CN1579518A - Trditional Chinese medicinal composition for treating colonitis, its preparation method and quality control method - Google Patents

Trditional Chinese medicinal composition for treating colonitis, its preparation method and quality control method Download PDF

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CN1579518A
CN1579518A CN 200410038268 CN200410038268A CN1579518A CN 1579518 A CN1579518 A CN 1579518A CN 200410038268 CN200410038268 CN 200410038268 CN 200410038268 A CN200410038268 A CN 200410038268A CN 1579518 A CN1579518 A CN 1579518A
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methanol
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CN100540021C (en
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邹节明
孟杰
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Guilin Sanjin Pharmaceuticals Co Ltd
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Guilin Sanjin Pharmaceuticals Co Ltd
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Abstract

The invention discloses a Chinese traditional medicine compound for curing colonitis and its manufacturing method, quality control method. The compound is made up of Chinese goldthread, psoralea fruit, astragalus root, aucklandia root, downy rosemyrtle root, and notoginseng. The astraglaus root, aucklandia root and downy rosemyrtle root are immersed, stewed, condensed, thus acquires the supernatant; carries on alcohol extraction to the Chinese goldthread, psoralea fruit and notoginseng, and filters them, then the filtered liquid is combined with above mentioned supernatant, and adds in accessories, and they are produced into each kind of preparation. At the same time, the invention also provides a quality control method for the compound. The invention can be applied to cure colonitis, and it has prominent effect for curing chronic nonspecific ulcerous colonitis.

Description

Chinese medicine composition of treatment colitis and preparation method thereof, method of quality control
Invention field
The present invention relates to the preparation method and the quality standard of a kind of Chinese medicine composition and said composition, particularly a kind of Chinese medicine composition that is used for the treatment of colitis relates to the preparation method and the quality standard of said composition simultaneously.
Background technology
Colitis is that a kind of symptom is diarrhoea, stomachache, tenesmus, and serious case can have loss of appetite, the glutted discomfort of upper abdomen, the disease of nausea and vomiting etc.Colitis onset minority is hurried, and most slowly the course of disease can be divided persistence, or is the chronic process that stage of attack and catabasis alternate.The inducement of outbreak mostly is direct stimulation, fatigue, drinking and eating irregularly.The Therapeutic Method of modern medicine adopts hormone more, can alleviate in various degree, but side effect is arranged.The invention provides a kind of Chinese patent medicine for the treatment of colitis, definite effect, and do not have obvious toxic-side effects, more obvious to the chronic non-specific ulcerative colitis effect especially.The present invention is under instructing according to Chinese medical theory, and the Chinese patent medicine preparation that utilizes modernized pharmaceutical technology to make is fit to industrialized great production.
Summary of the invention
One object of the present invention is to disclose a kind of Chinese medicine composition of new treatment colitis; Another object of the present invention is to disclose a kind of preparation method of Chinese medicine composition of new treatment colitis; The 3rd purpose of the present invention is to disclose a kind of method of quality control of Chinese medicine composition of new treatment colitis.
The present invention seeks to be achieved through the following technical solutions:
The crude drug composition and the proportioning of pharmaceutical composition of the present invention are as follows:
Rhizoma Coptidis 100-400 weight portion Fructus Psoraleae 350-900 weight portion Radix Astragali 450-1350 weight portion
Radix Aucklandiae 120-380 weight portion Radix Rhodomyrti 345-900 weight portion Radix Notoginseng 175-600 weight portion
The above-mentioned raw materials optimum ratio is: Rhizoma Coptidis 225 weight portions, Fructus Psoraleae 750 weight portions, the Radix Astragali 900 weight portions, the Radix Aucklandiae 250 weight portions, Radix Rhodomyrti 750 weight portions, Radix Notoginseng 375 weight portions
Press practice of pharmacy, the above-mentioned raw materials medicine can be prepared into various clinical acceptable forms, include but not limited to a kind of in the middle of the following dosage form: as solid preparations such as tablet, pill, capsule, granule, drop pill, soft capsule and suppositorys, liquid preparations such as suspensoid, oral liquid, enema, preferred capsule formulation, tablet, granule dosage form.
This preparation of drug combination method: above Six-element crude drug, get the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti and add the water that 2-12 doubly measures, soaked 0-2 hour, decoct 1-4 time, each 0.5-4 hour, collecting decoction filters, and it is 1.05-1.45 (40 ℃-80 ℃) that filtrate is concentrated into relative density, add 60-95% ethanol and reach 40-80% to containing the alcohol amount, stir evenly, left standstill 6-48 hour, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng adds 4-12 and doubly measures the 30%-95% alcohol reflux 2-4 time, each 0.5-4 hour, filter, merge with above-mentioned supernatant, reclaim ethanol, being concentrated into relative density is the extractum of 1.05～1.48 (45-80 ℃), dry, pulverize, add starch and/or other suitable adjuvants, as zein, dextrin, starch derivatives such as beta-schardinger dextrin-, cellulose and derivant thereof, mannitol, lactose, Polyethylene Glycol, polyvinylpyrrolidone, magnesium stearate, micropowder silica gel, sodium lauryl sulphate etc., its consumption is equivalent to the 3%-30% of extract powder weight, mixing is granulated, encapsulated or direct compression or make suitable preparation such as granule.
The method of quality control that this compositions is made medicament comprises discriminating and/or assay.
Discrimination method comprises a kind of and/or several in the following method:
(1) get unit formulation content 1g, add the methanol 20ml of 5%-99.5%, supersound process 20～40 minutes filters, and filtrate is concentrated into 8～12ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.5g～0.8g, gets control medicinal material solution with legal system; Get the berberine hydrochloride reference substance again, the methanol that adds 5%-99.5%, make the solution that every 1ml contains 0.3～1.0mg, product solution in contrast, the thin layer chromatography test, draw each 1～3 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, benzene-ethyl acetate-isopropyl alcohol-methanol-the strong ammonia solution that with the ratio is 3-8: 2-6: 1-4: 1-4: 0.2-3 is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 12～18 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
(2) get unit formulation content 2.5g, add the ethyl acetate 20ml of 5%-99.5%, supersound process 10～60 minutes filters, and filtrate is concentrated into 1.6～2.5ml, as need testing solution; Other gets psoralen, the isopsoralen reference substance, the ethyl acetate that adds 5%-99.5%, make the solution that every 1ml contains 1～3mg, product solution in contrast, the thin layer chromatography test, draw each 3～6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that benzene-ethyl acetate of 5-12: 0.2-2 is developing solvent with the ratio, launch, take out, dry, spray is with 5～15% potassium hydroxide methanol solutions, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get unit formulation content 2.5g, add kieselguhr 2～4g, mixing, put in the flask, add 1～5% sodium hydrate methanol solution, 75～92ml, reflux, extract, 50～80 minutes filters, the filtrate evaporate to dryness, residue adds water 40～65ml makes dissolving, moves in the separatory funnel, with water saturated n-butanol extraction 2～6 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.4～0.8%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with 30～70ml water elution, discard water lotion, the ethanol elution of reuse 35～60ml40～50% earlier, discard ethanol elution, continue with the ethanol elution of 80～150ml 70～80%, collect ethanol elution, evaporate to dryness, methanol 0.7～1.5ml that residue adds 5%-99.5% makes dissolving, as need testing solution; Other gets the astragaloside reference substance, and the methanol that adds 5%-99.5% is made the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance, add methanol and make the solution that every 1ml contains 0.6～1.5mg, product solution in contrast, the thin layer chromatography test, draw each 4～7 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol-the water that with the ratio is 3-9: 2-6: 0.2-3 is developing solvent, and 8～12 ℃ are launched down, take out, dry, spray 7～12% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 90～110 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Content assaying method comprises a kind of and/or several in the following method:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 70-85: 25-35 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000.
The preparation precision of phosphoric acid triethylamine buffer is measured phosphatase 11-5ml, triethylamine 1-5ml, and thin up is to 1000ml, promptly.
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 10～15mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 8～15ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and hydrochloric berberine 30～90 μ g of wherein every 1ml.
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, accurate 0.5～1.5% methanol hydrochloride solution, the 40～60ml that adds, claim to decide weight, supersound process (power 250W, 40kHz) 20～40 minutes, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.5～1.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution.
Algoscopy: accurate respectively reference substance solution and each 8～12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride (C 20H 17NO 4.HCl) meter must not be less than 2.0mg.
Wherein in method of quality control, used methanol of discrimination method or ethyl acetate concentration range are 10-35%, 40-65% or 70-95%; Methanol or ethyl acetate concentration preferred 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90% or 95%.
This pharmaceutical preparation is mainly used in the application of treatment colitis, and is evident in efficacy to chronic non-specific ulcerative colitis especially.Following experimental example further specifies the present invention.
Experimental example 1: acetic acid is caused the protective effect of rat ulcer colitis
Knot recovering capsule (technical scheme gained capsule of the present invention) 0.64g/kg, 0.32g/kg and the 0.16g/kg body weight to acetic acid modeling rat reduces obviously influence of nothing by bursting; The heavy index of intestinal (total colectomy weight/total colectomy length) to rat improves significantly; And obviously alleviate the colonic mucosal injury index and reduce the MPO of colon level.The knot recovering capsule of bursting also can reduce rat colonitis intestinal tissue MDA, NO content, increases SOD and GSH-Px level.
Histopathology result shows that model group rat colon mucous epithelium comes off, and is damaged, fills with a large amount of inflammatory leukocytes and lymphocyte, has ulcer, slough to form.Intestinal mucosa crypts part or diffusivity disappear, mucoprotein secretion reduce or lack as.Water breakthrough is swollen, congested and hemorrhage around the ulcer.The knot recovering capsule group of bursting rat colon mucous epithelium damaged the alleviating that come off, the ulcer zone obviously dwindles, ulcer periphery intestinal mucosa covering epithelium proliferation for repairing, part covers; Inflammatory cell reduces, and the remarkable hypertrophy of granulation tissue shows certain therapeutical effect.The positive control drug sulfasalazine also can promote ulcer healing, alleviates inflammatory reaction, promotes enteric epithelium reparation and granulation tissue hyperplasia.
Experimental example 2: trinitro-benzene-sulfonic acid is caused the protective effect of rat ulcer colitis
Routed knot recovering capsule 0.64g/kg, 0.32g/kg and 0.16g/kg alleviate no obvious improvement effect to TNBS modeling rat body weight; The heavy index of intestinal (total colectomy weight/total colectomy length) increase to rat improves significantly; Burst knot recovering capsule 0.64g/kg and 0.32g/kg to the above-mentioned general pathology morphological change effect of having clear improvement, can obviously reduce the colonic mucosal injury index and reduce the MPO of colon level.3 the dosage groups of knot recovering capsule of bursting can be resisted atrophy of thymus gland, and burst knot recovering capsule 0.64g/kg and 0.32g/kg can obviously suppress spleen and increase, and reduce index and spleen index.The knot recovering capsule of bursting also can reduce rat colonitis intestinal tissue MDA content, increases the SOD level.
Histopathology result shows that model group rat colon mucous epithelium comes off, and is damaged, ulcer, the visible from top to bottom inflammatory exudate of ulcer, slough, granulation tissue and scar tissue.See under the mirror that big amount lymphocyte and neutrophilic leukocyte soaks and holostrome.Intestinal mucosa crypts part or diffusivity disappear, mucoprotein secretion reduce or lack as.Water breakthrough is swollen, congested and hemorrhage around the ulcer.The knot recovering capsule group of bursting rat colon mucous epithelium damaged the alleviating that come off, ulcer periphery intestinal mucosa covering epithelium proliferation for repairing, part covers, and inflammatory cell reduces, and the remarkable hypertrophy of granulation tissue shows certain therapeutical effect.The positive control drug sulfasalazine also can alleviate inflammatory reaction, promotes enteric epithelium reparation and granulation tissue hyperplasia.
Experimental example 3: antiinflammatory action experiment
1, routed knot recovering capsule xylol causes the influence of mice ear
The knot recovering capsule 0.8g/kg that bursts can obviously suppress dimethylbenzene induced mice ear thickness, and suppression ratio is 20.7%; Routed knot recovering capsule 0.4g/kg and 0.2g/kg do not have obvious influence to the mice ear degree.
2, routed knot recovering capsule is to the influence of rat carrageenan foot swelling
Burst knot recovering capsule 0.64g/kg and 0.32g/kg all can obviously suppress rat paw edema due to the carrageenin, and 3 hours suppression ratio are respectively 40.5% and 33.2% after medication; Rat paw edema does not have obvious influence due to the knot recovering capsule 0.16g/kg on Carrageenan of bursting.
3, burst the knot recovering capsule to the bullate influence of rat granuloma
Routed knot recovering capsule 0.64g/kg and 0.32g/kg all can obviously suppress the hypertrophy of rat granulation tissue, and suppression ratio is respectively 12.9% and 12.1%; The knot recovering capsule 0.16g/kg that bursts does not have obvious influence to the hypertrophy of rat granulation tissue.
Experimental example 4: analgesic activity experiment
Mice hot plate method experimental result shows, the knot recovering capsule gastric infusion of bursting, 0.8g/kg and 0.4g/kg all can obviously improve the pain threshold of mice in 1 hour after administration, and 0.2g/kg does not have obvious effect.The mouse writhing experimental result shows, burst knot recovering capsule 0.8g/kg and 0.4g/kg all can obviously prolong mice turn round body incubation period and reduce mice turn round the body number of times.
Experimental example 5: the diarrhea effect reaches the experiment to the normal mouse bowel movement function
1, routed knot recovering capsule causes the influence of diarrhea of mouse to Folium Sennae
Burst and tie the recovering capsule gastric infusion, the just sum minimizing of mice dehumidifying that 0.8g/kg, 0.4g/kg and 0.2g/kg all can make Folium Sennae cause.
2, burst the knot recovering capsule to the hyperfunction influence of neostigmine induced mice intestinal propulsion
Burst and tie the recovering capsule gastric infusion, the mouse small intestine propelling that 0.8g/kg and 0.4g/kg can obviously suppress due to the neostigmine is hyperfunction, and 0.2g/kg does not have obvious inhibitory action.
3, routed knot recovering capsule is to the influence of normal mouse defecation
Burst and tie the recovering capsule gastric infusion, 0.8g/kg, 0.4g/kg and 0.2g/kg can obviously suppress the defecation motion of mice in 2h and 6h; Three dosage of knot recovering capsule of bursting can obviously prolong mice defecation incubation period.
4, burst the knot recovering capsule to the propulsive influence of small intestine movement of mice
Burst and tie the recovering capsule gastric infusion, 0.8g/kg has the obvious suppression effect to the intestinal ahead running of normal mouse, and 0.4g/kg and 0.2g/kg do not have obvious influence.
Experimental example 6: to the experiment of body's immunity
This drug capsules dosage form 0.8g/kg and 0.4g/kg are to 2, and the inflammatory reaction that the 4-dinitrofluorobenzene causes, lymphopoiesis and cytokine TNF-α increase all tangible antagonism, but IL-1 β is increased obviously influence of nothing.
The specific embodiment
Embodiment 1The capsule preparation
Get Rhizoma Coptidis 100g, Fructus Psoraleae 400g, Radix Astragali 550g, Radix Aucklandiae 150g, Radix Rhodomyrti 400g, Radix Notoginseng 200g, get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 4 times of amounts, decoct 1 time, each 1 hour, collecting decoction filtered, its relative density was 1.05 when filtrate was concentrated into 50 ℃, added 65% ethanol and reached 50% to containing the alcohol amount, stirred evenly, left standstill 10 hours, and got supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 6 times of amount 40% alcohol reflux 2 times, each 1 hour, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.1 extractum when being concentrated into 45 ℃-80 ℃, drying, pulverize, add starch, its consumption is equivalent to 5% of extract powder weight, mixing, granulate, encapsulated.
Embodiment 2Preparation tablets
Get Rhizoma Coptidis 200g, Fructus Psoraleae 500g, Radix Astragali 650g, Radix Aucklandiae 250g, Radix Rhodomyrti 600g, Radix Notoginseng 300g, get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 6 times of amounts, soaked 0.5 hour, decoct 2 times, each 2 hours, collecting decoction, filter, its relative density was 1.15 when filtrate was concentrated into 60 ℃, added 75% ethanol and reached 60% to containing the alcohol amount, stir evenly, left standstill 20 hours, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 8 times of amount 50% alcohol reflux 3 times, each 2 hours, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.2 extractum when being concentrated into 60 ℃, drying, pulverize, add beta-schardinger dextrin-, its consumption is equivalent to 10% of extract powder weight, mixing, granulate direct compression.
Embodiment 3The granule preparation
Get Rhizoma Coptidis 300g, Fructus Psoraleae 700g, Radix Astragali 850g, Radix Aucklandiae 300g, Radix Rhodomyrti 700g, Radix Notoginseng 400g, get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 8 times of amounts, soaked 1 hour, decoct 3 times, each 3 hours, collecting decoction, filter, its relative density was 1.25 when filtrate was concentrated into 70 ℃, added 85% ethanol and reached 70% to containing the alcohol amount, stir evenly, left standstill 30 hours, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 10 times of amount 60% alcohol reflux 4 times, each 3 hours, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.3 extractum when being concentrated into 70 ℃, drying, pulverize, add mannitol, its consumption is equivalent to 15% of extract powder weight, mixing, granulate, make granular preparation.
Embodiment 4The capsule preparation
Get Rhizoma Coptidis 400g, Fructus Psoraleae 800g, Radix Astragali 1050g, Radix Aucklandiae 350g, Radix Rhodomyrti 800g, Radix Notoginseng 500g, get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 10 times of amounts, soaked 1.5 hours, decoct 4 times, each 4 hours, collecting decoction, filter, its relative density was 1.35 when filtrate was concentrated into 80 ℃, added 90% ethanol and reached 80% to containing the alcohol amount, stir evenly, left standstill 40 hours, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 12 times of amount 80% alcohol reflux 3 times, each 4 hours, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.4 extractum when being concentrated into 80 ℃, drying, pulverize, add lactose, its consumption is equivalent to 25% of extract powder weight, mixing, granulate, encapsulated.
Embodiment 5Preparation tablets
Get Rhizoma Coptidis 400g, Fructus Psoraleae 350g, Radix Astragali 450g, Radix Aucklandiae 380g, Radix Rhodomyrti 345g, Radix Notoginseng 600g, get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 4 times of amounts, soaked 1.5 hours, decoct 1 time, each 4 hours, collecting decoction, filter, its relative density was 1.35 when filtrate was concentrated into 50 ℃, added 65% ethanol and reached 80% to containing the alcohol amount, stir evenly, left standstill 10 hours, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 12 times of amount 40% alcohol reflux 4 times, each 1 hour, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.1 extractum when being concentrated into 80 ℃, drying, pulverize, add sodium lauryl sulphate, its consumption is equivalent to 25% of extract powder weight, mixing, granulate direct compression.
Embodiment 6The granule preparation
Get Rhizoma Coptidis 100g, Fructus Psoraleae 900g, Radix Astragali 1350g, Radix Aucklandiae 120g, Radix Rhodomyrti 900g, Radix Notoginseng 175g, get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 10 times of amounts, decoct 4 times, each 1 hour, collecting decoction filtered, its relative density was 1.05 when filtrate was concentrated into 80 ℃, added 90% ethanol and reached 50% to containing the alcohol amount, stirred evenly, left standstill 40 hours, and got supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 6 times of amount 80% alcohol reflux 2 times, each 4 hours, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.4 extractum when being concentrated into 50 ℃, drying, pulverize, add polyvinylpyrrolidone, its consumption is equivalent to 5% of extract powder weight, mixing, granulate, make granular preparation.
Embodiment 7The capsule preparation
Get Rhizoma Coptidis 225g, Fructus Psoraleae 750g, Radix Astragali 900g, Radix Aucklandiae 250g, Radix Rhodomyrti 750g, Radix Notoginseng 375g, above Six-element crude drug is got the water that the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti add 8 times of amounts, soaks 0.5 hour, decoct 2 times, each 1 hour, collecting decoction, filter, it is 1.25 (60 ℃) that filtrate is concentrated into relative density, adds 85% ethanol and reaches 60% to containing the alcohol amount, stir evenly, left standstill 12 hours, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng add 8 times of amount 60% alcohol reflux 3 times, each 2 hours, filter, merge with above-mentioned supernatant, reclaim ethanol, being concentrated into relative density is the extractum of 1.25 (65 ℃), dry, pulverize, add starch and beta-schardinger dextrin-, its consumption is equivalent to 25% of extract powder weight, mixing, granulate, encapsulated, promptly.
Embodiment 8Discrimination test
A. get this product content 1g, add methanol 20ml, supersound process 30 minutes filters, and filtrate is concentrated into 10ml, as need testing solution.Other gets Rhizoma Coptidis control medicinal material 0.8g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.5mg, product solution in contrast, test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be 7: 5: 0.8 with ratio: benzene-ethyl acetate of 1.5: 3-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove in addition side adds isopyknic strong ammonia solution, pre-equilibration 15 minutes, launch, take out, dry in the air out, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color.
B. get this product content 2.5g, add ethyl acetate 20ml, supersound process 30 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add ethyl acetate and make the solution that every 1ml contains 1mg, product solution in contrast, test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 5: 0.3 is developing solvent, launches, and takes out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected, in the test sample chromatograph with 8% potassium hydroxide methanol solution, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. get this product content 2.5g, add kieselguhr 3g, mixing, put in the flask, add 1% sodium hydrate methanol solution 65ml, reflux, extract, 45 minutes, filter, filtrate evaporate to dryness, residue add water 50ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 3 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.5%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 60% ethanol 50ml eluting earlier, discard 60% ethanol elution, continue with 65% ethanol 100ml eluting, collect 65% ethanol elution, evaporate to dryness, residue adds methanol 1.5ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds methanol and makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance, add methanol and make the solution that every 1ml contains 0.5mg, product solution in contrast, test according to thin layer 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 adhesive with the sodium carboxymethyl cellulose, with ratio is that chloroform-methanol-water of 5: 3: 0.6 is developing solvent, and 10 ℃ are launched down, take out, dry, spray 5% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 100 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 9Discrimination test
A. get unit formulation content 1g, add 10% methanol 20ml, supersound process 20 minutes filters, and filtrate is concentrated into 8ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.5g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 10% methanol, make the solution that every 1ml contains 0.4mg, product solution in contrast, each 1 μ l of above-mentioned three kinds of solution is drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 3: 2: 1: benzene-ethyl acetate of 1: 0.5-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 13 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 10% ethyl acetate 20ml, supersound process 10 minutes filters, and filtrate is concentrated into 1.6ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 10% ethyl acetate and make the solution that every 1ml contains 1mg, product solution in contrast, the thin layer chromatography test, draw each 3 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 5: 0.2 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 5% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 2g, mixing, put in the flask, add 1% sodium hydrate methanol solution 75ml, reflux, extract, 50 minutes, filter, filtrate evaporate to dryness, residue add water 40ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 2 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.4%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 30ml eluting, discard water liquid, reuse 30% ethanol 35ml eluting earlier, discard ethanol elution, continue with 70% ethanol 80ml eluting, collect ethanol elution, evaporate to dryness, residue adds 10% methanol 0.7ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 10% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance adds 10% methanol and makes the solution that every 1ml contains 0.6mg, in contrast product solution; The thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 4: 2: 0.2 is that developing solvent launches down for 8 ℃ with ratio, take out, dry, spray 7% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 90 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 10Discrimination test
A. get unit formulation content 1g, add 20% methanol 25ml, supersound process 25 minutes filters, and filtrate is concentrated into 9ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.6g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 20% methanol, make the solution that every 1ml contains 0.5mg, product solution in contrast, each 2 μ l of above-mentioned three kinds of solution are drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 4: 3: 2: benzene-ethyl acetate of 2: 1-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 14 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 20% ethyl acetate 25ml, supersound process 20 minutes filters, and filtrate is concentrated into 1.8ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 20% ethyl acetate and make the solution that every 1ml contains 2mg, product solution in contrast, the thin layer chromatography test, draw each 4 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 7: 0.5 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 7% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 2.5g, mixing, put in the flask, add 2% sodium hydrate methanol solution 78ml, reflux, extract, 55 minutes, filter, filtrate evaporate to dryness, residue add water 45ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 3 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.5%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 35ml eluting, discard water liquid, reuse 35% ethanol 40ml eluting earlier, discard ethanol elution, continue with 75% ethanol 90ml eluting, collect ethanol elution, evaporate to dryness, residue adds 20% methanol 0.9ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 20% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance adds 20% methanol and makes the solution that every 1ml contains 0.8mg, in contrast product solution; The thin layer chromatography test, 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 adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 5: 3: 0.5 is that developing solvent launches down for 10 ℃ with ratio, take out, dry, spray 8% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 100 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 11Discrimination test
A. get unit formulation content 1g, add 40% methanol 30ml, supersound process 30 minutes filters, and filtrate is concentrated into 10ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.7g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 40% methanol, make the solution that every 1ml contains 0.6mg, product solution in contrast, each 3 μ l of above-mentioned three kinds of solution are drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 5: 4: 3: benzene-ethyl acetate of 3: 1.5-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 15 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 40% ethyl acetate 30ml, supersound process 30 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 40% ethyl acetate and make the solution that every 1ml contains 3mg, product solution in contrast, the thin layer chromatography test, 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 adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 8: 0.8 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 9% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 3g, mixing, put in the flask, add 3% sodium hydrate methanol solution 82ml, reflux, extract, 60 minutes, filter, filtrate evaporate to dryness, residue add water 50ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 4 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.6%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 40ml eluting, discard water liquid, reuse 40% ethanol 45ml eluting earlier, discard ethanol elution, continue with 80% ethanol 100ml eluting, collect ethanol elution, evaporate to dryness, residue adds 40% methanol 1ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 40% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance adds 40% methanol and makes the solution that every 1ml contains 1mg, in contrast product solution; The thin layer chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 6: 4: 1 is that developing solvent launches down for 12 ℃ with ratio, take out, dry, spray 9% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 110 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 12Discrimination test
A. get unit formulation content 1g, add 60% methanol 20ml, supersound process 35 minutes filters, and filtrate is concentrated into 11ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.8g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 60% methanol, make the solution that every 1ml contains 0.7mg, product solution in contrast, each 1 μ l of above-mentioned three kinds of solution is drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 6: 5: 4: benzene-ethyl acetate of 4: 2-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 16 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 60% ethyl acetate 35ml, supersound process 40 minutes filters, and filtrate is concentrated into 2.2ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 60% ethyl acetate and make the solution that every 1ml contains 1mg, product solution in contrast, the thin layer chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 9: 1.2 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 10% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 3.5g, mixing, put in the flask, add 4% sodium hydrate methanol solution 88ml, reflux, extract, 70 minutes, filter, filtrate evaporate to dryness, residue add water 60ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 5 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.7%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 45% ethanol 50ml eluting earlier, discard ethanol elution, continue with 70% ethanol 120ml eluting, collect ethanol elution, evaporate to dryness, residue adds 60% methanol 1.1ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 60% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance adds 60% methanol and makes the solution that every 1ml contains 1.2mg, in contrast product solution; The thin layer chromatography test, draw each 7 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 7: 5: 1.5 is that developing solvent launches down for 8 ℃ with ratio, take out, dry, spray 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 90 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 13Discrimination test
A. get unit formulation content 1g, add 80% methanol 25ml, supersound process 40 minutes filters, and filtrate is concentrated into 12ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.7g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 80% methanol, make the solution that every 1ml contains 0.8mg, product solution in contrast, each 2 μ l of above-mentioned three kinds of solution are drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 7: 6: 4: benzene-ethyl acetate of 4: 2.5-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 17 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 80% ethyl acetate 40ml, supersound process 50 minutes filters, and filtrate is concentrated into 2.5ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 80% ethyl acetate and make the solution that every 1ml contains 2mg, product solution in contrast, the thin layer chromatography test, 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 adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 10: 1.5 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 12% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 4g, mixing, put in the flask, add 5% sodium hydrate methanol solution 90ml, reflux, extract, 75 minutes, filter, filtrate evaporate to dryness, residue add water 65ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 6 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.8%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 60ml eluting, discard water liquid, reuse 50% ethanol 55ml eluting earlier, discard ethanol elution, continue with 75% ethanol 140ml eluting, collect ethanol elution, evaporate to dryness, residue adds 80% methanol 1.2ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 80% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance adds 80% methanol and makes the solution that every 1ml contains 1.4mg, in contrast product solution; The thin layer chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 8: 6: 2 is that developing solvent launches down for 10 ℃ with ratio, take out, dry, spray 11% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 100 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 14Discrimination test
A. get unit formulation content 1g, add 99.5% methanol 30ml, supersound process 40 minutes filters, and filtrate is concentrated into 12ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.8g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 99.5% methanol, make the solution that every 1ml contains 0.9mg, product solution in contrast, each 3 μ l of above-mentioned three kinds of solution are drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 6: 3: 1.5: benzene-ethyl acetate of 1.5: 0.5-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 18 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 99.5% ethyl acetate 40ml, supersound process 60 minutes filters, and filtrate is concentrated into 2.5ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 99.5% ethyl acetate and make the solution that every 1ml contains 3mg, product solution in contrast, the thin layer chromatography test, draw each 6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 12: 2 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 15% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 4g, mixing, put in the flask, add 5% sodium hydrate methanol solution 92ml, reflux, extract, 80 minutes, filter, filtrate evaporate to dryness, residue add water 65ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 6 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.8%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 70ml eluting, discard water liquid, reuse 50% ethanol 60ml eluting earlier, discard ethanol elution, continue with 80% ethanol 150ml eluting, collect ethanol elution, evaporate to dryness, residue adds 99.5% methanol 1.5ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 99.5% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance adds 99.5% methanol and makes the solution that every 1ml contains 1.5mg, in contrast product solution; The thin layer chromatography test, draw each 7 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that chloroform-methanol-water of 9: 6: 2.5 is that developing solvent launches down for 12 ℃ with ratio, take out, dry, spray 12% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 110 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 15The berberine hydrochloride content test
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 72: 28 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000.
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphatase 11 .7ml, triethylamine 1.8ml, and thin up is to 1000ml, promptly.
The preparation precision of reference substance solution takes by weighing the berberine hydrochloride reference substance 15mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, and promptly gets (the hydrochloric berberine 45 μ g of every 1ml).
The preparation of need testing solution: get the content under this product content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 0.8% methanol hydrochloride solution 50ml that adds, claim to decide weight, supersound process (power 250W, 40kHz) 30 minutes, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.8% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Every of this product contains Rhizoma Coptidis with berberine hydrochloride (C 20H 17NO 4.HCl) meter must not be less than 2.0mg.
Embodiment 16The berberine hydrochloride content test
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 70: 25 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphoric acid 2ml, triethylamine 2ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 10mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 8ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and the hydrochloric berberine 32 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 0.5% methanol hydrochloride solution 40ml that adds, claim to decide weight, at power 250W, supersound process is 20 minutes under the 40kHz, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 8 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
Embodiment 17The berberine hydrochloride content test
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 75: 30 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphoric acid 3ml, triethylamine 3ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 12mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 10ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and the hydrochloric berberine 48 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 1% methanol hydrochloride solution 50ml that adds, claim to decide weight, at power 250W, supersound process is 30 minutes under the 40kHz, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 1% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
Embodiment 18The berberine hydrochloride content test
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 80: 35 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphatase 24 ml, triethylamine 4ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 15mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 12ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and the hydrochloric berberine 72 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 1.5% methanol hydrochloride solution 60ml that adds, claim to decide weight, at power 250W, supersound process is 40 minutes under the 40kHz, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 1.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
Embodiment 19The berberine hydrochloride content test
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 80: 25 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphatase 24 ml, triethylamine 2ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 15mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 8ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and the hydrochloric berberine 48 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 0.5% methanol hydrochloride solution 60ml that adds, claim to decide weight, at power 250W, supersound process is 20 minutes under the 40kHz, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 1.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 8 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
Embodiment 20The berberine hydrochloride content test
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 70: 35 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphoric acid 2ml, triethylamine 4ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 10mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 12ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and the hydrochloric berberine 48 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 1.5% methanol hydrochloride solution 40ml that adds, claim to decide weight, at power 250W, supersound process is 40 minutes under the 40kHz, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
Embodiment 21The preparation of capsule
Get Rhizoma Coptidis 225g, Fructus Psoraleae 750g, Radix Astragali 900g, Radix Aucklandiae 250g, Radix Rhodomyrti 750g, Radix Notoginseng 375g, 1000 of the capsules that makes by the preparation method of above-mentioned capsule, every heavy 0.5g, colitis patient is oral, 3 times on the one, one time 2.
Embodiment 22The preparation of capsule
Get Rhizoma Coptidis 225g, Fructus Psoraleae 750g, Radix Astragali 900g, Radix Aucklandiae 250g, Radix Rhodomyrti 750g, Radix Notoginseng 375g makes 1000 of capsules by the preparation method of above-mentioned capsule, every heavy 0.5g, chronic colitis patient is oral, 3 times on the one, one time 2.
Embodiment 23The preparation of capsule
Get Rhizoma Coptidis 225g, Fructus Psoraleae 750g, Radix Astragali 900g, Radix Aucklandiae 250g, Radix Rhodomyrti 750g, Radix Notoginseng 375g makes 1000 of capsules by the preparation method of above-mentioned capsule, every heavy 0.5g, chronic non-specific ulcerative colitis patient is oral, 3 times on the one, one time 2.

Claims (12)

1, a kind of pharmaceutical composition for the treatment of colitis is characterized in that this pharmaceutical composition is made up of following crude drug:
Rhizoma Coptidis 100-400 weight portion Fructus Psoraleae 350-900 weight portion
Radix Astragali 450-1350 weight portion Radix Aucklandiae 120-380 weight portion
Radix Rhodomyrti 345-900 weight portion Radix Notoginseng 175-600 weight portion.
2, pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is made up of following crude drug:
The Rhizoma Coptidis 225 weight portion Fructus Psoraleaes 750 weight portion Radixs Astragali 900 weight portions
The Radix Aucklandiae 250 weight portion Radix Rhodomyrtis 750 weight portion Radix Notoginseng 375 weight portions.
3, pharmaceutical composition as claimed in claim 1 or 2, it is characterized in that said composition can make clinically any or pharmaceutically acceptable dosage form, as tablet, pill, capsule, granule, drop pill, soft capsule, suppository, suspensoid, oral liquid, enema.
4, preparation of drug combination method as claimed in claim 1 or 2 is characterized in that this method may further comprise the steps:
Get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water that 2-12 doubly measures, soaked 0-2 hour, decoct 1-4 time, each 0.5-4 hour, collecting decoction filters, and its relative density was 1.05-1.45 when filtrate was concentrated into 40 ℃-80 ℃, add 60-95% ethanol and reach 40-80% to containing the alcohol amount, stir evenly, left standstill 6-48 hour, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng adds 4-12 and doubly measures the 30%-95% alcohol reflux 2-4 time, each 0.5-4 hour, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.05～1.48 extractum when being concentrated into 45 ℃-80 ℃, dry, pulverize, add starch and/or other starch derivatives: zein, dextrin, beta-schardinger dextrin-, cellulose and derivant thereof, mannitol, lactose, Polyethylene Glycol, polyvinylpyrrolidone, magnesium stearate, micropowder silica gel, sodium lauryl sulphate, its consumption is equivalent to the 3%-30% of extract powder weight, mixing is granulated, encapsulated or direct compression or make granular preparation.
5, preparation of drug combination method as claimed in claim 4 is characterized in that this method may further comprise the steps:
Get the Six-element crude drug in proportion, the Radix Astragali, the Radix Aucklandiae, Radix Rhodomyrti are added the water of 8 times of amounts, soaked 0.5 hour, decoct 2 times, each 1 hour, collecting decoction filters, and its relative density was 1.20 when filtrate was concentrated into 60 ℃, add 85% ethanol and reach 60% to containing the alcohol amount, stir evenly, left standstill 12 hours, get supernatant; Rhizoma Coptidis, Fructus Psoraleae, Radix Notoginseng adds 8 times of amount 60% alcohol reflux 3 times, each 2 hours, filter, merge with above-mentioned supernatant, reclaim ethanol, relative density is 1.20～1.30 extractum when being concentrated into 60 ℃, dry, pulverize, add starch and/other starch derivatives: zein, dextrin, beta-schardinger dextrin-, cellulose and derivant thereof, mannitol, lactose, Polyethylene Glycol, polyvinylpyrrolidone, magnesium stearate, micropowder silica gel, sodium lauryl sulphate, its consumption is equivalent to 25% of extract powder weight, mixing is granulated, encapsulated or direct compression or make granular preparation.
6, the method for quality control of claim 1 or 2 described pharmaceutical compositions is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A. get unit formulation content 1g, add the methanol 20ml of 5%-99.5%, supersound process 20～40 minutes filters, and filtrate is concentrated into 8～12ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.5g～0.8g, gets control medicinal material solution with legal system; Get the berberine hydrochloride reference substance again, the methanol that adds 5%-99.5%, make the solution that every 1ml contains 0.3～1.0mg, product solution in contrast, the thin layer chromatography test, draw each 1～3 μ 1 of above-mentioned three kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, benzene-ethyl acetate-isopropyl alcohol-methanol-the strong ammonia solution that with the ratio is 3-8: 2-6: 1-4: 1-4: 0.2-3 is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 12～18 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add the ethyl acetate 20ml of 5%-99.5%, supersound process 10～60 minutes filters, and filtrate is concentrated into 1.6～2.5ml, as need testing solution; Other gets psoralen, the isopsoralen reference substance, the ethyl acetate that adds 5%-99.5%, make the solution that every 1ml contains 1～3mg, product solution in contrast, the thin layer chromatography test, draw each 3～6 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be that benzene-ethyl acetate of 5-12: 0.2-2 is developing solvent with the ratio, launch, take out, dry, spray is with 5～15% potassium hydroxide methanol solutions, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 2～4g, mixing, put in the flask, add 1～5% sodium hydrate methanol solution, 75～92ml, reflux, extract, 50～80 minutes filters, the filtrate evaporate to dryness, residue adds water 40～65ml makes dissolving, moves in the separatory funnel, with water saturated n-butanol extraction 2～6 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.4～0.8%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with 30～70ml water elution, discard water lotion, reuse 35～60ml earlier, 30～50% ethanol elution, discard ethanol elution, continue with the ethanol elution of 80～150ml 70～80%, collect ethanol elution, evaporate to dryness, methanol 0.7～1.5ml that residue adds 5%-99.5% makes dissolving, as need testing solution; Other gets the astragaloside reference substance, and the methanol that adds 5%-99.5% is made the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance, the methanol that adds 5%-99.5% is made the solution that every lml contains 0.6～1.5mg, product solution in contrast, the thin layer chromatography test, draw each 4～7 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, chloroform-methanol-the water that with the ratio is 3-9: 2-6: 0.2-3 is developing solvent, and 8～12 ℃ are launched down, take out, dry, spray 7～12% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 90～110 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
7, require the method for quality control of 6 described pharmaceutical compositions as profit, it is characterized in that discrimination method in this method comprises one or more in the following discriminating:
A. get unit formulation content 1g, add 99.5% methanol 20ml, supersound process 30 minutes filters, and filtrate is concentrated into 10ml, as need testing solution; Other gets Rhizoma Coptidis control medicinal material 0.5g, gets control medicinal material solution with legal system.Get the berberine hydrochloride reference substance again, add 99.5% methanol, make the solution that every 1ml contains 0.5mg, product solution in contrast, each 2 μ l of above-mentioned three kinds of solution are drawn in thin layer chromatography test, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with ratio is 6: 3: 1.5: benzene-ethyl acetate of 1.5: 0.5-isopropyl alcohol-methanol-strong ammonia solution is developing solvent, groove side in addition adds isopyknic strong ammonia solution, and pre-equilibration 15 minutes launches, take out, dry in the air out, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with control medicinal material, on the corresponding position of reference substance chromatograph, show the fluorescence speckle of same color;
B. get unit formulation content 2.5g, add 99.5% ethyl acetate 20ml, supersound process 30 minutes filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets psoralen, isopsoralen reference substance, add 99.5% ethyl acetate and make the solution that every 1ml contains 2mg, product solution in contrast, the thin layer chromatography test, 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 adhesive with the sodium carboxymethyl cellulose, with ratio is that benzene-ethyl acetate of 9.5: 0.5 is developing solvent, launches, and takes out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 10% potassium hydroxide methanol solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get unit formulation content 2.5g, add kieselguhr 3g, mixing, put in the flask, add 2% sodium hydrate methanol solution 80ml, reflux, extract, 60 minutes, filter, filtrate evaporate to dryness, residue add water 50ml makes dissolving, move in the separatory funnel, with water saturated n-butanol extraction 3 times, each 30ml, merge n-butyl alcohol liquid, evaporate to dryness adds 0.5%NaOH solution 20ml and makes dissolving, solution leads to macroporous adsorptive resins, with water 50ml eluting, discard water liquid, reuse 30% ethanol 50ml eluting earlier, discard ethanol elution, continue with 70% ethanol 100ml eluting, collect ethanol elution, evaporate to dryness, residue adds 99.5% methanol 1ml makes dissolving, as need testing solution; Other gets the astragaloside reference substance, adds 99.5% methanol, makes the solution that every 1ml contains 1mg, gets ginsenoside Rb again 1, ginsenoside Re, ginsenoside Rg 1And Panax Notoginseng saponin R 1Reference substance, add 99.5% methanol and make the solution that every 1ml contains 1mg, product solution in contrast, the thin layer chromatography test, 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 adhesive with the sodium carboxymethyl cellulose, with ratio is that chloroform-methanol-water of 7: 3: 0.5 is that developing solvent launches down for 10 ℃, take out, dry, spray 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
8, require the method for quality control of 1 or 2 described pharmaceutical compositions as profit, it is characterized in that the content assaying method in this method comprises following assay method:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 70-85: 25-35 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphatase 11-5ml, triethylamine 1-5ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 10～15mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 8～15ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and hydrochloric berberine 30～90 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, accurate 0.5～1.5% methanol hydrochloride solution, the 40～60ml that adds, claim to decide weight, at power 250W, supersound process is 20～40 minutes under the 40kHz, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.5～1.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 8～12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
9, require the method for quality control of 8 described pharmaceutical compositions as profit, it is characterized in that the assay in this method comprises following assay method:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 70-80: 26-32 is a mobile phase; Detect wavelength 264 ± 5nm.Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation precision of phosphoric acid triethylamine buffer is measured phosphatase 11-2.5ml, triethylamine 1-2.5ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 11～14mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 9～11ml, puts in the 25ml measuring bottle, adds methanol to scale, shake up, that is, and hydrochloric berberine 35～72 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under the unit formulation content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, accurate 0.6～1.2% methanol hydrochloride solution, the 40～60ml that adds, claim to decide weight, power 250W, supersound process is 20～40 minutes under the 40kHz condition, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.5～1.5% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 8～12 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of unit formulation contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg.
10, require the method for quality control of 8 described pharmaceutical compositions as profit, it is characterized in that the assay in this method comprises following assay method:
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Ratio is that phosphoric acid triethylamine buffer-acetonitrile of 72: 28 is a mobile phase; Detect wavelength 264 ± 5nm; Number of theoretical plate calculates by berberine hydrochloride should be lower than 3000;
The preparation of phosphoric acid triethylamine buffer: precision is measured phosphatase 11 .7ml, triethylamine 1.8ml, and thin up is to 1000ml, promptly;
The preparation of reference substance solution: precision takes by weighing the berberine hydrochloride reference substance 15mg that is dried to constant weight through phosphorus pentoxide, puts in the measuring bottle of 100ml, adds dissolve with methanol and is diluted to scale, shakes up; Precision is measured 10ml, puts in the 25ml measuring bottle, adds methanol to scale, shakes up, the hydrochloric berberine 60 μ g of wherein every 1ml;
The preparation of need testing solution: get the content under this product content uniformity item, mixing is got 0.25g, put in the conical flask, the accurate title, decide, the accurate 0.8% methanol hydrochloride solution 50ml that adds, claim to decide weight, power 250W, supersound process is 30 minutes under the 40kHz condition, put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with 0.8% methanol hydrochloride solution, filter, get subsequent filtrate as need testing solution;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of this product contains Rhizoma Coptidis with berberine hydrochloride C 20H 17NO 4.HCl meter must not be less than 2.0mg;
11, the application of pharmaceutical composition as claimed in claim 1 or 2 in the medicine of preparation treatment colitis.
12, the application of pharmaceutical composition as claimed in claim 1 or 2 in the medicine of preparation treatment ulcerative colitis.
CNB2004100382680A 2004-05-19 2004-05-19 Chinese medicine composition of treatment colitis and preparation method thereof, method of quality control Expired - Lifetime CN100540021C (en)

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101596296B (en) * 2008-06-02 2011-08-17 北京亚东生物制药有限公司 Method for controlling quality of infant antidiarrheal granules
CN102228530A (en) * 2011-06-25 2011-11-02 南方医科大学 Capsule for treating ulcerative colitis
JP2012116838A (en) * 2005-07-26 2012-06-21 Shanxi Yabao Pharmaceutical Group Corp Medicinal substance having narcotic addiction treatment action and preparation method thereof
CN102908430A (en) * 2012-09-29 2013-02-06 刘敏 Oral combined medicament for treating chronic colitis
CN103926366A (en) * 2013-01-15 2014-07-16 天士力制药集团股份有限公司 Detection method for effective components of astragalus Salvia Miltiorrhiza qi-benefiting dropping pill
CN109342619A (en) * 2018-11-14 2019-02-15 神威药业集团有限公司 Stilbene Huang leads to the measuring method of Astragaloside content in secret soft capsule
CN109521118A (en) * 2018-12-18 2019-03-26 广西壮族自治区兽医研究所 Method that is a kind of while measuring 4 kinds of phenolic substancess in myrtle fruit
CN110794078A (en) * 2019-11-20 2020-02-14 刘圣梅 Method for identifying medicine for treating colitis
CN110794080A (en) * 2019-11-20 2020-02-14 刘圣梅 Method for detecting quality of medicine for treating colitis

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012116838A (en) * 2005-07-26 2012-06-21 Shanxi Yabao Pharmaceutical Group Corp Medicinal substance having narcotic addiction treatment action and preparation method thereof
CN101596296B (en) * 2008-06-02 2011-08-17 北京亚东生物制药有限公司 Method for controlling quality of infant antidiarrheal granules
CN102228530A (en) * 2011-06-25 2011-11-02 南方医科大学 Capsule for treating ulcerative colitis
CN102228530B (en) * 2011-06-25 2012-08-08 南方医科大学 Capsule for treating ulcerative colitis
CN102908430A (en) * 2012-09-29 2013-02-06 刘敏 Oral combined medicament for treating chronic colitis
CN103926366A (en) * 2013-01-15 2014-07-16 天士力制药集团股份有限公司 Detection method for effective components of astragalus Salvia Miltiorrhiza qi-benefiting dropping pill
CN103926366B (en) * 2013-01-15 2016-08-31 天士力制药集团股份有限公司 A kind of detection method of QISHEN YIQI DIWAN active ingredient
CN109342619A (en) * 2018-11-14 2019-02-15 神威药业集团有限公司 Stilbene Huang leads to the measuring method of Astragaloside content in secret soft capsule
CN109521118A (en) * 2018-12-18 2019-03-26 广西壮族自治区兽医研究所 Method that is a kind of while measuring 4 kinds of phenolic substancess in myrtle fruit
CN110794078A (en) * 2019-11-20 2020-02-14 刘圣梅 Method for identifying medicine for treating colitis
CN110794080A (en) * 2019-11-20 2020-02-14 刘圣梅 Method for detecting quality of medicine for treating colitis

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