CN101417020B - Medicine composition capable of eliminating the mass and relieving swelling, absorbing clots and alleviating pain, preparation method and quality control method thereof - Google Patents
Medicine composition capable of eliminating the mass and relieving swelling, absorbing clots and alleviating pain, preparation method and quality control method thereof Download PDFInfo
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Abstract
The invention discloses a pharmaceutical composition used for eliminating stagnation, reducing swelling, resolving blood stasis and relieving pain, and a preparation method and a quality control method thereof. The raw materials of the pharmaceutical composition consist of musk, semen momordicae (going through shelling and oil removal), prepared kusnezoff monkshood root, resin of sweetgum, frankincense (prepared), myrrh (prepared), excrementum pteropi (going through stir-heating with rice vinegar), angelica (going through stir-heating with liquor), earthworm and prepared ink. The preparation method comprises the steps: in the ten ingredients, except the artificial musk, other nine ingredients such as semen momordicae and the like are ground into fine powder; the artificial musk is porphyrized and matched with the fine powder; and the powder is sieved and directly prepared into clinically acceptable dose form by regular procedures or adding pharmaceutically acceptable inborn nature agents. The quality control method comprises the steps of carrying out microscopical identification to the medicine composition, carrying out thin-layer identification to the angelica, the frankincense and the earthworm, carrying out limit tests to aconitine in the kusnezoff monkshood root and carrying out content measurement to muscone in the musk. The pharmaceutical composition has very good effects of eliminating stagnation, reducing swelling, resolving blood stasis and relieving pain.
Description
Invention field
The present invention relates to a kind of Chinese medicine composition, particularly have mass dissipating and swelling eliminating, the Chinese medicine composition of effect of dissolving stasis and relieving pain relates to the preparation method and the method for quality control of said composition simultaneously, belongs to technical field of traditional Chinese medicines.
Background technology
Breast cancer is human modal a kind of malignant tumour, also is one of women's major malignant tumor.Estimate that according to American Cancer Society there is 120,000 breast cancer new cases every year in the U.S., the incidence of disease is that the number of dying from breast cancer in 72.2/10 ten thousand, 1976 is 33000.Breast cancer is different at the incidence of disease of China each department, though hanging down of China's genus women with breast cancer sent out a state in the world.But the incidence of disease of breast cancer obviously increases in recent years.Especially Shanghai, capital, Tianjin and coastland are the hotspots of China's breast cancer.The highest with Shanghai, the breast cancer incidence in Shanghai in 1972 be 20.1/10 ten thousand, 1988 be 28,/10 ten thousand then, occupy second in women's malignant tumour.
See from traditional Chinese medical science angle, be born in the women more.Because of depressed rage impairing the liver, worry impairing spleen, so that stagnation of the circulation of vital energy phlegm forms with fixed attention.Or dash wantonly two through lacking of proper care, qi stagnation hemagglutination and giving birth to.
Mostly adopting with the operation at present is main complex treatment.Radical excision breast cancer is still the main means of breast cancer treatment.But the modern medicine viewpoint thinks that it promptly is a systemic disease that the breast cancer idiopathy rises, and profile and the upper extremity function in order to preserve breast carried out multiple operation and integrated application radiotherapy, chemotherapy and drug therapy less than the full milk excision simultaneously.And mastectomy and radiotherapy, chemotherapy all have certain limitation, therefore, invent a kind of conscientiously, the medicine of efficacious therapy breast cancer is very necessary.
Summary of the invention
One object of the present invention is to disclose a kind of new have mass dissipating and swelling eliminating, the Chinese medicine composition of effect of dissolving stasis and relieving pain; Another object of the present invention is to disclose a kind of new have mass dissipating and swelling eliminating, the preparation method of effect of dissolving stasis and relieving pain Chinese medicine composition; The object of the invention also is to disclose a kind of method of quality control of new Chinese medicine composition.
Of the present invention have a mass dissipating and swelling eliminating, and the Chinese medicine composition of effect of dissolving stasis and relieving pain is to be processed by the bulk drug of following weight ratio:
Moschus 8-20 weight portion, semen momordicae (shell and deoil) 80-100 weight portion, wild aconite root 80-100 weight portion, motherwort 80-100 weight portion, frankincense (system) 30-50 weight portion, dandelion 30-50 weight portion, corydalis tuber 80-100 weight portion, Radix Angelicae Sinensis (wine stir-fry) 30-50 weight portion, earthworm 80-100 weight portion, scented ink 5-10 weight portion;
The above-mentioned raw materials optimum ratio is:
Moschus 10 weight portions, semen momordicae (shell and deoil) 90 weight portions, wild aconite root 90 weight portions, motherwort 90 weight portions, frankincense (system) 40 weight portions, dandelion 40 weight portions, corydalis tuber 90 weight portions, Radix Angelicae Sinensis (wine stir-fry) 40 weight portions, earthworm 90 weight portions, scented ink 8 weight portions;
Of the present invention have a mass dissipating and swelling eliminating, and the Chinese medicine composition of effect of dissolving stasis and relieving pain can be processed by the bulk drug of following weight ratio:
Moschus 8-20 weight portion, semen momordicae (shell and deoil) 80-100 weight portion, wild aconite root 80-100 weight portion, resina liquidamberis 80-100 weight portion, frankincense (system) 30-50 weight portion, myrrh (system) 30-50 weight portion, excrementum pteropi (vinegar stir-fry) 80-100 weight portion, Radix Angelicae Sinensis (wine stir-fry) 30-50 weight portion, earthworm 80-100 weight portion, scented ink 5-10 weight portion;
The above-mentioned raw materials optimum ratio is:
Moschus 10 weight portions, semen momordicae (shell and deoil) 90 weight portions, wild aconite root 90 weight portions, resina liquidamberis 90 weight portions, frankincense (system) 40 weight portions, myrrh (system) 40 weight portions, excrementum pteropi (vinegar stir-fry) 90 weight portions, Radix Angelicae Sinensis (wine stir-fry) 40 weight portions, earthworm 90 weight portions, scented ink 8 weight portions;
The above-mentioned raw materials optimum ratio can also for:
Moschus 12 weight portions, semen momordicae (shell and deoil) 88 weight portions, wild aconite root 88 weight portions, resina liquidamberis 40 weight portions, frankincense (system) 30 weight portions, myrrh (system) 37.5 weight portions, excrementum pteropi (vinegar stir-fry) 90 weight portions, Radix Angelicae Sinensis (wine stir-fry) 30 weight portions, earthworm 40 weight portions, scented ink 5 weight portions;
Composition of the present invention can add auxiliary material by common process and process clinical acceptable forms such as tablet, capsule, oral liquid, pill, spray, granule; Said auxiliary material comprises solvent, disintegrant, flavouring, antiseptic, colorant, bonding agent, lubricant, matrix etc.
The preparation method of Chinese medicine composition pill of the present invention is:
Choose bulk drug:
Moschus 8-20 weight portion, semen momordicae (shell and deoil) 80-100 weight portion, wild aconite root 80-100 weight portion, resina liquidamberis 80-100 weight portion, frankincense (system) 30-50 weight portion, myrrh (system) 30-50 weight portion, excrementum pteropi (vinegar stir-fry) 80-100 weight portion, Radix Angelicae Sinensis (wine stir-fry) 30-50 weight portion, earthworm 80-100 weight portion, scented ink 5-10 weight portion;
Method for making: above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get.
The preparation method of Chinese medicine composition pill of the present invention is:
Choose bulk drug: Moschus 8-20 weight portion, semen momordicae (shell and deoil) 80-100 weight portion, wild aconite root 80-100 weight portion, motherwort 80-100 weight portion, frankincense (system) 30-50 weight portion, dandelion 30-50 weight portion, corydalis tuber 80-100 weight portion, Radix Angelicae Sinensis (wine stir-fry) 30-50 weight portion, earthworm 80-100 weight portion, scented ink 5-10 weight portion;
Method for making: above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get.
Said parts by volume/weight portion is corresponding with ml/g.
The method of quality control of Chinese medicine composition of the present invention comprises discriminating and/or assay and/or inspection.Discrimination method comprises a kind of in the following method and/or several kinds:
(1) it is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, take by weighing to be equivalent to crude drug 3-4g, and the 10-30ml that adds diethyl ether, sonicated 10-30 minute, filter, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, with normal hexane-ethyl acetate (7-9: 1-3) be developping agent; Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(2) get frankincense control medicinal material 0.1g, the 1ml that adds diethyl ether flooded 1-3 hour, and supernatant is as control medicinal material solution.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each the 5 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate; With sherwood oil (60-90 ℃)-ethyl acetate (90-100: 0-10) be developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(3) it is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, takes by weighing to be equivalent to crude drug 3-4g, adds the ethanol 40-60ml of 60-80%; Placement is spent the night, and filters, and filtrating is steamed to there not being the ethanol flavor, adds water 10-30ml dissolving; With chloroform extraction 1-3 time, each 10-30ml merges methenyl choloride liquid; Evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution.Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H thin layer plate; With cyclohexane-ethyl acetate (8-10: 0-2) be developping agent, launch twice, take out; Dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Assay comprises following method:
Measure according to vapor-phase chromatography (2005 editions one appendix VI E of Chinese Pharmacopoeia).
Chromatographic condition and system suitability test are stationary phase with silicone (OV-17), and coating concentration is 5%; 190 ℃ of column temperatures, 220 ℃ of injector temperatures, 240 ℃ of detector temperatures are carrier gas with nitrogen.Number of theoretical plate calculates by the muskone peak should be not less than 1500.It is an amount of that correction factor mensuration is got NSC 77136, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as inner mark solution.It is an amount of that other gets the muskone reference substance, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as the reference substance storing solution.Above two kinds of each 2ml of solution of accurate absorption put in the measuring bottle of same 10ml, add cyclohexane and are diluted to scale, shake up, as reference substance solution.Draw reference substance solution 2 μ l, inject gas chromatograph, the calculation correction factor.
Assay method is got pharmaceutical preparation of the present invention, is ground into fine powder, gets powder and is equivalent to crude drug 0.5-1.5g, and accurate the title decides, mark liquid 2ml in accurate the adding; Cyclohexane 8ml, close plug, jolting, ultrasonic 20-40min filters; The accurate subsequent filtrate 2 μ l that draw, inject gas chromatograph calculates, and promptly gets.
Of the present invention pharmaceutical preparation suitable with the 0.77g crude drug contains the muscone with muskone (C
16H
30O) calculate, must not be less than 0.3mg.
Inspection comprises following method:
It is an amount of that aconitine limit is got pharmaceutical composition of the present invention, is ground into fine powder, takes by weighing to be equivalent to crude drug 7-8g, puts in the conical flask, adds ammonia solution 10ml; Mix thoroughly, placed 1-3 hour, add absolute ether 100-150ml, jolting 0.5-2 hour, placed 12-36 hour; Filter, filtrating adds hydrochloric acid solution (4 → 100) jolting extraction 3 times, and (15-25ml, 10-20ml 10-20ml), merge hydrochloric acid solution; Hydrochloric acid solution adds strong ammonia solution, transfers Ph value to 9～10, adds the absolute ether jolting and extracts 3 times, each 15-25ml; Merge ether solution, volatilize, residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets the aconitine reference substance, adds absolute ethyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw need testing solution 15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, with benzene-ethyl acetate-diethylamine (5-10: 1-3: 0.5-2) be developping agent; Presaturation launched after 2 hours; Take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of appearance should or spot not occur less than the spot of reference substance.
The present composition has good effect at mass dissipating and swelling eliminating on the blood-activating analgetic, said composition toxicity is very little, and clinical practice is safe and reliable.Warming channel and expelling cold, the channels-freeing dampness-dispelling of wild aconite root is monarch drug in a prescription in the side.Earthworm invigorate blood circulation dysmenorrhoea, semen momordicae vanishing sputum and dispelling knot, Radix Angelicae Sinensis, excrementum pteropi, frankincense, myrrh promoting blood circulation to remove blood stasis are ministerial drug altogether.Assistant is with resina liquidamberis, scented ink subdhing swelling and detoxicating, and the hot perfume (or spice) of Moschus is walked string, warming and activating meridian, the detoxifcation pain relieving.All medicines share, and play the effect of mass dissipating and swelling eliminating, blood-activating analgetic altogether.
Present composition preparation has stronger mass dissipating and swelling eliminating, effect of dissolving stasis and relieving pain, and can be through improving S
180The microcirculation of mouse ear, reduction mice with tumor WBV suppress tumor growth, the effect of unrestraint weight of mice.
Present composition preparation production technique is advanced, and method of quality control can carry out effective and stable control to the quality of product.Following experimental example is used to further specify the present invention.
The research of experimental example 1 technological experiment
1, smashing fineness test
Press recipe quantity configuration medicinal material; Every part contains Moschus 10g, semen momordicae (shell and deoil) 90g, wild aconite root 90g, resina liquidamberis 90g, frankincense (system) 40g, myrrh (system) 40g, excrementum pteropi (vinegar stir-fry) 90g, Radix Angelicae Sinensis (wine stir-fry) 40g, earthworm 90g, scented ink 8g; Divide four groups to do experiment respectively: smashing fineness is respectively: 50 orders, 65 orders, 80 orders, 100 orders are that index is confirmed smashing fineness with pill viscosity, pill outward appearance, pulverizing loss respectively.The result sees table 1:
Table 1: pulverize test findings
| The group number | 1 | 2 | 3 | 4 |
| Pulverize loss (%) | 4.47 | 5.12 | 5.94 | 8.18 |
| Pill viscosity | Normally | Normally | Normally | More sticking |
| The pill outward appearance | Coarse | More coarse | Bright and clean | Bright and clean |
Above result shows: when smashing fineness was 80 orders, each item index was better, so select 80 orders for use in producing.
2, starch amount of water test
Press the recipe quantity configuration; Get respective amount starch and divide four groups to experimentize, 2 times of amounts of first group of amount of water, 4 times of amounts of second group of amount of water; 6 times of amounts of the 3rd group of amount of water, 8 times of amounts of the 4th group of amount of water are that index is confirmed amount of water with pill viscosity, pill outward appearance, drying time respectively.The result sees table 2,
Table 2: amount of water test findings
| The group number | 1 | 2 | 3 | 4 |
| Drying time (h) | 10.5 | 10.8 | 11 | 11.8 |
| Pill viscosity | Loose | More diffusing | Normally | Sticking and inhomogeneous |
| The pill outward appearance | Be difficult for into ball | More coarse | Bright and clean | Bright and clean |
With pill viscosity, pill outward appearance is index, can find out that pill viscosity is better when adding 6 times of amounts of water, selects the 6 times of amounts of water that add in the production for use.
Table 3: three batches of pilot scale production datas
| Lot number | 05010701 | 05010802 | 05010903 |
| Pulverize inventory (kg) | 0.987 | 0.987 | 0.987 |
| Pulverize quantum of output (kg) | 0.972 | 0.971 | 0.973 |
| Moschus powder inventory (kg) | 0.03 | 0.03 | 0.03 |
| Moschus powder outlet quantity (g) | 0.029 | 0.029 | 0.029 |
| Starch inventory (kg) | 0.3 | 0.3 | 0.3 |
| Purified water addition (kg) | 0.3 | 0.3 | 0.3 |
| Wet ball weight (kg) | 1.533 | 1.534 | 1.532 |
| Dried ball weight (kg) | 1.231 | 1.233 | 1.231 |
| Finished product bottle number (120 ball/bottle) | 341 | 342 | 341 |
| Yield rate (%) | 99.7 | 99.9 | 99.7 |
Experimental example 2 discrimination method experimental studies
1. Radix Angelicae Sinensis discrimination test screening
(1) preparation of need testing solution
Method one: get pharmaceutical preparation of the present invention and be equivalent to crude drug 3.85g, porphyrize, the 20ml that adds diethyl ether, sonicated 10 minutes filters, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.
Method two: get pharmaceutical preparation of the present invention and be equivalent to crude drug 3.85g, porphyrize, the 20ml that adds diethyl ether, sonicated 20 minutes filters, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.
Method three: get pharmaceutical preparation of the present invention and be equivalent to crude drug 3.85g, porphyrize, the 20ml that adds diethyl ether, sonicated 30 minutes filters, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.
Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw each 5 μ l of above-mentioned three kinds of need testing solutions and control medicinal material solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-ethyl acetate (9: 1); Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
| The clear spot degree | The hangover situation | Disturbed condition | |
| Method one | Unintelligible | Do not have | Do not have |
| Method two: | Clear | Do not have | Do not have |
| Method three: | Clear | Do not have | Do not have |
(2) the developping agent proportioning is preferred:
Developping agent one: normal hexane-ethyl acetate (7: 3) is a developping agent
Developping agent two: normal hexane-ethyl acetate (8: 2) is a developping agent
Developping agent three: normal hexane-ethyl acetate (9: 1) is a developping agent
It is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, and take by weighing preparation and be equivalent to crude drug 3.85g, the 10-30ml that adds diethyl ether, sonicated 10-30 minute, filter, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, developping agent one, two, three; Launch respectively; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
| The clear spot degree | The hangover situation | Disturbed condition | |
| Developping agent one | Unintelligible | Do not have | Do not have |
| Developping agent two: | Clear | Do not have | Have |
| Developping agent three: | Clear | Do not have | Do not have |
Can find out that from last table developping agent is at 9: 1 o'clock, on thin layer plate, launch effectively that principal spot is clear, does not have hangover, and is identical with the speckle displacement and the color of reference substance, is fit to testing requirements.
(3) sample solution point sample amount is preferred:
It is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, and take by weighing preparation and be equivalent to crude drug 3.85g, the 10-30ml that adds diethyl ether, sonicated 10-30 minute, filter, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw above-mentioned two kinds of solution each 1 μ l, 3 μ l, 5 μ l, 10 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-ethyl acetate (9: 1); Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Sample solution point sample amount optimization experiment is table as a result
| The point sample amount | 1μl | 3μl | 5μl | 10μl |
| Effect | Test sample is immaculate in corresponding reference substance position | Test sample in corresponding reference substance position spot colors very shallow | Spot colors is identical in corresponding reference substance position for test sample | Spot colors is identical in corresponding reference substance position for test sample, but hangover is arranged slightly. |
Can find out test sample point sample amount when the 5 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
2. frankincense discrimination test screening
(1) the developping agent proportioning is preferred:
Developping agent one: sherwood oil (60-90 ℃)-ethyl acetate (90: 10);
Developping agent two: sherwood oil (60-90 ℃)-ethyl acetate (95: 5);
Developping agent three: sherwood oil (60-90 ℃);
Get frankincense control medicinal material 0.1g, the 1ml that adds diethyl ether flooded 1 hour, and supernatant is as control medicinal material solution.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each the 5 μ l of need testing solution under control medicinal material solution and discriminating (2) item, put respectively on same silica gel g thin-layer plate; With developping agent one, two, three; Launch respectively, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
| The clear spot degree | The hangover situation | Disturbed condition | |
| Developping agent one | Clear | Do not have | Have |
| Developping agent two: | Clear | Do not have | Do not have |
| Developping agent three: | Clear | Do not have | Do not have |
It is clear to find out that from last table above developping agent two, three all develops the color, and does not have hangover, but considers that the simple preferred developping agent of technology is sherwood oil (60-90 a ℃).
(2) sample solution point sample amount is preferred:
Get frankincense control medicinal material 0.1g, the 1ml that adds diethyl ether flooded 1 hour, and supernatant is as control medicinal material solution.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each the 5 μ l of need testing solution under control medicinal material solution and discriminating (2) item, put respectively on same silica gel g thin-layer plate; With developping agent one, two, three; Launch respectively, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Sample solution point sample amount optimization experiment is table as a result
| The point sample amount | 1μl | 3μl | 5μl | 10μl |
| Effect | Test sample is immaculate in corresponding reference substance position | Test sample in corresponding reference substance position spot colors very shallow | Spot colors is identical in corresponding reference substance position for test sample | Spot colors is identical in corresponding reference substance position for test sample, but hangover is arranged slightly. |
Can find out test sample point sample amount when the 5 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
3. earthworm discrimination test screening
(1) preparation of need testing solution
The selection of extraction solvent
Extractant one: methenyl choloride
Extractant two: normal hexane
Extractant three: normal butyl alcohol
It is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, takes by weighing preparation and is equivalent to crude drug 3.08g, adds 70% ethanol 50ml; Placement is spent the night, and filters, and filtrating is steamed to there not being the ethanol flavor, adds water 20ml dissolving; Use extractant one, two, three respectively, extraction is secondary altogether, and each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution.
Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H thin layer plate; With cyclohexane-ethyl acetate (9: 1) is developping agent, launches twice, takes out; Dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
The result
| Launch effect | The forward position | Hangover | Disturb | |
| Extraction one | Clear spot | Do not have | Do not have | Do not have |
| Extraction two | Immaculate | - | - | - |
| Extraction three | Clear spot | Do not have | Do not have | Have |
(2) the developping agent proportioning is preferred:
Developping agent one: cyclohexane-ethyl acetate (8: 2);
Developping agent two: cyclohexane-ethyl acetate (9: 1);
Developping agent three: cyclohexane
It is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, takes by weighing preparation and is equivalent to crude drug 3.08g, adds 70% ethanol 50ml; Placement is spent the night, and filters, and filtrating is steamed to there not being the ethanol flavor, adds water 20ml dissolving; With chloroform extraction 2 times, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution.Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H thin layer plate; With developping agent one, two, three, launch twice respectively, take out; Dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
| The clear spot degree | The hangover situation | Disturbed condition | |
| Developping agent one | Clear | Do not have | Have |
| Developping agent two: | Clear | Do not have | Do not have |
| Developping agent three: | Clear | Have | Do not have |
When last table can find out that developping agent is cyclohexane-ethyl acetate (9: 1), on thin layer plate, launch effectively, principal spot is clear, does not have hangover, and is identical with the speckle displacement and the color of reference substance, is fit to testing requirements.
(3) sample solution point sample amount is preferred:
It is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, takes by weighing preparation and is equivalent to crude drug 3.08g, adds 70% ethanol 50ml; Placement is spent the night, and filters, and filtrating is steamed to there not being the ethanol flavor, adds water 20ml dissolving; With chloroform extraction 2 times, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution.Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Drawing each 1 μ l of above-mentioned two kinds of solution, 3 μ l, 5 μ l, 10 μ l, put respectively on same silica gel H thin layer plate, is developping agent with cyclohexane-ethyl acetate (9: 1); Launch twice; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
Sample solution point sample amount optimization experiment is table as a result
| The point sample amount | The clear spot degree | The hangover situation | Disturbed condition |
| 1μl | Unintelligible | Do not have | Do not have |
| 3μl | The principal spot very slight color | Do not have | Do not have |
| 5μl | Color is clear | Do not have | Do not have |
| 10μl | Color is clear | Have | Do not have |
Can find out test sample point sample amount when the 5 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
Experimental example 3 an inspection experimental study
The research of heavy metal and arsenic salt
The inspection of 1 heavy metal
Assay method: get these article fine powder 2g, put in the crucible, low-temperature carbonization, to 600 ℃ of complete ashing, its residue adds hydrochloric acid 2ml again, and water bath method adds water 15ml, in accordance with the law inspection (an appendix IX of Chinese Pharmacopoeia version in 2005 E second method).Altogether the heavy metal limit of three lot sample article is checked that by assay method content is all less than 10ppm, so exclude text.The result sees table 1.
The heavy metal check result of table 1 three lot sample article
| Lot number | Content of beary metal is in Pb (ppm) |
| 051221010512220205122303 | ＜10＜10＜10 |
The inspection of 2 arsenic salt
Assay method:
The preparation of standard arsenic spot: press first method operation under an appendix IX of Chinese Pharmacopoeia version in 2005 the F item, accurate absorption standard arsenic solution 2ml, preparation in accordance with the law.
Test sample is measured: get these article fine powder 1g, put low-temperature heat charing in the crucible, put cold; Blazingly make ashing gradually at 600 ℃, put coldly, add 10% ammonium nitrate solution and make residue moistening; Put evaporate to dryness in the water-bath then, residue 600 ℃ of blazing ashing extremely fully, is put cold again; Add hydrochloric acid 5ml, add water 23ml and move into to survey in the arsenic bottle, according to " preparation of standard arsenic spot " inspection down.
By the preparation method of arsenic salt inspection under the assay method item arsenic salt of three lot sample article is limited the quantity of and to check that content is all less than 2ppm, so exclude text.The result sees table 2.
The arsenic salt check result of table 2 three lot sample article
| Lot number | Arsenic salt content (ppm) |
| 051221010512220205122303 | ＜2＜2＜2 |
The aconitine limit inspection
The standard items source: the aconitine reference substance is purchased lot number: the 720-200208 in Nat'l Pharmaceutical & Biological Products Control Institute
This is the limit examine of wild aconite root mesaconitine, uses silica gel g thin-layer plate, is developping agent with benzene-ethyl acetate-diethylamine (7: 2: 0.5), launches, and takes out, and dries, and spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of appearance is less than the spot of reference substance.
Experimental example 4 assay experimental studies
The muskone assay
Detecting instrument: Agilent gas phase 4890 chromatographs
Chromatographic column: silicone (OV-17) coating concentration is 5%
Carrier gas: nitrogen
Detector temperature: 240 ℃ of injector temperatures: 220 ℃ of column temperatures: 190 ℃
Reference substance: muskone
Internal standard compound: NSC 77136
Assay method: it is an amount of to get pharmaceutical preparation of the present invention, is ground into fine powder, takes by weighing preparation and is equivalent to crude drug 0.77g, and accurate the title decides, mark liquid 2ml in accurate the adding; Cyclohexane 8ml, close plug, jolting, ultrasonic 30min filters; The accurate subsequent filtrate 2 μ l that draw, inject gas chromatograph calculates, and promptly gets;
Muscone's blank sample preparation: get semen momordicae (shell and deoil) 90g, wild aconite root 90g, resina liquidamberis 90g, frankincense (system) 40g, myrrh (system) 40g, excrementum pteropi (vinegar stir-fry) 90g, Radix Angelicae Sinensis (wine stir-fry) 40g, earthworm 90g, scented ink 8g nine and distinguish the flavor of and be ground into fine powder, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system magma, general ball, low temperature drying promptly gets; The negative controls preparation: get muscone's blank sample, be ground into fine powder, get powder 1g, the accurate title, decide, mark liquid 2ml in accurate the adding, and cyclohexane 8ml, close plug, jolting, ultrasonic 30min, subsequent filtrate is got in filtration, promptly gets.
1. content assaying method is investigated:
(1) stability test
Get reference substance solution (muskone 0.049948mg/ml, NSC 77136 0.0415mg/ml), respectively at 0,4,8,12, the 24 hour sample introduction 2ul in preparation back, measure in accordance with the law, the result shows that it is basicly stable in 24 hours, and the result sees the following form
| Time | 0 | 4 | 8 | 12 | 24 |
| Muskone peak area internal standard compound peak area peak area than mean value RSD | 1578.09877 1376.47678 1.14648 | 1683.76813 1516.55891 1.11026 | 1642.05776 1472.77279 1.11494 1.12648 1.321％ | 1666.26682 1467.02252 1.13518 | 1569.19000 1394.97249 1.12489 |
(2) linear relationship is investigated
| Reference substance concentration (mg/ml) | 0.0099896 | 0.0199792 | 0.024974 | 0.049948 | 0.12487 |
| Internal standard compound concentration (mg/ml) sampling volume (μ l) reference substance average peak area internal standard compound average peak area peak area ratio reference substance sample size (μ g) | 0.0415 2 428.99626 1435.59217 0.29883 0.0199792 | 0.0415 2 594.54983 1351.69904 0.43985 0.0399584 | 0.0415 2 775.31534 1352.28078 0.57334 0.099896 | 0.0415 2 1627.87630 1445.56070 1.12648 0.049948 | 0.0415 2 4127.22159 1438.57991 2.86896 0.24974 |
Ratio with peak area is an ordinate, and the reference substance sample size is a horizontal ordinate, and the drawing standard curve gets regression equation Y=22.7364X+0.0167 (r=0.99945)
(3) precision test
Accurate reference substance solution (muskone concentration is that 0.024974mg/ml, NSC 77136 concentration are 0.0415mg/ml) the 2 μ l that draw repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, and the result sees the following form
| Number of times | 1 | 2 | 3 | 4 | 5 |
| Reference substance peak area internal standard compound peak face | 819.18803 141?5.47752 | 845.26288 1492.46584 | 839.45644 1456.78913 | 832.3?1723 1447.17555 | 782.38522 1387.71853 |
| The ratio mean value RSD correction factor of long-pending peak area | 0.57874 | 0.56635 | 0.57624 0.57205 1.14757％ 1.05209 | 0.57513 | 0.56379 |
(4) reappearance test
Press the text method, get 5 parts in same lot number sample, every part is measured, try to achieve relative standard deviation＜2%, the result sees the following form
| Sample | Sampling amount | The internal standard compound peak area | The muskone peak area | Muskone content | Average content | RSD |
| 12345 | 1.0005 1.0004 1.0007 1.0001 0.9998 | 1605.15101 1075.58918 1130.35463 1302.25319 1376.11908 | 1676.73136 1272.29255 11?83.79078 1435.44985 1447.71338 | 0.4559mg/g 0.4757mg/g 0.4569mg/g 0.4645mg/g 0.4594mg/g | 0.4625mg/g | 1.7525％ |
(5) recovery test sample thief 0.5g, accurate title is fixed, accurate muskone solution (0.24974mg/ml) 1ml that adds, mark liquid 2ml in the accurate again adding, cyclohexane 7ml presses the text method and measures its content, and calculates its recovery, measures the result and sees the following form:
| Sample | 1 | 2 | 3 | 4 | 5 |
| Muskone content mg reference substance addition mg internal standard compound peak area muskone peak area muskone content mg recovery % average recovery rate %RSD% in the sampling amount g sample | 0.5001 0.2313 0.24974 1291.36152 1408.87342 0.47635 98.1234 | 0.5003 0.2314 0.24974 1507.77551 1657.07829 0.47986 99.4861 | 0.5007 0.2316 0.24974 1392.17513 1537.12584 0.48208 100.29700 100.0312 1.3997 | 0.5001 0.2313 0.24974 1129.93304 1257.64236 0.48597 101.9741 | 0.4997 0.2311 0.24974 1276.29388 1407.56147 0.48153 100.27560 |
2. assay result:
| Lot number | Content (mg/g) |
| 051222101 | 0.4625 |
| 051222202 | 0.4587 |
| 051222303 | 0.4421 |
According to above data, content limit is decided to be: the every 1g of these article contains the muscone in muskone, must not be less than 0.3mg.
Experimental example 5 pharmacodynamic experiments
Experimental technique
1, experiment medicine
(1) Hai Pu pharmaceutical factory in 5-FU Shanghai produces.
(2) drug group of the present invention: Moschus 10g, semen momordicae (shell and deoil) 50g, wild aconite root 50g, resina liquidamberis 50g, frankincense (system) 25g, myrrh (system) 25g, excrementum pteropi (vinegar stir-fry) 50g, Radix Angelicae Sinensis (wine stir-fry) 25g, earthworm 50g, scented ink 4g.
[method for making] above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get.
(3) the Chinese medicine side of contrast xiaojin pill is commercially available.
2, experimental technique
(1) inoculates under the aseptic condition S
180Written treaty 2 * 2 * 2mm size is cut apart in the knurl strain, and being inoculated in the right front armpit of kunming mice, subcutaneous (hereinafter to be referred as this mouse is S
180Mouse).
(2) divide into groups to inoculate back second day with S
180Mouse is divided into 4 groups at random; 20 of drug group of the present invention, 18 of Chinese medicine control groups, 5-FU group 19 only reaches S
18030 of mouse control groups.Establish 33 of one group of normal mouse control groups in addition again.
For the demonstration test result, this experiment successively repeats twice with same method.Therefore, above-mentioned animal used as test is divided into two batches at random and experimentizes.
(3) administration drug group of the present invention oral bolus of drug of the present invention every day, the suitable crude drug of dosage is the 0.03g/10g body weight, the Chinese medicine control group oral traditional Chinese medicine every day side of contrast granule, the suitable crude drug of dosage is the 0.03g/10g body weight; 5-FU group lumbar injection 5-FU parenteral solution every day, dosage is the 0.25mg/10g body weight; S
180Mouse control group and normal group mouse then every day oral normal saline 0.4ml, 10 days courses of treatment.
Through pharmacology toxicity test medicine LD of the present invention
50Be 42.3g/kg, the Chinese medicine side of contrast LD
50Be 41.1g/kg.
1. 20 ℃ of microcirculation (ear) room temperatures, after the anesthesia, with the VPV of biology microscope sem observation auricle portion parteriole, veinlet and capillary, and with oscillograph (SBD
-6) record.
Result: microcirculation (ear) normal group mouse and S
180Ear's microcirculation observations before the mouse control group is dead, the VPV of normal mouse parteriole, veinlet and capillary is respectively 0.647 ± 0.131mm/s, 0.610 ± 0.078mm/s and 0.672 ± 0.046mm/s, and S
180The mouse control group then is respectively 0.394 ± 0.047mm/s, 0.249 ± 0.048mm/s and 0.264 ± 0.089mm/s, and both have highly significant difference.Be limited to condition, do not observe the microcirculation of other group mouse.
2. WBV cone and plate viscometer (NEX-1).
The result: WBV mensuration result saw table 1 before each group mouse of WBV was put to death.Under low shear rate (46r/min), the blood viscosity of normal group mouse is starkly lower than S
180Mouse control group and Chinese medicine control group.(under the 230r/min, each organizes mouse blood viscosity no significant difference (P＜0.05), sees table 1 at high shear rate.
Table 1: each experimental mice WBV mensuration (unit: pool gram x ± SD)
| Group | First experiment | Second batch of experiment | ||||
| n | 46r/min | 230r/min | n | 46r/min | 230r/min | |
| The normal mouse group | 10 | 6.784±0.726 | 5.226±5.549 | 15 | 6.216±0.807 | 5.095±0.535 |
| S 180The mouse control group | 17 | 8.512±0.947 | 5.631±0.676 | 17 | 8.24±0.653 | 5.481±0.696 |
| Drug group of the present invention | 10 | 7.730±0.913 | 5.543±0.479 | 8 | 7.013±0.605 | 5.288±0.477 |
| The Chinese medicine control group | 8 | 8.680±0.935 | 5.786±0.722 | 9 | 8.532±1.014 | 5.552±0.745 |
| The 5-FU group | 9 | 7.473±0.673 | 5.506±0.412 | 4 | 7.318±0.593 | 5.410±0.414 |
Low shear rate each group and compared with normal, P＜0.05; The 5-FU group compares P＜0.05 with the S180 control group;
Drug group of the present invention and Chinese medicine control group compare, P＜0.05
Each group of high shear rate compares no significant difference P＞0.05 with normal group
3. isolate tumour behind the heavy sacrifice of animal of knurl, coating around rejecting is claimed weight in wet base immediately.
The result: the knurl repeated root has obvious tumor-inhibiting action according to tumor weight prompting medicine of the present invention that records and 5-FU group, sees table 2.
Each experimental mice tumor-inhibiting action of table 2 is observed
| Group | First experiment | Second batch of experiment | ||||||||
| n | The knurl weight (g, x ± SD) | Tumour inhibiting rate (%) | The t value | P | n | The knurl weight (g, x ± SD) | Tumour inhibiting rate (%) | The t value | P | |
| S 180The mouse control group | 19 | 1.648± 0.648 | 19 | 1.402± 0.667 | ||||||
| Drug group of the present invention | 10 | 0.918± 0.383 | 44.3 | 3.258 | ＜0.01 | 10 | 0.692± 0.337 | 50.8 | 3.115 | ＜0.01 |
| The Chinese medicine control group | 9 | 1.763± 0.632 | -7.0 | 0.442 | ＞0.05 | 9 | 1.351± 0.574 | 3.9 | 0.215 | ＞0.05 |
| The 5-FU group | 10 | 0.482± 0.136 | 70.8 | 5.580 | ＜0.001 | 9 | 0.407± 0.121 | 71.1 | 4.365 | ＜0.001 |
Drug group of the present invention and Chinese drug-treated group compare: P＜0.0.5
4. body weight
The result: 5-FU group mouse body weight does not have significant difference before and after the medication, and prompting 5-FU has the effect that suppresses weight of mice.All the other respectively organize the mouse body weight all increases more than the 4.26g, and there were significant differences before and after the medication sees table 3.
Changes of weight before and after each experimental mice experiment of table 3 (g, x ± SD)
| Group | First experiment | Second batch of experiment | ||||||||||
| n | Before the medicine | Behind the medicine | Weightening finish | The t value | P | n | Before the medicine | Behind the medicine | Weightening finish | The t value | P | |
| Normal mouse | 13 | 21.27 ± 2.02 | 27.81 ± 1.92 | 6.54 | 8.476 | ＜0.001 | 20 | 21.1 ± 1.804 | 30.08 ± 4.034 | 8.98 | 9.088 | ＜0.001 |
| S 180The mouse control group | 19 | 22.26 ± 1.49 | 26.69 ± 2.45 | 4.43 | 6.735 | ＜0.001 | 19 | 21.37 ± 1.892 | 27.51 ± 3.732 | 6.14 | 6.369 | ＜0.001 |
| Drug group of the present invention | 10 | 22.00 ± 1.80 | 26.55 ± 2.10 | 4.55 | 5.211 | ＜0.001 | 10 | 21.1 ± 1.853 | 26.27 ± 2.254 | 5.07 | 5.603 | ＜0.001 |
| The Chinese medicine control group | 9 | 22.28 ± 1.95 | 26.54 ± 3.08 | 4.26 | 3.506 | ＜0.01 | 9 | 21.44 ± 1.590 | 26.3 ± 4.619 | 4.86 | 2.985 | ＜0.05 |
| The 5-FU group | 10 | 22.05 ± 1.50 | 23.1 ± 4.38 | 1.05 | 0.717 | ＜0.01 | 9 | 21.44 ± 1.590 | 20.74 ± 3.418 | ?-0.7 | 0.557 | ＞0.05 |
The following example all can be realized the effect of above-mentioned experimental example.(formulation of the part of summary of the invention should all embody in an embodiment)
Embodiment 1
Moschus 10g, semen momordicae (shell and deoil) 50g, wild aconite root 50g, resina liquidamberis 50g, frankincense (system) 25g, myrrh (system) 25g, excrementum pteropi (vinegar stir-fry) 50g, Radix Angelicae Sinensis (wine stir-fry) 25g, earthworm 50g, scented ink 4g
[method for making] above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get.
Embodiment 2
Moschus 10g, semen momordicae (shell and deoil) 50g, wild aconite root 50g, resina liquidamberis 50g, frankincense (system) 25g, myrrh (system) 25g, excrementum pteropi (vinegar stir-fry) 50g, Radix Angelicae Sinensis (wine stir-fry) 25g, earthworm 50g, scented ink 4g
[method for making] above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve; Get fine powder, add the edible vegetable oil that 0.5-1.5 doubly measures, grind, be pressed into 1000 of soft capsules, promptly get the soft capsule of composition through conventional technology.
Embodiment 3
Moschus 10g, semen momordicae (shell and deoil) 50g, wild aconite root 50g, motherwort 50g, frankincense (system) 25g, dandelion 30g, corydalis tuber 50g, Radix Angelicae Sinensis (wine stir-fry) 25g, earthworm 50g, scented ink 4g
[method for making] above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get.
4 composition pills of embodiment discrimination method:
(1) it is an amount of to get embodiment 1 finished product, is ground into fine powder, takes by weighing 5g, the 20ml that adds diethyl ether, and sonicated 20 minutes filters, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-ethyl acetate (9: 1); Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(2) get frankincense control medicinal material 0.1g, the 1ml that adds diethyl ether flooded 1 hour, and supernatant is as control medicinal material solution.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each the 5 μ l of need testing solution under control medicinal material solution and discriminating (2) item, put respectively on same silica gel g thin-layer plate; With sherwood oil (60-90 ℃) is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(3) it is an amount of to get embodiment 1 finished product, is ground into fine powder, takes by weighing 4g, adds 70% ethanol 50ml; Placement is spent the night, and filters, and filtrating is steamed to there not being the ethanol flavor, adds water 20ml dissolving; With chloroform extraction twice, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution.Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H thin layer plate; With cyclohexane-ethyl acetate (9: 1) is developping agent, launches twice, takes out; Dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
5 composition pills of embodiment inspection method:
It is an amount of that aconitine limit is got embodiment 1 finished product, is ground into fine powder, takes by weighing 10g, puts in the conical flask, adds ammonia solution 10ml; Mix thoroughly, placed 2 hours, add absolute ether 120ml, jolting 1 hour was placed 24 hours; Filter, filtrating adds hydrochloric acid solution (4 → 100) jolting extraction 3 times, and (20ml, 15ml 15ml), merge hydrochloric acid solution; Hydrochloric acid solution adds strong ammonia solution, transfers Ph value to 9～10, adds the absolute ether jolting and extracts 3 times, each 20ml; Merge ether solution, volatilize, residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets the aconitine reference substance, adds absolute ethyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw need testing solution 15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, be developping agent with benzene-ethyl acetate-diethylamine (7: 2: 0.5); Presaturation launched after 2 hours; Take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of appearance should or spot not occur less than the spot of reference substance.
Other is not except that dissolve scattered time limit is checked, other should meet each item regulation (2005 editions one appendix I A of Chinese Pharmacopoeia) relevant under the pill item.
6 composition pills of embodiment content assaying method:
Measure according to vapor-phase chromatography (2005 editions one appendix VI E of Chinese Pharmacopoeia).
Chromatographic condition and system suitability test are stationary phase with silicone (OV-17), and coating concentration is 5%; 190 ℃ of column temperatures, 220 ℃ of injector temperatures, 240 ℃ of detector temperatures are carrier gas with nitrogen.Number of theoretical plate calculates by the muskone peak should be not less than 1500.It is an amount of that correction factor mensuration is got NSC 77136, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as inner mark solution.It is an amount of that other gets the muskone reference substance, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as the reference substance storing solution.Above two kinds of each 2ml of solution of accurate absorption put in the measuring bottle of same 10ml, add cyclohexane and are diluted to scale, shake up, as reference substance solution.Draw reference substance solution 2 μ l, inject gas chromatograph, the calculation correction factor.
Assay method is got embodiment 1 finished product, is ground into fine powder, gets powder 1g, and accurate the title decides, mark liquid 2ml in accurate the adding, and cyclohexane 8ml, close plug, jolting, ultrasonic 30min, filtration, the accurate subsequent filtrate 2 μ l that draw, inject gas chromatograph calculates, and promptly gets.
The every 1g of embodiment 1 finished product contains the muscone with muskone (C
16H
30O) calculate, must not be less than 0.3mg.
7 composition pills of embodiment method of quality control:
Moschus 10g, semen momordicae (shell and deoil) 50g, wild aconite root 50g, resina liquidamberis 50g, frankincense (system) 25g, myrrh (system) 25g, excrementum pteropi (vinegar stir-fry) 50g, Radix Angelicae Sinensis (wine stir-fry) 25g, earthworm 50g, scented ink 4g
[method for making] above ten flavors, except that the muscone, nine flavors such as all the other semen momordicaes are ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieve.Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get.
[discriminating]
(1) it is an amount of to get embodiment 1 finished product, is ground into fine powder, takes by weighing 5g, the 20ml that adds diethyl ether, and sonicated 20 minutes filters, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-ethyl acetate (9: 1); Launch; Take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(2) get frankincense control medicinal material 0.1g, the 1ml that adds diethyl ether flooded 1 hour, and supernatant is as control medicinal material solution.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each the 5 μ l of need testing solution under control medicinal material solution and discriminating (1) item, put respectively on same silica gel g thin-layer plate; With sherwood oil (60-90 ℃) is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(3) it is an amount of to get embodiment 1 finished product, is ground into fine powder, takes by weighing 4g, adds 70% ethanol 50ml; Placement is spent the night, and filters, and filtrating is steamed to there not being the ethanol flavor, adds water 20ml dissolving; With chloroform extraction twice, each 20ml merges methenyl choloride liquid; Evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution.Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system.According to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H thin layer plate; With cyclohexane-ethyl acetate (9: 1) is developping agent, launches twice, takes out; Dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
It is an amount of that [inspection] aconitine limit is got embodiment 1 finished product, is ground into fine powder, takes by weighing 10g, puts in the conical flask, adds ammonia solution 10ml; Mix thoroughly, placed 2 hours, add absolute ether 120ml, jolting 1 hour was placed 24 hours; Filter, filtrating adds hydrochloric acid solution (4 → 100) jolting extraction 3 times, and (20ml, 15ml 15ml), merge hydrochloric acid solution; Hydrochloric acid solution adds strong ammonia solution, transfers Ph value to 9～10, adds the absolute ether jolting and extracts 3 times, each 20ml; Merge ether solution, volatilize, residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution.Other gets the aconitine reference substance, adds absolute ethyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution.Test according to thin-layered chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia); Draw need testing solution 15 μ 1, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, be developping agent with benzene-ethyl acetate-diethylamine (7: 2: 0.5); Presaturation launched after 2 hours; Take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of appearance should or spot not occur less than the spot of reference substance.
Other is not except that dissolve scattered time limit is checked, other should meet each item regulation (2005 editions one appendix I A of Chinese Pharmacopoeia) relevant under the pill item.
[assay] measured according to vapor-phase chromatography (2005 editions one appendix VI E of Chinese Pharmacopoeia).
Chromatographic condition and system suitability test are stationary phase with silicone (OV-17), and coating concentration is 5%; 190 ℃ of column temperatures, 220 ℃ of injector temperatures, 240 ℃ of detector temperatures are carrier gas with nitrogen.Number of theoretical plate calculates by the muskone peak should be not less than 1500.It is an amount of that correction factor mensuration is got NSC 77136, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as inner mark solution.It is an amount of that other gets the muskone reference substance, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as the reference substance storing solution.Above two kinds of each 2ml of solution of accurate absorption put in the measuring bottle of same 10ml, add cyclohexane and are diluted to scale, shake up, as reference substance solution.Draw reference substance solution 2 μ l, inject gas chromatograph, the calculation correction factor.
Assay method is got embodiment 1 finished product, is ground into fine powder, gets powder 1g, and accurate the title decides, mark liquid 2ml in accurate the adding, and cyclohexane 8ml, close plug, jolting, ultrasonic 30min, filtration, the accurate subsequent filtrate 2 μ l that draw, inject gas chromatograph calculates, and promptly gets.
The every 1g of embodiment 1 finished product contains the muscone with muskone (C
16H
30O) calculate, must not be less than 0.3mg.
[function cures mainly] mass dissipating and swelling eliminating, blood-activating analgetic.Be used for scrofula, goiter and tumor, mammary cancer, the newborn addiction of mental disorder due to stagnating, disease is seen lump one place or number place under skin or the skin, pushes away actively, or bone and osteoarthritis, color of the leather is constant, swollen has a pain firmly.
It is oral that [usage and dosage] smashed the back, a 1.2～3g, and 2 times on the one, children's is cut down according to the circumstance.
[attention] pregnant woman forbidding.
The heavy 3g of [specification] per 100 balls.
[storage] sealing.
Claims (1)
1. one kind has mass dissipating and swelling eliminating, and the detection method of the Chinese medicine composition of effect of dissolving stasis and relieving pain is characterized in that this method comprises the steps:
Said Chinese medicine composition is to be processed by following method:
Bulk drug is: shell deoil 50g, wild aconite root 50g, resina liquidamberis 50g, frankincense 25g, myrrh 25g, Oletum Trogopterori (parched with vinegar) 50g, wine of Moschus 10g, semen momordicae fries Radix Angelicae Sinensis 25g, earthworm 50g, scented ink 4g; More than ten flavors, except that the muscone, all the other semen momordicaes etc. nine flavor is ground into fine powder, with muscone's porphyrize, with above-mentioned powder facing-up, sieves; Every 100g powder adds starch 25g, mixing, and in addition with starch 5g system 14% starch slurry, general ball, dry below 80 ℃, promptly get;
Said detection method comprises following discrimination method, assay and aconitine limit inspection method:
Differentiate:
A, to get finished product an amount of, is ground into fine powder, takes by weighing 5g, the 20ml that adds diethyl ether, and sonicated 20 minutes filters, the filtrating evaporate to dryness, residue adds ethanol 1ml makes dissolving, as need testing solution; Other gets Radix Angelicae Sinensis control medicinal material 1g, shines medicinal material solution in pairs with legal system; Test according to 2005 editions one appendix VI B of Chinese Pharmacopoeia thin-layered chromatography; Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, be developping agent with normal hexane-ethyl acetates of 9: 1; Launch; Take out, dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
B, get frankincense control medicinal material 0.1g, the 1ml that adds diethyl ether flooded 1 hour, and supernatant is as control medicinal material solution; According to the test of 2005 editions one appendix VI B of Chinese Pharmacopoeia thin-layered chromatography, draw control medicinal material solution and each the 5 μ l of need testing solution that differentiate under a item, put respectively on same silica gel g thin-layer plate; With sherwood oil 60-90 ℃ is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
C, to get finished product an amount of, is ground into fine powder, takes by weighing 4g, adds 70% ethanol 50ml, and placement is spent the night; Filter, filtrating is steamed to there not being the ethanol flavor, adds water 20ml dissolving, with chloroform extraction twice, and each 20ml; Merge methenyl choloride liquid, evaporate to dryness, residue is with methyl alcohol 2ml dissolving, as need testing solution; Other gets earthworm control medicinal material 1g, shines medicinal material solution in pairs with legal system; According to the test of 2005 editions one appendix VI B of Chinese Pharmacopoeia thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel H thin layer plate; With cyclohexane-ethyl acetate of 9: 1 was developping agent, launched twice, took out; Dry, put under the 365nm ultraviolet lamp and inspect; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
Inspection: it is an amount of that aconitine limit is got finished product, is ground into fine powder, takes by weighing 10g, puts in the conical flask, adds ammonia solution 10ml; Mix thoroughly, placed 2 hours, add absolute ether 120ml, jolting 1 hour was placed 24 hours; Filter, filtrating adds hydrochloric acid solution 4 → 100 joltings extracts 3 times, is respectively 20ml, 15ml, 15ml; Merge hydrochloric acid solution, hydrochloric acid solution adds strong ammonia solution, transfers Ph value to 9～10, adds the absolute ether jolting and extracts 3 times, each 20ml; Merge ether solution, volatilize, residue adds absolute ethyl alcohol 1ml makes dissolving, as need testing solution; Other gets the aconitine reference substance, adds absolute ethyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; Test according to 2005 editions one appendix VI B of Chinese Pharmacopoeia thin-layered chromatography; Draw need testing solution 15 μ l, reference substance solution 5 μ l, put respectively in same be on the silica gel g thin-layer plate of bonding agent with the sodium carboxymethyl cellulose, be developping agent with benzene-ethyl acetate of 7: 2: 0.5-diethylamine; Presaturation launched after 2 hours; Take out, dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of appearance should or spot not occur less than the spot of reference substance;
Other is not except that dissolve scattered time limit is checked, other should meet each item regulation relevant under 2005 editions one appendix I A of the Chinese Pharmacopoeia pill item;
Assay: according to 2005 editions one appendix VI E of Chinese Pharmacopoeia gas chromatography determination;
Chromatographic condition and system suitability test are stationary phase with silicone OV-17, and coating concentration is 5%; 190 ℃ of column temperatures, 220 ℃ of injector temperatures, 240 ℃ of detector temperatures are carrier gas with nitrogen; Number of theoretical plate calculates by the muskone peak should be not less than 1500;
It is an amount of that correction factor mensuration is got NSC 77136, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as inner mark solution; It is an amount of that other gets the muskone reference substance, and accurate the title decides, and adds cyclohexane and processes the solution that every 1ml contains 0.2mg, as the reference substance storing solution; Above two kinds of each 2ml of solution of accurate absorption put in the measuring bottle of same 10ml, add cyclohexane and are diluted to scale, shake up, as reference substance solution; Draw reference substance solution 2 μ l, inject gas chromatograph, the calculation correction factor; Assay method is got finished product, is ground into fine powder, gets powder 1g, and accurate the title decides, mark liquid 2ml in accurate the adding, and cyclohexane 8ml, close plug, jolting, ultrasonic 30min, filtration, the accurate subsequent filtrate 2 μ l that draw, inject gas chromatograph calculates, and promptly gets;
The every 1g of finished product contains the muscone and calculates with muskone, must not be less than 0.3mg.
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| CN102114090A (en) * | 2009-12-30 | 2011-07-06 | 成都永康制药有限公司 | Preparation and medical use of minor gold pills for male testicular nodular lesions |
| CN102520111A (en) * | 2011-12-16 | 2012-06-27 | 西藏奇正藏药股份有限公司 | Method for detecting eight-flavour agilawood preparation |
| CN102419357B (en) * | 2011-12-26 | 2014-11-12 | 西藏奇正藏药股份有限公司 | Method for detecting eighteen-component codonopsis pilosula preparation |
| CN102641398A (en) * | 2012-04-22 | 2012-08-22 | 李承平 | Drug composition for phlegm reduction, stasis removal and detumescence |
| CN102759598B (en) * | 2012-07-31 | 2014-10-15 | 山东阿如拉药物研究开发有限公司 | Quality detection method for 29-componnet stagnation dissipation powder as Tibetan medicinal composition and preparations thereof |
| CN106770881A (en) * | 2016-12-08 | 2017-05-31 | 中国人民解放军第三〇七医院 | Bone aches quiet capsule quality control method |
| CN114636762B (en) * | 2022-01-19 | 2023-04-25 | 山东宏济堂制药集团股份有限公司 | Quality control method of musk Xintongning tablet |
| CN115590834A (en) * | 2022-10-28 | 2023-01-13 | 北京亚东生物制药有限公司（Cn） | Cassia twig and poria cocos pills and preparation method thereof |
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Effective date of registration: 20180110 Address after: Anguo City in Hebei province 071299 Baoding Yifeng Road No. 1 Patentee after: Beijing Ya Dong Biological Pharmaceutical Co. Ltd. (Yasukuni) Address before: 102200, 8, Zhenxing Road, Zhongguancun science and Technology Park, Beijing, Changping District Patentee before: Beijing Asia-East Bio-Pharmaceutical Co., Ltd. |