, and its preparation method |
| CN102886002A (en) * | 2012-10-31 | 2013-01-23 | 天津集合科技有限公司 | Traditional Chinese medicine composition for treating coxitis of dairy cattle and treatment method |
| CN109030701A (en) * | 2018-08-20 | 2018-12-18 | 四川新绿色药业科技发展有限公司 | A kind of thin-layer identification method for the control of root of fangji medicinal material, medicine materical crude slice and granule quality |
| CN110297046A (en) * | 2019-07-01 | 2019-10-01 | 中国药科大学 | Baseline etc. is than method joint mathematical model screening medicine to the method for active constituent and its ratio optimization |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101444616B (en) * | 2008-11-13 | 2013-04-17 | 徐玲 | Medicated wine for curing chronic rheumatism and method for preparing same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430077A (en) * | 2011-11-29 | 2012-05-02 | 尹涓 | A Chinese medicinal composition for treating rheumatic arthritis and rheumatoid arthritis, and its preparation method |
| CN102886002A (en) * | 2012-10-31 | 2013-01-23 | 天津集合科技有限公司 | Traditional Chinese medicine composition for treating coxitis of dairy cattle and treatment method |
| CN102886002B (en) * | 2012-10-31 | 2014-11-05 | 天津集合科技有限公司 | Traditional Chinese medicine composition for treating coxitis of dairy cattle and treatment method |
| CN109030701A (en) * | 2018-08-20 | 2018-12-18 | 四川新绿色药业科技发展有限公司 | A kind of thin-layer identification method for the control of root of fangji medicinal material, medicine materical crude slice and granule quality |
| CN110297046A (en) * | 2019-07-01 | 2019-10-01 | 中国药科大学 | Baseline etc. is than method joint mathematical model screening medicine to the method for active constituent and its ratio optimization |
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