CN101485872B - Chinese medicinal composition for treating gastropathy as well as preparation and detection method thereof - Google Patents
Chinese medicinal composition for treating gastropathy as well as preparation and detection method thereof Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine composition for treating gastrosis. The traditional Chinese medicine composition is prepared from starfish, alum, dried orange peels, blood clam shells, oysters, Atractylodes macrocephaia, Astragalus membranaceus, dried ginger, peppers and other medicines according to weight ratio, and has good effect of treating diseases such as weakness of the spleen and the stomach, stomach cold and pain, acid stomach and gastroduodenal ulcer. Moreover, the invention discloses a method for preparing the traditional Chinese medicine composition and a quality control method for the traditional Chinese medicine composition.
Description
Technical field
The present invention relates to a kind of new compound Chinese medicinal preparation for the treatment of gastropathy, more particularly, relate to a kind of Chinese medicine composition for the treatment of diseases such as weakness of the spleen and stomach, cold syndrome of the stomach are had a pain, hyperchlorhydria, gastric and duodenal ulcers and preparation method thereof and method of quality control.
Background technology
Peptic Ulcers is a kind of common chronic systemic disease, is divided into gastric ulcer and duodenal ulcer, is called peptic ulcer again.Peptic ulcer mainly is because gastric acid and pepsin are formed to the mucosa autodigestion, and Peptic Ulcers belongs to categories such as " gastric abscess ", " stomachache due to hyperactive liver-QI attacking the stomach ", " pained ", " acid regurgitation " of motherland's medical science." epigastric pain ", " peratodynia ", " stomachache ", " the hungry full consumptive disease " etc. of being called among the people more.Peptic Ulcers is a clinical characters with the rhythmicity upper abdominal pain of outbreak repeatedly, often with belch, return acid, sensation such as scorching hot, noisy, even also have and feel sick, vomiting, hematemesis, have blood in stool.Circle, oval chronic ulcer are arranged in the gastrointestinal part.The sickness rate of Peptic Ulcers increases year by year in recent years, and should the disease course of disease longer, and the Chang Fanfu outbreak is not touchingly healed.If therapeutic effect is not obvious, violent stomachache often takes place, can cause complication such as gastrorrhagia, gastric perforation, pyloric obstruction to occur, also there is severe patient can develop into canceration.
Treatment peptic ulcer common chemical medicine has sucralfate, bismuth aluminate compound, cimetidine, ranitidine, omeprazole etc. at present, but often costs an arm and a leg, and has taken certain side effect for a long time; Chinese patent medicine commonly used has KUAIWEI PIAN, Fuzi Lizhong Wan etc., but the prescription of above-mentioned Chinese patent medicine and stress the face difference is also very big to the curative effect difference of dissimilar Peptic Ulcerss.Therefore, the Chinese patent medicine of new treatment gastropathy is still thirsted in this area.
Summary of the invention
The present invention is according to the Chinese medicine theory, in conjunction with modern pharmacy, pharmacodynamic experiment, invented a kind of Chinese medicine composition, can treat diseases such as weakness of the spleen and stomach, cold syndrome of the stomach are had a pain, hyperchlorhydria, gastric and duodenal ulcers, especially caused stomachache of cold syndrome of the stomach and gastric and duodenal ulcers there is good curative effect, and have instant effect, good analgesic effect, characteristics such as have no adverse reaction.
The purpose of this invention is to provide a kind of Chinese medicine composition for the treatment of gastropathy.
Another object of the present invention provides the preparation method of this Chinese medicine composition.
Another object of the present invention provides the method for quality control of this Chinese medicine composition.
For achieving the above object, the invention provides following technical scheme:
The invention provides a kind of Chinese medicine composition for the treatment of gastropathy, it is by comprising that following bulk drugs makes:
Asterias amurensis Lutken 1-25 part Alumen 1-10 part Pericarpium Citri Reticulatae 1-15 part
Concha Arcae 1-15 part Concha Ostreae 1-15 part Rhizoma Atractylodis Macrocephalae 1-15 part
Radix Astragali 1-15 part Rhizoma Zingiberis 1-15 part Fructus Piperis 1-10 part.
Preferably, the invention provides a kind of Chinese medicine composition for the treatment of gastropathy, it is by comprising that following bulk drugs makes:
Asterias amurensis Lutken 2-20 part Alumen 1-8 part Pericarpium Citri Reticulatae 1-10 part
Concha Arcae 1-10 part Concha Ostreae 1-10 part Rhizoma Atractylodis Macrocephalae 1-10 part
Radix Astragali 1-10 part Rhizoma Zingiberis 1-10 part Fructus Piperis 1-8 part.
More preferably, the invention provides a kind of Chinese medicine composition for the treatment of gastropathy, it is by comprising that following bulk drugs makes:
Asterias amurensis Lutken 5-18 part Alumen 1-5 part Pericarpium Citri Reticulatae 1-8 part
Concha Arcae 1-8 part Concha Ostreae 1-8 part Rhizoma Atractylodis Macrocephalae 1-8 part
Radix Astragali 1-8 part Rhizoma Zingiberis 1-8 part Fructus Piperis 1-5 part.
Particularly preferably, the invention provides a kind of Chinese medicine composition for the treatment of gastropathy, it is by comprising that following bulk drugs makes:
4 parts of 2 parts of Pericarpium Citri Reticulataes of 8 parts of Alumens of Asterias amurensis Lutken
4 parts of 4 parts of Rhizoma Atractylodis Macrocephalaes of 4 portions of Concha Ostreaes of Concha Arcae
2 parts in 4 portions of Fructus Piperiss of 4 portions of Rhizoma Zingiberiss of the Radix Astragali.
In technical scheme of the present invention, wherein, Asterias amurensis Lutken randomly is an Asterias amurensis Lutken (processed); Alumen randomly is a dried Alumen; Pericarpium Citri Reticulatae randomly is the Pericarpium Citri Reticulatae charcoal; Concha Arcae randomly is a Concha Arcae (calcined); Concha Ostreae randomly is a Concha Ostreae (calcined); The Rhizoma Atractylodis Macrocephalae randomly is a Rhizoma Atractylodis Macrocephalae (parched).
In Chinese medicine composition of the present invention, Asterias amurensis Lutken, Alumen are monarch drug.Described Asterias amurensis Lutken is the dry all of Asteriidae animal Luo Shi sea dish (Asterias rollestoni bell), solaster dakisoni Verrill (Solaster DawsoniVerrill), Potiria pectinifera (Mukller et Tro Sehel) (Asterinia Pectinifera (M ü ller et Troschel)), wheel Asterias amurensis Lutken (Crossasterpapposus (Linne)) or sand starfish (Luidia quinariavon Marterns), distinguish the flavor of, property is put down, be good at stomach function regulating antacid, promote ulcer healing; To be sulfuric acid based mineral alunite through processing refine described Alumen makes, and sour in the mouth, puckery is cold in nature, is good at removing dampness and holds back bleb, and hemostasisization is rotten, match with Asterias amurensis Lutken, and the stomach reinforcing infections that heals, removing the necrotic tissue and promoting granulation is at a main disease main therapeutical effect.
Pericarpium Citri Reticulatae, Concha Arcae, Concha Ostreae are ministerial drug.Described Pericarpium Citri Reticulatae is the dry mature skin of rutaceae orange (Citrus reticulataBlanco) and variety thereof, and bitter in the mouth, suffering are warm in nature, but regulating qi-flowing for strengthening spleen, drying dampness to eliminate phlegm; Described Concha Arcae is the shell of Carnis Arca inflata section animal Scapharca subcrenata (Arca subcrenata Lischke) or Scapharca broughtonii (Arca inflata Reeve), salty in the mouth, and property is flat, is good at the expectorant blood stasis dispelling, hard masses softening and resolving, relieving gastric hyperacidity to alleviate stomachache; Described Concha Ostreae is the shell of long Concha Ostreae (Ostrea gigas Thunberg), Dalian Bay Concha Ostreae (Ostrea talienwhanensis Crosse) or Crassostrea rivularis (Ostrea rivularis Gould) of Ostreidae animal, distinguish the flavor of, cold nature, but hard masses softening and resolving, the convergence blood stasis dispelling.Above-mentioned three flavor medicines share, and can assist monarch drug to strengthen the treatment qi depression to blood stasis, stomach network damage disease.
The Rhizoma Atractylodis Macrocephalae, the Radix Astragali, Rhizoma Zingiberis, Fructus Piperis are adjuvant drug, and the described Rhizoma Atractylodis Macrocephalae is the dry rhizome of the feverfew Rhizoma Atractylodis Macrocephalae (Atractylodesmacrocephala Koidz.), and bitter in the mouth, sweet is warm in nature, is good at invigorating the spleen and benefiting QI, the dampness diuretic; The described Radix Astragali is the dry root of leguminous plant Radix Astagali (Astragalus membranaceus (Fisch.) Bge.var.mongholicus (Bge.) Hsiao) or Radix Astragali (Astragalus membranaceus (Fisch.) Bge.), sweet in the mouth, warm in nature, be good at invigorating QI to consolidate the body surface resistance, expelling pus and promoting granulation; Described Rhizoma Zingiberis is the dry rhizome of zingiber (Zingiber officinale Rosc.), and acrid in the mouth is hot in nature, is good at warming spleen and stomach for dispelling cold, the dampness expectorant; Described Fructus Piperis is dry near maturation or the mature fruit of Piperaceae plant Fructus Piperis (Piper nigrum L.), and acrid in the mouth is hot in nature, is used for gastrofrigid vomiting, matches with Rhizoma Zingiberis, directly treats stomachache with cool feeling, and makes the sour and astringent property of Asterias amurensis Lutken, dried Alumen.
Above-mentioned nine flavor medicines share, and cold and heat are also transferred, and giving consideration to both the incidental and fundamental can make the strong fortune of taste, stagnantization of stagnation resolvation, and stomach network recovering of injured, and all diseases are from removing.
The above-mentioned raw materials medicine all should meet the current edition " regulation of relevant medical material in the Chinese pharmacopoeia, and concoct processing by the concocted specification of corresponding pharmacopeia regulation or recognition of state.
As for Chinese medicine composition of the present invention,,, can make clinical required various dosage forms, for example tablet, pill, granule and capsule in conjunction with the modern Chinese medicine preparation process with above crude drug.
On the other hand, the invention provides a kind of method for preparing above-mentioned Chinese medicine composition, comprise the steps:
(1) it is standby to take by weighing described materials of weight proportions medicine;
(2) Asterias amurensis Lutken is put in the steam pot and to steam 1 to 4 hour, preferred 2-3 hour, preferred especially 2 hours, dry for standby;
(3) above nine flavor medicine mixed powders are broken into fine powder, cross the 100-300 mesh sieve; Fully mix homogeneously gets mixture;
(4) said mixture is added acceptable accessories, make required dosage form by rules of preparations.
Above-described rules of preparations is meant what the pharmaceutics those of ordinary skill was grasped, maybe the general technology of preparing of the related preparations that can learn from document and textbook.
On the other hand, in order effectively to control the quality of product of the present invention, the present invention also provides the method for quality control of above-mentioned Chinese medicine composition, the one or more kinds of combinations that comprise the following steps: the thin layer discriminating of the Radix Astragali, the discriminating of Asterias amurensis Lutken gel electrophoresis, dried Alumen assay and Pericarpium Citri Reticulatae assay.
Here, the thin layer of the described Radix Astragali is differentiated: get this product powder 5g, porphyrize adds methanol 60ml, reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extract 2-4 time with water saturated n-butyl alcohol jolting, be preferably 3 times, each 20ml merges n-butyl alcohol liquid, with 1% sodium hydroxide solution washing 1-3 time, preferably 2 times, be respectively 100ml and 50ml, the water 50ml washing that the reuse n-butyl alcohol is saturated, get n-butyl alcohol liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Astragali control medicinal material 0.5g, adds methanol 30ml, shines medical material solution in pairs with legal system; Get the astragaloside reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of need testing solution 8 μ l, control medicinal material solution and reference substance solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (preferably, volume ratio is 13: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing at 105 ℃, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color under the daylight; The fluorescence speckle of apparent same color under the ultraviolet light;
Here, the gel electrophoresis of described Asterias amurensis Lutken is differentiated and is: get this product powder 2g, porphyrize adds 6ml hot water, cover preservative film, 100 ℃ heating in water bath 10-60 minute, be preferably 30 minutes, put the centrifugalize of cold back, preferably 4000rpm is centrifugal 20 minutes, divides and gets supernatant, as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; According to electrophoresis method (2005 editions three appendix IV C of Chinese Pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution respectively, carry out the SDS-polyacrylamide gel electrophoresis by following deposition condition, promptly; In the test sample Zone electophoresis band, with the corresponding position of control medicinal material Zone electophoresis band on show the protein band of same color; Described deposition condition is: resolving gel concentration 12.5%; Concentrate gum concentration 5%; Constant current 30mA; Voltage 200V; Electrophoresis time is 2 hours; With coomassie brilliant blue R250 dyeing 4 hours, the shaking table decolouring;
Here, the content assaying method of described dried Alumen is: get this product, porphyrize is got about 1g, the accurate title, decide, add dilute hydrochloric acid 10ml, heating is preferably boiled, 5-30 minute altogether, preferably 10 minutes, filter water 100ml gradation washing container and filtering residue, merge washing liquid and filtrate, add water 50ml respectively, 2 of instructions phenolphthalein solutions, 10% potassium hydroxide solution 9ml shakes up, and drips 10% potassium hydroxide solution to blush, drip dilute hydrochloric acid again to red the disappearance, add acetic acid-ammonium acetate buffer (pH4.8) 25ml, precision adds Calcium Disodium Versenate volumetric solution (0.05mol/L) 25ml again, and heating keeps little boiling 10 minutes, put and be chilled to room temperature, add 0.5% xylenol orange indicator solution 1.5ml, change into orange redly with zinc volumetric solution (preferably concentration is 0.05mol/L) titration to solution from pale brown color, and titrating result proofreaied and correct with blank assay; Every 1ml Calcium Disodium Versenate volumetric solution (0.05mol/L) is equivalent to the aluminium potassium sulfate (KAl (SO of 12.91mg
4)
2); And the every 1g of regulation this product contains dried Alumen with aluminium potassium sulfate (KAl (SO
4)
2) meter, must not be less than 50mg;
Here, the content assaying method of described Pericarpium Citri Reticulatae is:
The preparation of reference substance solution: it is an amount of to get the Hesperidin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains Hesperidin 30 μ g, promptly;
The preparation of need testing solution: get this product, porphyrize is got about 0.5g, and accurate the title decides, put in the tool plug conical flask accurate methanol 10ml, the close plug of adding, claim to decide weight, supersound process (power 200W, 59kHz) 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 1ml, put in the 10ml measuring bottle, add methanol to scale, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water-acetic acid (30: 66: 4) is mobile phase; The detection wavelength is 283nm.Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
Algoscopy: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D), accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; And the every 1g of regulation this product contains Pericarpium Citri Reticulatae with Hesperidin (C
28H
34O
15) meter, must not be less than 3.0mg.
Particularly preferably, the invention provides a kind of method of quality control for the treatment of the Chinese medicine composition of gastropathy, comprising:
[discriminating]
(1) microscopical identification: get this product and put the microscopically observation: stone cell is faint yellow, similar round, polygon, rectangle, and hole ditch and cell are obvious; Fiber bunchy or loose from, diameter 8～30 μ m, wall is extremely thick, little lignify, there is longitudinal crack on the surface, and the normal lobe of the fiber broken ends of fractured bone becomes the broom shape; The fiber bunchy or loose from, colourless or fallow, more elongated, wavy or slightly present zigzag on one side usually, cell is roomy, Chang Kejian belittles tabula; It is brown to plant chrotoplast, polygon, and the wall beaded thickens;
(2) physicochemical identification of dried Alumen: get this product powder 0.5g, add dilute hydrochloric acid 10ml, fully stir, dissolving filters filtrate for later use; With platinum filament dip in get filtrate a little, in colourless flame, burn, flame promptly shows purple; Get filtrate 3ml, add ammonia solution to generating white gelatinous precipitate, drip alizarine S indicator solution number droplet, precipitation promptly shows cherry red; Other gets filtrate 5ml, adds 5 of barium chloride test solutions, promptly generates white precipitate, adds nitric acid 1ml, and precipitation is not dissolved;
(3) thin layer chromatography of Asterias amurensis Lutken is differentiated: get this product powder 2g, porphyrize adds water saturated n-butyl alcohol 5ml, and close plug soaked overnight shakes up, and filters, and filtrate is as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8 μ l, control medicinal material solution 4 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-acetone-methanol (6: 1: 2), presaturation 15 minutes, launch, take out, dry, put 120 ℃ of bakings after about 5 minutes, spray is with the ethanol solution of 5% phosphomolybdic acid, about 5 minutes of 120 ℃ of heating; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) thin layer chromatography of Pericarpium Citri Reticulatae is differentiated: get this product powder 2g, porphyrize adds methanol 10ml, and reflux 20 minutes filters, and filtrate is concentrated into about 1ml, as need testing solution; Other gets Pericarpium Citri Reticulatae (charcoal) medicinal powder 0.5g, shines medical material solution in pairs with legal system; Get the Hesperidin reference substance again, add methanol and make saturated solution, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 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, lower floor's solution with chloroform-ethyl acetate-ethanol-formic acid-water (4: 5: 2: 1: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(5) thin layer chromatography of the Radix Astragali is differentiated: get this product powder 5g, porphyrize adds methanol 60ml, reflux 1 hour filters the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, extracts 3 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, with 1% sodium hydroxide solution wash 2 times (100ml, 50ml), the water 50ml washing that the reuse n-butyl alcohol is saturated is got n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution; Other gets Radix Astragali control medicinal material 0.5g, adds methanol 30ml, shines medical material solution in pairs with legal system; Get the astragaloside reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of need testing solution 8 μ l, control medicinal material solution and reference substance solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color under the daylight; The fluorescence speckle of apparent same color under the ultraviolet light;
(6) gel electrophoresis analysis of Asterias amurensis Lutken: get this product powder 2g, porphyrize adds 6ml hot water, covers preservative film, and 100 ℃ of heating in water bath 30 minutes were put cold back 4000rpm centrifugal 20 minutes, divided and got supernatant, as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; According to electrophoresis method (2005 editions three appendix IV C of Chinese Pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution respectively, carry out the SDS-polyacrylamide gel electrophoresis by following deposition condition, promptly; In the test sample Zone electophoresis band, with the corresponding position of control medicinal material Zone electophoresis band on show the protein band of same color; Wherein said deposition condition is: resolving gel concentration 12.5%; Concentrate gum concentration 5%; Constant current 30mA; Voltage 200V; Electrophoresis time is 2 hours; With coomassie brilliant blue R250 dyeing 4 hours, the shaking table decolouring;
[assay]
(1) dried Alumen assay
Get this product, porphyrize, get about 1g, the accurate title, decide, add dilute hydrochloric acid 10ml, heated and boiled 10 minutes filters water 100ml gradation washing container and filtering residue, merge washing liquid and filtrate, add water 50ml respectively, 2 of instructions phenolphthalein solutions, 10% potassium hydroxide solution 9ml shakes up, and drips 10% potassium hydroxide solution to blush, drip dilute hydrochloric acid again to red the disappearance, add acetic acid-ammonium acetate buffer (pH4.8) 25ml, precision adds Calcium Disodium Versenate volumetric solution (0.05mol/L) 25ml again, and heating keeps little boiling 10 minutes, put and be chilled to room temperature, add 0.5% xylenol orange indicator solution 1.5ml, change into orange redly with zinc volumetric solution (0.05mol/L) titration to solution from pale brown color, and titrating result proofreaied and correct with blank assay; Every 1ml Calcium Disodium Versenate volumetric solution (0.05mol/L) is equivalent to the aluminium potassium sulfate (KAl (SO of 12.91mg
4)
2);
The every 1g of this product contains dried Alumen with aluminium potassium sulfate (KAl (SO
4)
2) meter, must not be less than 50mg;
(2) Pericarpium Citri Reticulatae assay
The preparation of reference substance solution: it is an amount of to get the Hesperidin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains Hesperidin 30 μ g, promptly;
The preparation of need testing solution: get this product, porphyrize is got about 0.5g, and accurate the title decides, put in the tool plug conical flask accurate methanol 10ml, the close plug of adding, claim to decide weight, supersound process (power 200W, 59kHz) 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 1ml, put in the 10ml measuring bottle, add methanol to scale, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water-acetic acid (30: 66: 4) is mobile phase; The detection wavelength is 283nm; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
Algoscopy: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this product contains Pericarpium Citri Reticulatae with Hesperidin (C
28H
34O
15) meter, must not be less than 3.0mg;
(3) Fructus Piperis assay
The preparation of reference substance solution: it is an amount of that precision takes by weighing the piperine reference substance, puts in the brown measuring bottle, adds dehydrated alcohol and make the solution that every 1ml contains 10 μ g, shakes up, promptly;
The preparation of need testing solution: get this product powder 3g, the accurate title, decided porphyrize, get 0.5g, the accurate title, decide, and puts in the brown measuring bottle of 50ml tool plug, add dehydrated alcohol 40ml, supersound process 30 minutes is placed to room temperature, add dehydrated alcohol and be diluted to scale, shake up, filter, discard filtrate just, collect subsequent filtrate, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler, is mobile phase with methanol-water (77: 23), and the detection wavelength is 343nm; Number of theoretical plate is pressed the piperine peak and is calculated, and should be not less than 2500;
Algoscopy: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this product contains Fructus Piperis with piperine (C
17H
19NO
3) meter, must not be less than 0.95mg.
The inventor is according to traditional Chinese medical science rule of treatment such as determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs, treatment must aim at the pathogenesis of disease, treating both the principal and the secondary aspects of a disease at the same time, utilization temperature and, disappear, tcm treatment method such as benefit, in conjunction with modern medical theory, pathogeny according to peptic ulcer, the plurality of raw materials medicine is carried out screening test, determine best proportion relation, developed this medicine.This prescription to be so that the Asterias amurensis Lutken of better antacid antiulcer action to be arranged, at symptom, and treating both the principal and secondary aspects of a disease.The pharmacodynamics test digital proof, Chinese medicine composition of the present invention has tangible curative effect aspect the anti-acute and chronic ulcer function.Case 151 examples are observed in clinical trial, and wherein 50 routine patients take pharmaceutical composition tablet of the present invention, and the ulcer healing total effective rate is 84%; 101 routine patients take pharmaceutical composition pill of the present invention, and the ulcer healing total effective rate is 89.1%.Aspect doing well,improving, medicine of the present invention has good analgesic effect, and clinical observation has no adverse reaction simultaneously.Drug combination preparation Coming-of-Age Day taking dose of the present invention is equivalent to day take crude drug amount 5.4g, divides three times one after each meal, the 4-6 week course of treatment.
The present invention remedies the deficiencies in the prior art, improve the quality control standard of such medicine, 1. monarch drug composition Asterias amurensis Lutken derives from the end the dry all of reptile Asteriidae animal of dwelling in this prescription, in recent years, the research of relevant Asterias amurensis Lutken active component and pharmacologically active receives concern both domestic and external day by day, Asterias amurensis Lutken not only contains saponin, sterol, compositions such as alkaloid, also be rich in multiple proteins, aminoacid ingredient, the present invention adopts sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE electrophoresis method) that the contained protein component of Asterias amurensis Lutken is carried out qualitative identification, adopt the Asterias amurensis Lutken control medicinal material, and exclusive through methodology test confirmation method, feasible, negative noiseless; 2. the present invention has increased the thin layer chromatography qualitative identification method of the Radix Astragali, adopts Radix Astragali control medicinal material, and is exclusive, feasible, negative noiseless through methodology test confirmation method; 3. the present invention increases the content assaying method of another monarch drug composition dried Alumen in the prescription, and aluminium potassium sulfate is the main active of dried Alumen, and the present invention utilizes the content of aluminium potassium sulfate in this medicine of chemical titration, and the result is accurate, favorable reproducibility; 4. the present invention increases the content assaying method of Pericarpium Citri Reticulatae, Hesperidin content in Pericarpium Citri Reticulatae is abundant, it is the main active of Pericarpium Citri Reticulatae, the present invention utilizes Determination of Hesperidin Content in this medicine of high effective liquid chromatography for measuring, method is easy, the result is accurate, favorable reproducibility, and through methodology test affirmation negative noiseless (collection of illustrative plates is arranged).
Description of drawings
Fig. 1 represents is Asterias amurensis Lutken thin-layer chromatogram (1, sample solution 2, Asterias amurensis Lutken control medicinal material solution 3, negative control solution).
Fig. 2 represents is Pericarpium Citri Reticulatae thin-layer chromatogram (1, sample solution 2, Hesperidin reference substance solution 3, Pericarpium Citri Reticulatae (charcoal) control medicinal material solution 4, negative control solution).
Fig. 3 represents is Asterias amurensis Lutken gel electrophoresis spectrogram (1, negative control solution 2, sample solution 3, Asterias amurensis Lutken control medicinal material solution).
What Fig. 4 represented is Hesperidin reference substance high-efficient liquid phase chromatogram.
What Fig. 5 represented is medicine test sample high-efficient liquid phase chromatogram of the present invention.
What Fig. 6 represented is medicine Pericarpium Citri Reticulatae negative sample high-efficient liquid phase chromatogram of the present invention.
What Fig. 7 represented is piperine reference substance high-efficient liquid phase chromatogram.
What Fig. 8 represented is medicine test sample high-efficient liquid phase chromatogram of the present invention
What Fig. 9 represented is medicine Fructus Piperis negative sample high-efficient liquid phase chromatogram of the present invention.
The specific embodiment
Further describe exploitativeness of the present invention below by embodiment; for a person skilled in the art; should be understood to, the following examples are not limiting the scope of the invention, and the replacement that is equal to of some technical characterictic is still belonged to protection scope of the present invention.
Prescription: Asterias amurensis Lutken 600g dried Alumen 150g Pericarpium Citri Reticulatae (charcoal) 300g
Concha Arcae (forging) 300g Concha Ostreae (forging) the 300g Rhizoma Atractylodis Macrocephalae (stir-fry) 300g
Radix Astragali 300g Rhizoma Zingiberis 300g Fructus Piperis 150g
Method for making: it is standby to take by weighing described materials of weight proportions medicine; Asterias amurensis Lutken put in the steam pot steamed dry for standby two hours; Above nine flavor medicine mixed powders are broken into fine powder, cross 150 mesh sieves; Fully mix homogeneously gets mixture; Said mixture is added an amount of magnesium stearate, be pressed into plain sheet, make 9000 altogether, the bag film-coat, promptly.
Prescription: Asterias amurensis Lutken 700g dried Alumen 200g Pericarpium Citri Reticulatae (charcoal) 300g
Concha Arcae (forging) 300g Concha Ostreae (forging) the 300g Rhizoma Atractylodis Macrocephalae (stir-fry) 300g
Radix Astragali 250g Rhizoma Zingiberis 300g Fructus Piperis 150g
Method for making: it is standby to take by weighing described materials of weight proportions medicine; Asterias amurensis Lutken put in the steam pot steamed dry for standby two hours; Above nine flavor medicine mixed powders are broken into fine powder, cross 200 mesh sieves; Fully mix homogeneously gets mixture; Said mixture is packed in the hard capsule, make 9000 altogether, promptly.
Prescription: Asterias amurensis Lutken 1500g dried Alumen 300g Pericarpium Citri Reticulatae (charcoal) 600g
Concha Arcae (forging) 600g Concha Ostreae (forging) the 600g Rhizoma Atractylodis Macrocephalae (stir-fry) 600g
Radix Astragali 600g Rhizoma Zingiberis 600g Fructus Piperis 150g
Method for making: it is standby to take by weighing described materials of weight proportions medicine; Asterias amurensis Lutken put in the steam pot steamed dry for standby two hours; Above nine flavor medicine mixed powders are broken into fine powder, cross 200 mesh sieves; Fully mix homogeneously gets mixture; Said mixture is added an amount of amylum pregelatinisatum, make pill, promptly.
The tablet that embodiment 1 is made carries out quality inspection.
[discriminating]
(1) microscopical identification: get this product and put the microscopically observation: stone cell is faint yellow, similar round, polygon, rectangle, and hole ditch and cell are obvious; Fiber bunchy or loose from, diameter 8～30 μ m, wall is extremely thick, little lignify, there is longitudinal crack on the surface, and the normal lobe of the fiber broken ends of fractured bone becomes the broom shape; The fiber bunchy or loose from, colourless or fallow, more elongated, wavy or slightly present zigzag on one side usually, cell is roomy, Chang Kejian belittles tabula; It is brown to plant chrotoplast, polygon, and the wall beaded thickens;
(2) physicochemical identification of dried Alumen: get 2 of this product, remove coating, porphyrize adds dilute hydrochloric acid 10ml, fully stirs, and dissolving filters filtrate for later use; With platinum filament dip in get filtrate a little, in colourless flame, burn, flame promptly shows purple; Get filtrate 3ml, add ammonia solution to generating white gelatinous precipitate, drip alizarine S indicator solution number droplet, precipitation promptly shows cherry red; Other gets filtrate 5ml, adds 5 of barium chloride test solutions, promptly generates white precipitate, adds nitric acid 1ml, and precipitation is not dissolved;
(3) thin layer chromatography of Asterias amurensis Lutken is differentiated: get 7 of this product, remove coating, porphyrize adds water saturated n-butyl alcohol 5ml, and close plug soaked overnight shakes up, and filters, and filtrate is as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 8 μ l, control medicinal material solution 4 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-acetone-methanol (6: 1: 2), presaturation 15 minutes, launch, take out, dry, put 120 ℃ of bakings after about 5 minutes, spray is with the ethanol solution of 5% phosphomolybdic acid, about 5 minutes of 120 ℃ of heating; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) thin layer chromatography of Pericarpium Citri Reticulatae is differentiated: get 7 of this product, remove coating, porphyrize adds methanol 10ml, and reflux 20 minutes filters, and filtrate is concentrated into about 1ml, as need testing solution; Other gets Pericarpium Citri Reticulatae (charcoal) medicinal powder 0.5g, shines medical material solution in pairs with legal system; Get the Hesperidin reference substance again, add methanol and make saturated solution, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 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, lower floor's solution with chloroform-ethyl acetate-ethanol-formic acid-water (4: 5: 2: 1: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(5) thin layer chromatography of the Radix Astragali is differentiated: get 15 of this product, remove coating, porphyrize, add methanol 60ml, reflux 1 hour filters, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracts 3 times with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, with 2 (100ml of 1% sodium hydroxide solution washing, 50ml), n-butyl alcohol liquid is got in the water 50ml washing that the reuse n-butyl alcohol is saturated, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Astragali control medicinal material 0.5g, adds methanol 30ml, shines medical material solution in pairs with legal system; Get the astragaloside reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of need testing solution 8 μ l, control medicinal material solution and reference substance solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts respectively under daylight and the ultra-violet lamp (365nm) and inspects; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color under the daylight; The fluorescence speckle of apparent same color under the ultraviolet light;
(6) gel electrophoresis analysis of Asterias amurensis Lutken: get 7 of this product, remove coating, porphyrize adds 6ml hot water, covers preservative film, and 100 ℃ of heating in water bath 30 minutes were put cold back 4000rpm centrifugal 20 minutes, divided and got supernatant, as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; According to electrophoresis method (2005 editions three appendix IV C of Chinese Pharmacopoeia) test, draw each 10 μ l of above-mentioned two kinds of solution respectively, carry out the SDS-polyacrylamide gel electrophoresis by following deposition condition, promptly; In the test sample Zone electophoresis band, with the corresponding position of control medicinal material Zone electophoresis band on show the protein band of same color; Wherein said deposition condition is: resolving gel concentration 12.5%; Concentrate gum concentration 5%; Constant current 30mA; Voltage 200V; Electrophoresis time is 2 hours; With coomassie brilliant blue R250 dyeing 4 hours, the shaking table decolouring;
[assay]
(1) dried Alumen assay
It is an amount of to get this product, remove coating, porphyrize, get about 1g, the accurate title, decide, and adds dilute hydrochloric acid 10ml, heated and boiled 10 minutes, filter, water 100ml gradation washing container and filtering residue merge washing liquid and filtrate, add water 50ml respectively, 2 of instructions phenolphthalein solutions, 10% potassium hydroxide solution 9ml, shake up, drip 10% potassium hydroxide solution to blush, drip dilute hydrochloric acid again to red the disappearance, add acetic acid-ammonium acetate buffer (pH4.8) 25ml, precision adds Calcium Disodium Versenate volumetric solution (0.05mol/L) 25ml again, heating keeps little boiling 10 minutes, puts and is chilled to room temperature, adds 0.5% xylenol orange indicator solution 1.5ml, change into orange redly with zinc volumetric solution (0.05mol/L) titration to solution from pale brown color, and titrating result proofreaied and correct with blank assay; Every 1ml Calcium Disodium Versenate volumetric solution (0.05mol/L) is equivalent to the aluminium potassium sulfate (KAl (SO of 12.91mg
4)
2);
The every 1g of this product contains dried Alumen with aluminium potassium sulfate (KAl (SO
4)
2) meter, be 60mg;
(2) Pericarpium Citri Reticulatae assay
The preparation of reference substance solution: it is an amount of to get the Hesperidin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains Hesperidin 30 μ g, promptly;
The preparation of need testing solution: it is an amount of to get this product, removes coating, and porphyrize is got about 0.5g, the accurate title, decide, and puts in the tool plug conical flask, accurate methanol 10ml, the close plug of adding, claim to decide weight, supersound process (power 200W, 59kHz) 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 1ml, put in the 10ml measuring bottle, add methanol to scale, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With acetonitrile-water-acetic acid (30: 66: 4) is mobile phase; The detection wavelength is 283nm; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
Algoscopy: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this product contains Pericarpium Citri Reticulatae with Hesperidin (C
28H
34O
15) meter, be 3.7mg;
(3) Fructus Piperis assay
The preparation of reference substance solution: it is an amount of that precision takes by weighing the piperine reference substance, puts in the brown measuring bottle, adds dehydrated alcohol and make the solution that every 1ml contains 10 μ g, shakes up, promptly;
The preparation of need testing solution: it is an amount of to get this product, removes coating, gets 3g, porphyrize, the accurate title, decide, and gets 0.5g, the accurate title, decide, and puts in the brown measuring bottle of 50ml tool plug, adds dehydrated alcohol 40ml, supersound process 30 minutes is placed to room temperature, adds dehydrated alcohol and is diluted to scale, shake up, filter, discard filtrate just, collect subsequent filtrate, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler, is mobile phase with methanol-water (77: 23), and the detection wavelength is 343nm; Number of theoretical plate is pressed the piperine peak and is calculated, and should be not less than 2500;
Algoscopy: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005); Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this product contains Fructus Piperis with piperine (C
17H
19NO
3) meter, be 1.1mg.
Below by testing the beneficial effect of further setting forth medicine of the present invention, these tests comprise the pharmacodynamics test and the clinical trial of medicine of the present invention.
Pharmacodynamics test
Medicine of the present invention has replenishing QI to invigorate the spleen, and the function of warming middle-JIAO to relieve pain has tangible curative effect to gastric and duodenal ulcers etc.The inventor cures mainly according to its function, studying aspect the anti-acute and chronic ulcer function, so that its beneficial effect to be described.
Laboratory animal: Wistar rat, body weight 180-220g, male and female half and half.Provide by animal housing of Dalian Medical Univ.
Experimental drug: get tablet that embodiment 1 makes as the experiment medicine, be assigned to desired concn with distilled water during experiment.
All through " t " check, the result represents with X ± SD in statistical result.As adopting other method of inspection, other adds dated.
One, medicine of the present invention is to the inhibitory action of stress gastric ulcer
Get 40 of rats, be divided into 4 groups at random by body weight, press gastric infusion every day of dosage shown in the table 1 once, matched group gavages the equivalent distilled water, and successive administration 3 days begins fasting after administration in first day, can't help water, used etherization in 1 hour after the last administration, rat is tied up on fixing head, after head is placed 16 hours downward vertically, the dislocation of cervical vertebra method is put to death, dissect immediately, ligation cardia, pylorus, and inject 10% neutral formalin 10ml to gastric, the extraction stomach also is dipped in 10% neutral formalin, take out after 20 minutes, cut off and pave, check the gastric pathological changes along greater gastric curvature.
Observation caliber is with reference to Adamis improved method in " medical experiment animal model and cell line development and Application ", and quantitative criteria sees Table 2.
The inhibitory action of table 1 pair stress gastric ulcer
| Group | Number of animals (only) | Dosage (g/kg) | Ulcer progression | Suppression ratio (%) |
| Matched |
10 | --- | 3.5±0.2 | --- |
| Medicine of the |
10 | 0.5 | 3.0±0.3 | 14.3 |
| Medicine of the |
10 | 1.5 | 2.6±0.3 ** | 25.7 |
| Medicine of the |
10 | 2.0 | 2.5±0.3 ** | 28.6 |
Compare with matched group
*P＜0.01
The criterion of table 2 gastric ulcer and quantification score value table
| The ulcer rank | Criterion | |
| 0 | No pathological changes. | 0 |
| I | Hemorrhage, erosion or ulcer point (d＜1mm). | 1 |
| II | 1～5 aphtha (1mm＜d＜3mm) is arranged. | 2 |
| III | 6 above aphthas or big ulcer (d＞3mm) is arranged. | 3 |
| IV | Big ulcer more than 2 is arranged. | 4 |
| V | Perforation is arranged. | 5 |
Two, medicine of the present invention causes the inhibitory action of gastric ulcer to pylorus ligation
Get 40 of rats, be divided into 4 groups at random by body weight, press gastric infusion every day of dosage shown in the table 3 once, matched group gavages the equivalent distilled water, and successive administration 3 days begins fasting after administration in first day, can't help water, ligation pylorus after 4 hours after the last administration, and behind pylorus ligation, made the dislocation of cervical vertebra method in 17 hours and put to death, dissect immediately.Collect whole gastric juice, measure acid concentration and pepsin activity, inject 10% neutral formalin 10ml to gastric immediately behind the taking-up gastric juice, the extraction stomach also is dipped in 10% neutral formalin, take out after 20 minutes and cut open, evaluation gastric ulcer grade, quantitative criteria sees Table 2.Experimental result sees Table 3 and table 4.
Ligation pylorus gastric ulcer production behind the table 3 filling stomach
| Group | Number of animals (only) | Dosage (g/kg) | Ulcer progression | Suppression ratio (%) |
| Matched |
10 | --- | 3.2±0.7 | --- |
| Medicine of the |
10 | 0.5 | 1.3±0.3 ** | 59.4 |
| Medicine of the |
10 | 1.5 | 1.1±0.3 ** | 65.6 |
| Medicine of the |
10 | 2.0 | 1.1±0.3 ** | 65.6 |
Compare with matched group
*P＜0.01
Ligation pylorus gastric juice changed after table 4 was irritated stomach
| Group | Number of animals (only) | Dosage (g/kg) | Gastric juice amount (ml) | Stomach total acidity (mmo l) | Pepsin (u/ml) |
| Matched |
10 | --- | 13.2±1.0 | 141.1±10.4 | 3.6±0.2 |
| Medicine of the |
10 | 0.5 | 11.8±1.1* | 100.0±4.9* | 2.9±0.2* |
| Medicine of the |
10 | 1.5 | 9.3±0.8* | 93.5±8.8* | 2.2±0.3* |
| Medicine of the |
10 | 2.0 | 9.1±0.9* | 90.7±3.4* | 2.3±0.3* |
Compare with matched group
*P＜0.05
Three, medicine Dichlorodiphenyl Acetate method of the present invention causes the therapeutical effect of gastric ulcer
Get 40 of rats, fasting is 24 hours before the art, freely drinks water, use the pentobarbital lumbar injection, cut open the belly after the anesthesia, under the serous coat of microsyringe the nearly excess of the stomach of the outside of belly district of 20% acetic acid 0.012ml injection stomach, wipe away only with the normal saline cotton balls then, postoperative is divided into 5 groups at random with rat, begins by table 5 dosage gastric infusion every day once from second day after operation, and matched group gavages the equivalent distilled water, successive administration 5 days, the difference gastric infusion, the last administration was put to death rat after 3 days, observed its ulcer situation.
Table 5 Dichlorodiphenyl Acetate method causes the therapeutical effect of gastric ulcer
| Group | Number of animals (only) | Dosage (g/kg) | Ulcer area (mm 2) | Suppression ratio (%) |
| Matched |
10 | --- | ?20.5±2.2 | --- |
| Medicine of the |
10 | 0.5 | ?8.9±1.7 ** | 56.6 |
| Medicine of the |
10 | 1.5 | ?7.6±1.3 ** | 37.1 |
| Medicine of the |
10 | 2.0 | ?7.2±1.5 ** | 35.1 |
Compare with matched group
*P＜0.01
Get the tablet that embodiment 1 makes and carry out clinical trial
Table 6 gastroscope criterion
| Clinical cure | Ulcer heals fully and reaches S1 more than the phase, and the part is slightly rubescent, does not have obvious edema. |
| Produce effects | The ulcer size reduction is more than 50%. |
| Effectively | Ulcer size reduction, but less than 50%. |
| Invalid | No change. |
Table 7 is used medicinal tablet treatment of the present invention back tcm symptom efficacy analysis
The gastroscope result relatively before and after table 8 treatment
| The example number | Clinical cure (%) | Produce effects (%) | Effectively (%) | Invalid (%) | Total effective rate (%) |
| 50 | 44 | 20 | 12 | 16 | 84 |
Get the pill that embodiment 3 makes and carry out clinical trial
Clinical observation 101 routine patients are and are in hospital or the special outpatient clinic patient, are diagnosed as active stage ulcer through gastroscopy, and the Chinese medical discrimination typing meets gastric abscess (asthenic cold type).Each 1 bag of oral meal (2g), every day three times, be 4 weeks medicine time, carries out traditional Chinese medical science four diagnostic methods dialectical Analyses and fibergastroscopy after 4 weeks, the gastroscope criterion sees Table 1.In the 101 routine cases, symptoms such as in various degree pain, nausea and vomiting, acid regurgitation, abdominal distention are arranged all, take behind the medicine of the present invention pain 60 examples that disappear, 31 examples that take a turn for the better, total effective rate is 91%.The gastroscopy result shows, clinical cure 51 examples aspect the promotion ulcer healing, and produce effects 21 examples, effective 18 examples, total effective rate is 89.1%.
Table 9 is used bolus of drug treatment of the present invention back tcm symptom efficacy analysis
The gastroscope result relatively before and after table 10 treatment
| The example number | Clinical cure (%) | Produce effects (%) | Effectively (%) | Invalid (%) | Total effective rate (%) |
| 101 | 50.5 | 20.8 | 17.8 | 10.9 | 89.1 |
Claims (11)
1. Chinese medicine composition for the treatment of gastropathy is characterized in that this Chinese medicine composition is by comprising that following bulk drugs makes:
4 parts of 2 parts of Pericarpium Citri Reticulataes of 8 parts of Alumens of Asterias amurensis Lutken
4 parts of 4 parts of Rhizoma Atractylodis Macrocephalaes of 4 portions of Concha Ostreaes of Concha Arcae
2 parts in 4 portions of Fructus Piperiss of 4 portions of Rhizoma Zingiberiss of the Radix Astragali.
2. Chinese medicine composition according to claim 1 is randomly made tablet, pill, granule or capsule.
3. the preparation method of Chinese medicine composition as claimed in claim 1 or 2 comprises the steps:
(1) it is standby to take by weighing described materials of weight proportions medicine;
(2) Asterias amurensis Lutken is put 1 to 4 hour dry for standby of steaming in the steam pot;
(3) above nine flavor medicine mixed powders are broken into fine powder, cross the 100-300 mesh sieve; Fully mix homogeneously gets mixture;
(4) said mixture is added acceptable accessories, make required dosage form by rules of preparations.
4. preparation method according to claim 3 wherein in the step (2) is put Asterias amurensis Lutken and is steamed 2 hours dry for standby in the steam pot.
5. the detection method of Chinese medicine composition as claimed in claim 1 or 2 comprises the following steps one or more kinds of combinations: the thin layer discriminating of the Radix Astragali, the discriminating of Asterias amurensis Lutken gel electrophoresis, dried Alumen assay and Pericarpium Citri Reticulatae assay.
6. method according to claim 5, the thin layer of the wherein said Radix Astragali are differentiated and are: get this product powder 5g, porphyrize, add methanol 60ml, reflux 1 hour filters, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracts 2-4 time with water saturated n-butyl alcohol jolting, each 20ml merges n-butyl alcohol liquid, with 1% sodium hydroxide solution washing 1-3 time, the water 50ml washing that the reuse n-butyl alcohol is saturated is got n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution; Other gets Radix Astragali control medicinal material 0.5g, adds methanol 30ml, shines medical material solution in pairs with legal system; Get the astragaloside reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw each 5 μ l of need testing solution 8 μ l, control medicinal material solution and reference substance solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color under the daylight; The fluorescence speckle of apparent same color under the ultraviolet light.
7. detection method according to claim 6, wherein the volume ratio of chloroform-methanol-water is 13: 7: 2.
8. detection method according to claim 5, wherein, the gel electrophoresis of Asterias amurensis Lutken is differentiated and is: get this product powder 2g, porphyrize, add 6ml hot water, cover preservative film, 100 ℃ heating in water bath 10-60 minute, put cold back centrifugalize, divide and get supernatant, as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; According to the test of 2005 editions three appendix IV C of Chinese Pharmacopoeia electrophoresis method, draw each 10 μ l of above-mentioned two kinds of solution respectively, carry out the SDS-polyacrylamide gel electrophoresis by following deposition condition, promptly; In the test sample Zone electophoresis band, with the corresponding position of control medicinal material Zone electophoresis band on show the protein band of same color; Described deposition condition is: resolving gel concentration 12.5%; Concentrate gum concentration 5%; Constant current 30mA; Voltage 200V; Electrophoresis time is 2 hours; With coomassie brilliant blue R250 dyeing 4 hours, the shaking table decolouring.
9. detection method according to claim 5, wherein, the content assaying method of described dried Alumen is: get this product, porphyrize is got 1g, and accurate the title decides, add dilute hydrochloric acid 10ml, heated 5-30 minute, and filtered water 100ml gradation washing container and filtering residue, merge washing liquid and filtrate, add water 50ml respectively, 2 of instructions phenolphthalein solutions, 10% potassium hydroxide solution 9ml shakes up, and drips 10% potassium hydroxide solution to blush, drip dilute hydrochloric acid again to red the disappearance, acetic acid-the ammonium acetate buffer that adds 25ml pH4.8, to add 25ml concentration be 0.05mol/L Calcium Disodium Versenate volumetric solution to precision again, heating keeps little boiling 10 minutes, put and be chilled to room temperature, add 0.5% xylenol orange indicator solution 1.5ml, it is orange red to be with concentration that 0.05mol/L zinc volumetric solution titration to solution changes into from pale brown color, and titrating result is proofreaied and correct with blank assay; The aluminium potassium sulfate that every 1ml Calcium Disodium Versenate volumetric solution is equivalent to 12.91mg is KAl (SO
4)
2And the every 1g of regulation this product to contain dried Alumen be KAl (SO with aluminium potassium sulfate
4)
2Meter must not be less than 50mg.
10. detection method according to claim 5, wherein, the assay of described Pericarpium Citri Reticulatae is:
The preparation of reference substance solution: get the Hesperidin reference substance, the accurate title, decide, and adds methanol and make the solution that every 1ml contains Hesperidin 30 μ g, promptly;
The preparation of need testing solution: get this product, porphyrize is got about 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 10ml that adds, close plug claims to decide weight, supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 1ml, put in the 10ml measuring bottle, add methanol to scale, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With volume ratio is that 30: 66: 4 acetonitrile-water-acetic acid is mobile phase; The detection wavelength is 283nm, and number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
Algoscopy: according to an appendix VID of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; And the every 1g of regulation this product contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 3.0mg.
11. the detection method of a Chinese medicine composition as claimed in claim 1 or 2 comprises:
[discriminating]
(1) microscopical identification: get this product and put the microscopically observation: stone cell is faint yellow, similar round, polygon, rectangle, and hole ditch and cell are obvious; Fiber bunchy or loose from, diameter 8～30 μ m, wall is extremely thick, little lignify, there is longitudinal crack on the surface, and the normal lobe of the fiber broken ends of fractured bone becomes the broom shape; The fiber bunchy or loose from, colourless or fallow, more elongated, wavy or slightly present zigzag on one side usually, cell is roomy, Chang Kejian belittles tabula; It is brown to plant chrotoplast, polygon, and the wall beaded thickens;
(2) physicochemical identification of dried Alumen: get this product powder 0.5g, add dilute hydrochloric acid 10ml, fully stir, dissolving filters filtrate for later use; With platinum filament dip in get filtrate a little, in colourless flame, burn, flame promptly shows purple; Get filtrate 3ml, add ammonia solution to generating white gelatinous precipitate, drip alizarine S indicator solution number droplet, precipitation promptly shows cherry red; Other gets filtrate 5ml, adds 5 of barium chloride test solutions, promptly generates white precipitate, adds nitric acid 1ml, and precipitation is not dissolved;
(3) thin layer chromatography of Asterias amurensis Lutken is differentiated: get this product powder 2g, porphyrize adds water saturated n-butyl alcohol 5ml, and close plug soaked overnight shakes up, and filters, and filtrate is as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw need testing solution 8 μ l, control medicinal material solution 4 μ l, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with chloroform-acetone of 6: 1: 2 of volume ratio-methanol, presaturation 15 minutes, launch, take out, dry, put 120 ℃ of bakings after about 5 minutes, spray is with the ethanol solution of 5% phosphomolybdic acid, about 5 minutes of 120 ℃ of heating; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(4) thin layer chromatography of Pericarpium Citri Reticulatae is differentiated: get this product powder 2g, porphyrize adds methanol 10ml, and reflux 20 minutes filters, and filtrate is concentrated into about 1ml, as need testing solution; Other gets Pericarpium Citri Reticulatae charcoal drug material powder 0.5g, shines medical material solution in pairs with legal system; Get the Hesperidin reference substance again, add methanol and make saturated solution, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw each 10 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, with volume ratio is 4: 5: 2: lower floor's solution of 1: 1 chloroform-ethyl acetate-ethanol-formic acid-water is developing solvent, launch, take out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with the aluminum chloride test solution; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(5) thin layer chromatography of the Radix Astragali is differentiated: get this product powder 5g, porphyrize adds methanol 60ml, reflux 1 hour filters the filtrate evaporate to dryness, residue adds water 15ml makes dissolving, extracts 3 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, with 1% sodium hydroxide solution washing 2 times, 100ml and 50ml, the water 50ml washing that the reuse n-butyl alcohol is saturated is got n-butyl alcohol liquid, evaporate to dryness, residue adds methanol 2ml makes dissolving, as need testing solution; Other gets Radix Astragali control medicinal material 0.5g, adds methanol 30ml, shines medical material solution in pairs with legal system; Get the astragaloside reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin layer chromatography, draw each 5 μ l of need testing solution 8 μ l, control medicinal material solution and reference substance solution, put respectively on same silica gel g thin-layer plate, lower floor's solution of placing below 10 ℃ with chloroform-methanol-water of 13: 7: 2 of volume ratio is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, puts respectively under daylight and the 365nm ultra-violet lamp and inspects; In the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, the speckle of apparent same color under the daylight; The fluorescence speckle of apparent same color under the ultraviolet light;
(6) gel electrophoresis analysis of Asterias amurensis Lutken: get this product powder 2g, porphyrize adds 6ml hot water, covers preservative film, and 100 ℃ of heating in water bath 30 minutes were put cold back 4000rpm centrifugal 20 minutes, divided and got supernatant, as need testing solution; Other gets Asterias amurensis Lutken control medicinal material 1g, shines medical material solution in pairs with legal system; According to the test of 2005 editions three appendix IV C of Chinese Pharmacopoeia electrophoresis method, draw each 10 μ l of above-mentioned two kinds of solution respectively, carry out the SDS-polyacrylamide gel electrophoresis by following deposition condition, promptly; In the test sample Zone electophoresis band, with the corresponding position of control medicinal material Zone electophoresis band on show the protein band of same color; Wherein said deposition condition is: resolving gel concentration 12.5%; Concentrate gum concentration 5%; Constant current 30mA; Voltage 200V; Electrophoresis time is 2 hours; With coomassie brilliant blue R250 dyeing 4 hours, the shaking table decolouring;
[assay]
(1) dried Alumen assay
Get this product, porphyrize, get about 1g, the accurate title, decide, add dilute hydrochloric acid 10ml, heated and boiled 10 minutes filters water 100ml gradation washing container and filtering residue, merge washing liquid and filtrate, add water 50ml respectively, 2 of instructions phenolphthalein solutions, 10% potassium hydroxide solution 9ml shakes up, and drips 10% potassium hydroxide solution to blush, drip dilute hydrochloric acid again to red the disappearance, add 25ml pH4.8 acetic acid-ammonium acetate buffer, precision adds 25ml 0.05mol/L Calcium Disodium Versenate volumetric solution again, and heating keeps little boiling 10 minutes, put and be chilled to room temperature, add 0.5% xylenol orange indicator solution 1.5ml, change into orange redly with 0.05mol/L zinc volumetric solution titration to solution from pale brown color, and titrating result proofreaied and correct with blank assay; Every 1ml Calcium Disodium Versenate volumetric solution is equivalent to the aluminium potassium sulfate KAl (SO of 12.91mg
4)
2
The every 1g of this product contains dried Alumen with aluminium potassium sulfate KAl (SO
4)
2Meter must not be less than 50mg;
(2) Pericarpium Citri Reticulatae assay
The preparation of reference substance solution: it is an amount of to get the Hesperidin reference substance, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains Hesperidin 30 μ g, promptly;
The preparation of need testing solution: get this product, porphyrize is got about 0.5g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 10ml that adds, close plug claimed to decide weight, with power 200W, 59kHz supersound process 30 minutes, put coldly, claim again to decide weight, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 1ml, put in the 10ml measuring bottle, add methanol to scale, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler; With 30: 66: 4 acetonitrile-water-acetic acid of volume ratio is mobile phase; The detection wavelength is 283nm; Number of theoretical plate calculates by the Hesperidin peak should be not less than 2000;
Algoscopy: according to an appendix VID of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this product contains Pericarpium Citri Reticulatae with Hesperidin C
28H
34O
15Meter must not be less than 3.0mg;
(3) Fructus Piperis assay
The preparation of reference substance solution: it is an amount of that precision takes by weighing the piperine reference substance, puts in the brown measuring bottle, adds dehydrated alcohol and make the solution that every 1ml contains 10 μ g, shakes up, promptly;
The preparation of need testing solution: get this product powder 3g, the accurate title, decided porphyrize, get 0.5g, the accurate title, decide, and puts in the brown measuring bottle of 50ml tool plug, add dehydrated alcohol 40ml, supersound process 30 minutes is placed to room temperature, add dehydrated alcohol and be diluted to scale, shake up, filter, discard filtrate just, collect subsequent filtrate, promptly;
Chromatographic condition: with the octadecylsilane chemically bonded silica is filler, is mobile phase with 77: 23 methanol-water of volume ratio, and the detection wavelength is 343nm; Number of theoretical plate is pressed the piperine peak and is calculated, and should be not less than 2500;
Algoscopy: according to an appendix VID of Chinese Pharmacopoeia version in 2005 high effective liquid chromatography for measuring; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this product contains Fructus Piperis with piperine C
17H
19NO
3Meter must not be less than 0.95mg.
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| CN101865926B (en) * | 2010-06-13 | 2013-09-11 | 云南中医学院 | Detection method for trace protein of Chinese medicinal injection |
| CN101975845A (en) * | 2010-09-21 | 2011-02-16 | 成都中医药大学 | Automatic detecting system for quality of traditional Chinese medicines |
| CN102228477A (en) * | 2011-07-04 | 2011-11-02 | 沈阳药科大学 | Application of starfish extract to preparation of medicament for treating digestive system diseases |
| CN102621268B (en) * | 2012-02-17 | 2015-02-18 | 亚宝药业集团股份有限公司 | Quality detection method for spleen-invigorating, cold-dispersing and antidiarrheal medicine composition |
| CN110702840B (en) * | 2019-10-14 | 2022-06-07 | 河北地质大学华信学院 | Analysis device based on energy utilization rate of carbonized urban domestic sewage biomass |
| CN114166958B (en) * | 2021-10-29 | 2024-03-29 | 合肥创新医药技术有限公司 | Detection method of fingerprint of traditional Chinese medicine compound herba xanthil stomach-calming particles and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1895629A (en) * | 2006-05-05 | 2007-01-17 | 张军 | Chinese-medicinal composition for treating gastropathy |
| CN101062221A (en) * | 2007-05-16 | 2007-10-31 | 刘忠文 | Medicine for treating gastric ulcer and duodenal ulcer |
| CN101130030A (en) * | 2007-08-20 | 2008-02-27 | 闫位国 | Medicine composition for treating nephropathy and uses of the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1895629A (en) * | 2006-05-05 | 2007-01-17 | 张军 | Chinese-medicinal composition for treating gastropathy |
| CN101062221A (en) * | 2007-05-16 | 2007-10-31 | 刘忠文 | Medicine for treating gastric ulcer and duodenal ulcer |
| CN101130030A (en) * | 2007-08-20 | 2008-02-27 | 闫位国 | Medicine composition for treating nephropathy and uses of the same |
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