CN105395662A - Traditional Chinese medicine composition for treating bacillary dysentery and preparing method and quality control method thereof - Google Patents
Traditional Chinese medicine composition for treating bacillary dysentery and preparing method and quality control method thereof Download PDFInfo
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/484—Glycyrrhiza (licorice)
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/75—Rutaceae (Rue family)
- A61K36/752—Citrus, e.g. lime, orange or lemon
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention discloses a traditional Chinese medicine composition for treating bacillary dysentery and a preparing method and quality control method thereof. The traditional Chinese medicine composition is prepared from andrographis paniculata, picrasma quassioides, pericarpium citri reticulatae and liquorice. The traditional Chinese medicine composition can clear away heat and toxic materials and eliminate dampness and dysentery, and can be used for treating bacillary dysentery, acute enteritis and various acute infectious diseases.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof, particularly a kind of Chinese medicine composition, its preparation method and method of quality control thereof for the treatment of bacillary dysentery.
Background technology
Bacillary dysentery (bacillarydysentery), be the common acute infectious intestinal disease caused by dysentery bacterium, with colon suppurative inflammation for major lesions, have systemic toxicity profiles symptom, stomachache, diarrhoea, tenesmus, the clinical manifestations such as evacuation of pus hemafecia.Severe patient can be fainted from fear, goes into a coma, be suffered a shock.Annual morbidity, the most common with summer, season in autumn two.
Clinical symptoms is because entering the dysentery bacterium bacterial type difference of human body, and quantity and everyone resistance difference, so symptom is also different, be therefore divided into acute chronic two kinds clinically by dysentery.Acute dysentery is divided into again light-duty according to symptom, plain edition, heavy and toxic type 4 kinds, in toxic type, be divided into again shock type and brain type according to the state of an illness, although the head of a family need not carry out strict typing to the patient's condition of child, should be appreciated that the fundamental symptoms of dysentery and the final result of change of illness state.Walking dysentery is one the lightest in dysentery, generally only has slight stomachache, diarrhoea, stool every day 2-4 time, in water sample or pasty state, without pus and blood, mixed mucus sometimes, solution is suffered from abdominal pain alleviation after an action of the bowels, majority does not generate heat or only has low grade fever, due to atypical symptom, is usually misdiagnosed as general enteritis.Plain edition has the dysentery symptom compared with allusion quotation, has heating, and body temperature can up to about 39 DEG C, indivedual child can up to more than 40 DEG C, and starting can without stomachache, diarrhoea, only have nauseating, vomiting, the symptoms such as headache, therefore, start often to be misdiagnosed as heavy cold, start after a few hours to occur paroxysmal abdominal pain, diarrhoea, starts, for loose stool, then to occur bloody purulent stool, because now ulcer and necrosis have appearred in intestinal mucosa, therefore there is obvious bearing down.Lying-down dysentery onset is anxious, and have high heat, every day, times of defecation can reach 20-30 time, and stool is in sanguinopurulent, and amount is few, and stomachache is violent, drops heavier, does not even want to leave closet, coolness of extremities, occur dehydrating phenomena very soon, the occurred disturbance of consciousness had.Toxic dysentery is more common in the child in 2-7 year, normal sudden onset, high heat is only had during beginning, body temperature can reach 40 DEG C, lethargy, complexion is steel gray, lip fingernail is livid purple, often there is decorative pattern in skin, breathe shallow and weak, can repeatedly occur fainting from fear, most children is not suffered from abdominal pain, diarrhoea and vomiting, minority child only has slight stomachache, diarrhoea, stool is without pus and blood, except above-mentioned symptom, if what occur shock symptom is shock type, show as pulse thin and delicate, blood pressure drops or do not measure, oliguria or anuria, there is dyspnea, spitting of blood phenomenon, can be dead because there is heart failure, if occur, brain symptom is brain type, the main manifestations of brain type is fidgety, drowsiness, blood pressure is normal or increase, there is severe headache, frequent vomiting, tachypnea, sometimes there is asphyxia, Sighing respiration or double suction gas, enter comatose state very soon, and side pupil size not grade or suddenly big or suddenly small, normal dead because of respiratory failure.Chronic dysentery, all courses of disease, more than 2 months persons, are called chronic dysentery, and majority is because walking dysentery treatment is not thorough or child suffers from malnutrition, rickets, anemia, caused by the sick body matter such as parasite are more weak, such sick child is many can there is stomachache sometimes without high heat, diarrhoea, vomiting and low grade fever, stool every day 3-5 time, can have and normally just just alternately occur with bloody purulent stool with mucus, suffer from the sick child of chronic dysentery, because long-term nutrition is bad, resistance is poor, other bacteriological infection of easy merging, as pneumonia, tuberculosis etc.
At present clinically to bacillary dysentery to supplement the fluid infusion salt containing sodium chloride, potassium chloride and glucose, sodium citrate etc., be aided with chloromycetin, furazolidone etc.And modern medicine is for clinical a certain symptom treatment, often fall flat.In order to overcome above-mentioned defect, the present invention is based on the differential diagnosis of diseases of Chinese traditional treatment intestinal infection and the dialectical principle combined, treating both the principal and secondary aspects of a disease, deficiency and excess is also controlled, inside and outside logical tune, and emergency is taken in concurrently, filter out the natural plant of damp and hot, the regulating the stomach and sending down the abnormal ascending QI of digestion, relieving dyspepsia, spleen invigorating QI invigorating, according to theory of Chinese medical science prescription, according to the preparation of certain weight proportion, provide a kind of Chinese medicine preparation of evident in efficacy, with low cost, treatment acute enteritis that toxic and side effects is little.
Summary of the invention
The object of the present invention is to provide a kind of Chinese medicine composition for the treatment of bacillary dysentery and preparation method thereof.The crude drug of described Chinese medicine composition is made up of four Chinese medicine materials such as Herba Andrographis, Ramulus Et Folium Picrasmae, Pericarpium Citri Reticulatae, Radix Glycyrrhizaes.There is heat-clearing and toxic substances removing, effect of dampness-eliminating and dysentery-stopping, be used for the treatment of bacillary dysentery, acute enteritis and various samples illness.
The Chinese medicine composition being used for the treatment of bacillary dysentery of the present invention mainly with Herba Andrographis and Ramulus Et Folium Picrasmae for curing mainly, be aided with Pericarpium Citri Reticulatae and Radix Glycyrrhizae.They influence each other, synergism, thus play good clearing away heat-damp and promoting diuresis, the spleen and stomach regulating, the effect of removing toxic substances dysentery relieving, have good curative effect to bacillary dysentery, and its raw material is simple, taking convenience.
Herba Andrographis: bitter in the mouth; Cold in nature.GUIXIN, lung, large intestine, urinary bladder channel.There is heat-clearing and toxic substances removing, removing heat from blood, detumescence, dampness effect, once multi-infection disease was applied to clinically, comprise trauma infection contamination, furuncle, carbuncle, erysipelas, upper respiratory tract infection, acute and chronic tonsillitis, acute and chronic pharyngitis, acute/chronic bronchitis, acute bacillary dysentery, acute gastroenteritis, urinary tract infection, endometritis, pelvic inflammatory disease, otitis media, periodontitis etc., all have curative effect in various degree.Natural plants Herba Andrographis mainly contain effective constituent andrographolide, molecular formula C20H30O5, there is thermal detoxification of dispelling, effect of anti-inflammatory analgetic, have special efficacy to bacillary with viral upper respiratory tract infection and dysentery, be described as natural antibiotics medicine; This product is diterpenes diterpenoids lactones compound, is all insoluble in water, usually only can oral administration.In Herba Andrographis, contained neoandrographolide is excellent to the curative effect of bacillary dysentery compared with chloromycetin and furazolidone clinically, and has no side effect and toxicity.In vitro tests, Herba Andrographis water decoction and from the coarse crystallization wherein isolated, all have suppression or killing action to some type leptospiral, decoct has certain inhibitory action to streptococcus pneumoniae, first streptococcus and micrococcus catarrhalis.Therefore there is antibacterial and anti-inflammation functions.Andrographolide, neoandrographolide contained by it all have the effect suppressing and delay Diplococcus pneumoniae and the rising of the body temperature caused by hemolytic group B streptococcus, and the action intensity of the latter is not as good as the former.For the rabbit or 2 generated heat caused by TAB, the rat of the caused heating of 2, 4-dinitrophenol, deoxyandrographolide, andrographolide, new Herba Andrographis, lactone, dehydrorographolide all have certain refrigeration function, wherein the strongest with dehydrorographolide effect.With deoxyandrographolide and neoandrographolide suspendible intraperitoneal injection, to while subcutaneous injection Diplococcus pneumoniae and Hemolytic streptococcus culture caused by fever in rabbit can postpone the body temperature rise time, weaken body temperature rising degree, therefore show as antipyretic effect.
Clinical trial document shows to adopt dimethylbenzene, acetic acid induced mice skin or abdominal cavity capillary permeability to increase, gavage deoxyandrographolide or dehydrorographolide all can reduce oozing out of capillary wall, and compare P<0.05 or P<0.01.Ooze out hemorrhagic necrotic caused by rat Oleum Tiglii, deoxyandrographolide has obvious inhibitory action.Deoxyandrographolide, andrographolide and neoandrographolide have obvious inhibitory action to leukoplania in rat CMC capsule in 7.5 hours under the heavy dose of 100mg/ capsule.These four kinds of andrographolide are also observed in experiment has excitation in various degree to Adrenal Cortex function, is the strongest with dehydrorographolide.Andrographolide and neoandrographolide have the colibacillary effect of suppression.Show that Herba Andrographis has obvious effect to intestinal infection disease thus.
Ramulus Et Folium Picrasmae: bitter in the mouth; Cold in nature.Return lung, large intestine channel.There is heat-clearing and toxic substances removing, removing dampness and killing parasites effect.Your Majesty's respiratory tract infection; Pneumonia; Acute gastroenteritis; Dysentery; Biliary tract infection.Clinical in anemopyretic cold, laryngopharynx swelling and pain, diarrhoea dysentery, enteritis, eczema, furuncle, the diseases such as venom.
Pericarpium Citri Reticulatae: acrid in the mouth is bitter; Warm in nature.Return spleen, stomach, lung meridian.There is warming stomach for dispelling cold, regulating qi-flowing for strengthening spleen, whet the appetite in tune, effect of drying dampness to eliminate phlegm.Cure mainly stagnation of QI in spleen and stomach dampness, chest and diaphragm full vexed, abdominal distention, anorexia, lack of appetite and vomiting, difficulty in urination and defecation, the diseases such as cough with copious phlegm.
Radix Glycyrrhizae: sweet in the mouth, flat, nontoxic; Slightly cool in nature.Return spleen, stomach, lung meridian.There is QI invigorating invigorating middle warmer, relieving spasm to stop pain, nourishing the lung to arrest cough, eliminating fire and detoxication, the effects such as coordinating the actions of various ingredients in a prescription.For weakness of the spleen and stomach, fatigue and weakness, shortness of breath and palpitation, cough with copious phlegm, the anxious pain of gastral cavity abdomen, extremity contraction, carbuncle sore tumefacting virus, cushion toxicity, strong.
The crude drug that the present invention treats the Chinese medicine composition of bacillary dysentery consists of: Herba Andrographis 10-20 weight portion, Ramulus Et Folium Picrasmae 10-20 weight portion, Pericarpium Citri Reticulatae 2-6 weight portion, Radix Glycyrrhizae 2-6 weight portion.
The preferred Chinese medicine composition of the present invention, is characterized in that it is made up of following raw material medicaments: Herba Andrographis 20 weight portion, Ramulus Et Folium Picrasmae 20 weight portion, Pericarpium Citri Reticulatae 5 weight portion, Radix Glycyrrhizae 5 weight portion form.
The Chinese medicine composition for the treatment of bacillary dysentery of the present invention can add various customary adjuvant required when preparing different dosage forms, such as disintegrating agent, lubricant, filler etc. are prepared into multiple conventional oral formulations with the method for Chinese medicinal of routine, such as pill, capsule, tablet, granule or oral liquid etc., preferred capsule and tablet, most preferably capsule.
The Chinese medicine composition of the present invention to obtained treatment bacillary dysentery has carried out clinical efficacy and safety testing thereof.Method adopts Method of Random Test, observes the clinical efficacy that compositions of the present invention treats 200 routine bacillary dysenterys.Result is treatment group clinical recovery rate is 69%, and obvious effective rate is 12%, and effective percentage is 10%.The above results shows that compositions of the present invention has obvious curative effects for treatment bacillary dysentery.Safety testing does not find untoward reaction.
According to modern Chinese medicine pharmacological research, Chinese medicine clinical efficacy is embodied in the interaction between contained effective ingredient and multiple isomeric components.Chinese medicine ingredients is complicated, and have interaction between each taste medicine, extraction process changes a little, the composition of extraction just may be made to change, may have influence on clinical efficacy.Herba Andrographis in prescription is that its effective ingredient of monarch drug comprises deoxyandrographolide, andrographolide, neoandrographolide, dehydrorographolide etc., be the poor and case of thermal instability of Ginkgolide Component water solublity, about the report of Herba Andrographis extraction process is few, generally there are water extraction, alcohol extracting method, percolation etc.The present invention extracts Herba Andrographis with ethanol with reference to official method, and comprehensive analysis adopts infusion process to extract, and by orthogonal test preferred processing condition, avoids the loss of effective ingredient; Percolation is adopted to extract with reference to Fufang Kumu Xiaoyan Pian preparation technology to three taste medical materials such as Ramulus Et Folium Picrasmaes.In order to ensure this product curative effect, we adopt orthogonal test to screen extraction process, and choosing wherein Herba Andrographis effective ingredient andrographolide and dehydrorographolide sum is that content controls, preferred preparation technology, and formulates formulation content limit, improves the quality of products.
The preparation technology of the Chinese medicine composition for the treatment of bacillary dysentery of the present invention, the Herba Andrographis second alcohol and water of recipe quantity is comprised the steps: to extract, be condensed into extractum, the Ramulus Et Folium Picrasmae of the recipe quantity of recipe quantity, Pericarpium Citri Reticulatae, Radix Glycyrrhizae percolation are extracted, be condensed into extractum, then by the mixing of two kinds of extractum, then add different pharmaceutic adjuvants as required and be mixed and made into various preparation.The Herba Andrographis that preferred method comprises the steps: to get recipe quantity adds ethanol 12 times of Soakage extraction twice, each 12 hours, filters, merging filtrate, reclaims ethanol and is concentrated into the extractum I of relative density 1.30 ~ 1.35 (50 DEG C); Get the Ramulus Et Folium Picrasmae of recipe quantity, Pericarpium Citri Reticulatae, Radix Glycyrrhizae shatter into coarse powder, add ethanol 10 doubly slowly percolation, diacolation liquid recycling ethanol, is concentrated into the extractum II of relative density 1.30 ~ 1.35 (50 DEG C); By above-mentioned two kinds of extractum mixing, add different auxiliary material according to the process requirements making different dosage form and make preparation.
The invention provides a kind of method of quality control of Chinese medicine composition of above-mentioned treatment bacillary dysentery, it is characterized in that using chromatograph of liquid to detect andrographolide in Chinese medicine composition and dehydrorographolide, wherein chromatographic column filler is octadecyl silane (5 μm, 4.6 × 250mm), mobile phase is methanol-water (54 ︰ 46), andrographolide determined wavelength is 225nm, dehydrorographolide determined wavelength is 254nm, the preparation method detecting sample is: precision takes compositions fine powder 1g, add 70% methanol 20ml, leave standstill 2 hours, supersound extraction 30 minutes, be cooled to room temperature, add methanol constant volume to 25ml measuring bottle, shake up, filter and get final product.
Detailed description of the invention
Below in conjunction with specific embodiment, the invention will be further described, and to make those skilled in the art the present invention may be better understood and can be implemented, but illustrated embodiment is not as a limitation of the invention.
The preparation of embodiment 1 Chinese medicine composition
With ethanol, Soakage extraction is carried out to Herba Andrographis, ethanol consumption, concentration of alcohol, extraction time, Extracting temperature four factors are investigated, each factor gets three levels, L9 (34) orthogonal table is selected to test, factor level sees the following form, each experiment accurately takes 100g Common Andrographis Herd and extracts, and filtrate is condensed into extractum.
| Level | A: solid-liquid ratio | B: concentration of alcohol/% | C: extraction time/h | D: temperature/DEG C |
| 1 | 8 | 50 | 8 | 2～8 |
| 2 | 10 | 75 | 12 | 20～25 |
| 3 | 12 | 95 | 24 | 30～35 |
To extract andrographolide amount for inspection target, the results are shown in following table.
As can be seen from orthogonal test table 1-2, four factors investigated above have significant impact to extraction, and it affects size is B>C>A>D, and optimum process condition is A3B2C2D2.Experimental result shows that the impact of temperature is very little, for reducing production cost, selecting experiment at normal temperatures or producing, and repeating experiment with this experiment condition.Determination of Andrographolide the results are shown in following table.
Herba Andrographis extraction time
Show that Herba Andrographis extracts optimised process and is by orthogonal experiments, 75% alcohol at normal temperature adding 12 times amount floods 12 hours, for ensureing that in Herba Andrographis medical material, main component is fully extracted, we investigate dipping number of times on the basis of optimised process, experiment accurately takes 100g Common Andrographis Herd and extracts, collect respectively and flood filtrate and the thick extractum being condensed into relative density 1.30 ~ 1.35 (50 DEG C) at every turn, detect its Determination of Andrographolide.The results are shown in following table:
Third time extracts rear Determination of Andrographolide seldom as seen from the above table, and Herba Andrographis medicinal material extract twice is described, each dipping 12 hours, can ensure fully to extract andrographolide.
Percolation ethanol consumption
Complete for ensureing Ramulus Et Folium Picrasmae, Pericarpium Citri Reticulatae, Radix Glycyrrhizae three taste medical material extracts active ingredients, get each three parts of Ramulus Et Folium Picrasmae 100g, Pericarpium Citri Reticulatae 25g, Radix Glycyrrhizae 25g respectively, put in little percolation bucket, with the speed percolation of 1 ~ 3ml/min, add 8 times, 10 times respectively, the ethanol of 12 times amount carries out percolation, collect filtrate, be concentrated into the thick paste of relative density 1.30 ~ 1.35 (50 DEG C).The results are shown in following table:
10 times amount ethanol are added proper by the visible percolation of upper table result.
Screened by above-mentioned process conditions, determine that the extraction process of Chinese medicine composition of the present invention is: the Herba Andrographis getting recipe quantity adds ethanol 12 times of Soakage extraction twice, each 12 hours, filter, merging filtrate, reclaim ethanol and be concentrated into the extractum I of relative density 1.30 ~ 1.35 (50 DEG C), for subsequent use.Get the Ramulus Et Folium Picrasmae of recipe quantity, Pericarpium Citri Reticulatae, Radix Glycyrrhizae powder be broken into coarse powder, add ethanol 10 doubly slowly percolation, diacolation liquid recycling ethanol, is concentrated into the extractum II of relative density 1.30 ~ 1.35 (50 DEG C), for subsequent use.Above-mentioned two kinds of extractum mixing, adds different auxiliary material according to the process requirements making different dosage form and makes preparation.
Prepared by embodiment 2 Chinese medicinal composition capsules
Get Herba Andrographis 200g and add ethanol 12 times dipping twice, each 12 hours, filter, merging filtrate, reclaim ethanol and be concentrated into the extractum I of relative density 1.30 ~ 1.35 (50 DEG C), for subsequent use.Get Ramulus Et Folium Picrasmae 200g, Pericarpium Citri Reticulatae 50g, Radix Glycyrrhizae 50 is ground into coarse powder, add ethanol 10 doubly slowly percolation, diacolation liquid recycling ethanol, is concentrated into the extractum II of relative density 1.30 ~ 1.35 (50 DEG C), for subsequent use.Above-mentioned two kinds of extractum mixing, vacuum drying, pulverizes, and in addition starch mixes in right amount, and soft material made by the ethanol with 60%, granulates, dry, granulate, and in addition Magnesium Stearate proper quantity mixes, and incapsulates, makes 1000, to obtain final product.
Prepared by embodiment 3 Chinese medicine composition tablet
Get Herba Andrographis 250g Herba Andrographis and add ethanol 12 times dipping twice, each 12 hours, filter, merging filtrate, reclaim ethanol and be concentrated into the extractum I of relative density 1.30 ~ 1.35 (50 DEG C), for subsequent use.Get Ramulus Et Folium Picrasmae 250g, Pericarpium Citri Reticulatae 62.5g, Radix Glycyrrhizae 62.5g is ground into coarse powder, add ethanol 10 doubly slowly percolation, diacolation liquid recycling ethanol, is concentrated into the extractum II of relative density 1.30 ~ 1.35 (50 DEG C), for subsequent use.Above-mentioned two kinds of extractum mixing, vacuum drying, pulverizes, and in addition starch mixes in right amount, and soft material made by the ethanol with 60%, granulates, drying, and tabletting, makes 1000, to obtain final product.
The quality control of embodiment 4 Chinese medicine composition
Content method research is carried out to andrographolide and dehydrorographolide, choose the capsule sample of embodiment 1, andrographolide determined wavelength 225nm, dehydrorographolide determined wavelength 254nm, investigates test sample processing method, method specificity, precision, accuracy and stability of solution etc.
Instrument: Shimadzu LC-10ATvp, SPD-10Avp chromatograph of liquid, LC-Solution work station;
Chromatographic column: octadecylsilane chemically bonded silica post (5 μm, 4.6 × 250mm);
Reference substance: andrographolide (lot number 110797-201108), dehydrorographolide (lot number 110854-201007), provide by National Institute for Food and Drugs Control
Sample: self-control sample
The selection of mobile phase
With reference to " Chinese Pharmacopoeia " 2010 editions relevant Herba Andrographis assay item current downflow phase, get andrographolide reference substance, dehydrorographolide reference substance is appropriate, accurately weighed, add methanol and make every 1ml respectively containing the mixed solution of 0.1mg, as test solution, methanol-water (52:48) is as mobile phase, carry out debugging and confirm mobile phase, find through experiment, methanol: water (52:48) appearance time too late, each pin all needs 60 minutes, be unfavorable for Long-term analysis, methanol is found: water (54:46) is as mobile phase through debugging, two main peak separating effects are relatively good, and peak shape is good-looking, therefore selection methanol: water (54:46) is as mobile phase.
The selection of Extraction solvent
Get this product (lot number: 140801), removing softgel shell, porphyrize, accurately weighed fine powder 1g8 part, adds 40% methanol, 50% methanol, 70% methanol, each 20ml of 100% methanol respectively, leaves standstill 2h, supersound process 30 minutes, lets cool, then adds corresponding solvent to scale, shake up, filter, obtain the need testing solution under different solvents, precision measures mixing reference substance solution and each 10 μ l of above-mentioned need testing solution respectively, injection liquid chromatography, measures content, the results are shown in following table:
| Extraction solvent | 40% methanol | 50% methanol | 70% methanol | 100% methanol |
| Content (mg/ grain) | 0.143 | 0.148 | 0.170 | 0.106 |
Indicated by above result: the effect of 100% methanol extraction is the poorest; 40% methanol and 50% methanol extraction rate increase, andrographolide and dehydrorographolide, due to lighter than water, but often swim in liquid level upper strata in operation, be not less than standardize solution; 70% methanol extraction effect is best, therefore selects 70% methanol as the Extraction solvent of this product assay test sample.
The selection of extraction time
Get this product (lot number 140801), removing softgel shell, porphyrize, precision takes fine powder 1g, add 70% methanol 20ml, leave standstill 1,2,3 hour respectively, then supersound extraction 15,30,45 minutes, is cooled to room temperature, add 70% methanol constant volume to 25ml, shake up, filter, get subsequent filtrate as need testing solution.Get the test sample of extraction of above-mentioned time respectively, precision measures 10 μ l injection liquid chromatographies, the results are shown in following table.
Above result shows: the extraction effect leaving standstill 2h is better than the extraction effect of standing 1h, but be not that the longer the better for time of repose, therefore select to leave standstill 2h, leave standstill the ultrasonic 45min of 1h and standing 2h ultrasonic 30min extraction effect similar, but ultrasonic time is oversize is easy to heat-dissipating, be not less than next step carrying out, therefore the extraction time selected is the ultrasonic 30min of standing 2h.
Comprehensively above-mentioned: the preparation method of test sample is: to get this product in right amount, removing softgel shell, porphyrize, precision takes fine powder 1g, adds 70% methanol 20ml, and leave standstill 2 hours, supersound extraction 30 minutes, is cooled to room temperature, adds methanol constant volume to 25ml measuring bottle, shakes up, and filters, to obtain final product.
Specificity
Chromatographic condition and system suitability take octadecyl silane as filler; With methanol-water (54 ︰ 46) for mobile phase; Andrographolide determined wavelength is 225nm, and dehydrorographolide determined wavelength is 254nm.Number of theoretical plate calculates all should be not less than 2000 by andrographolide and dehydrorographolide.
Reference substance solution prepare andrographolide reference substance, dehydrorographolide reference substance is appropriate, accurately weighed, add methanol and make every lml respectively containing the mixed solution of 20 μ g, to obtain final product.
The preparation of need testing solution gets this product in right amount, removing softgel shell, porphyrize, and precision takes fine powder 1g, adds 70% methanol 20ml, and leave standstill 2 hours, supersound extraction 30 minutes, is cooled to room temperature, adds methanol constant volume to 25ml measuring bottle, shakes up, and filters, to obtain final product.
Algoscopy is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
Blank solvent: using 70% methanol as blank solution;
Negative need testing solution: get negative granules appropriate, porphyrize, precision takes fine powder 1g, puts in 25ml measuring bottle, adds 70% methanol 20ml, leave standstill 2h, supersound process 30 minutes, lets cool, then adds 70% methanol to scale, shakes up, and filters, as negative need testing solution;
Measure blank solvent, negative need testing solution, reference substance solution, each 10 μ l of need testing solution, inject high performance liquid chromatograph respectively, record chromatogram, the results are shown in following table:
Conclusion: need testing solution main peak is consistent with reference substance main peak, the separating degree at main peak and other impurities peak is all greater than 1.5, negative granules and blank solvent all noiseless to the mensuration of this product, show that method specificity is good.
Precision
The capsule of Example 1, removing softgel shell, porphyrize, accurately weighed, prepare 6 parts of need testing solutions, precision measures each 10 μ l injection liquid chromatographies of above-mentioned solution in accordance with the law, record chromatogram; By external standard method with calculated by peak area, the results are shown in following table.
Same batch sample, replication 6 times, the RSD of assay result is 1.28%<2.0%, shows that the method precision is good.
Accuracy
Andrographolide
Get this product (lot number: 140801), removing softgel shell, porphyrize, accurately weighed 0.5g9 part, precision adds each 3 parts of the single reference substance of dehydrorographolide (concentration is about 0.1994mg/ml) 1.8ml, 2.2ml, 2.7ml respectively, add the appropriate about 20ml of 70% methanol, leave standstill 2h, supersound process 30min, let cool, add 70% methanol dilution again to scale, shake up, filter, obtain application of sample and reclaim need testing solution; Get mixing reference substance 1, the 2 product solution in contrast of refrigerator cold-storage; Precision measures above-mentioned need testing solution and each 10 μ l of reference substance solution, injects high performance liquid chromatograph respectively, record chromatogram, and result of the test sees the following form:
Dehydrorographolide
Get this product (lot number: 140801), removing softgel shell, porphyrize, accurately weighed 0.5g9 part, precision adds each 3 parts of the single reference substance of dehydrorographolide (concentration is about 0.3854mg/ml) 3.2ml, 4.0ml, 4.8ml respectively, add the appropriate about 20ml of 70% methanol, leave standstill 2h, supersound process 30min, let cool, add 70% methanol dilution again to scale, shake up, filter, obtain application of sample and reclaim need testing solution; Get mixing reference substance 1, the 2 product solution in contrast of refrigerator cold-storage; Precision measures above-mentioned need testing solution and each 10 μ l of reference substance solution, and inject high performance liquid chromatograph respectively, result of the test sees the following form:
Conclusion: andrographolide is under 80%, 100%, 120% 3 concentration, and mean sample recovery rate is 99.41%, 99.39%, 99.33%, the average recovery rate of 9 increment product is 99.38%, RSD is 0.35%; Dehydrorographolide is under 80%, 100%, 120% 3 concentration, mean sample recovery rate is 99.64%, 99.40%, 99.28%, the average recovery rate of 9 increment product is 99.44%, RSD is 0.21%, namely andrographolide and the dehydrorographolide response rate are all within the scope of 98.0%-102.0%, show that the accuracy of method meets the requirements.
The stability of solution
Prepare need testing solution in accordance with the law, measure need testing solution 10 μ l respectively at 0,2,4,8,12 hour precision, measure in accordance with the law, calculate peak area RSD, and observe whether produce new impurity in 12h, the results are shown in following table:
Conclusion: place at ambient temperature, the RSD of the andrographolide peak area of test sample is 0.95%, the RSD of the peak area of dehydrorographolide is 0.91%, all be less than 2.0%, and whether producing new impurity at 12h, show that this product solution is stable in room temperature 12 hours, on assay without impact.
The above embodiment is only that protection scope of the present invention is not limited thereto in order to absolutely prove the preferred embodiment that the present invention lifts.The equivalent alternative or conversion that those skilled in the art do on basis of the present invention, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (7)
1. treat a Chinese medicine composition for bacillary dysentery, it is characterized in that, it is made up of following raw material medicaments: Herba Andrographis 10-20 weight portion, Ramulus Et Folium Picrasmae 10-20 weight portion, Pericarpium Citri Reticulatae 2-6 weight portion, Radix Glycyrrhizae 2-6 weight portion.
2. Chinese medicine composition according to claim 1, is characterized in that it is made up of following raw material medicaments: Herba Andrographis 20 weight portion, Ramulus Et Folium Picrasmae 20 weight portion, Pericarpium Citri Reticulatae 5 weight portion, Radix Glycyrrhizae 5 weight portion.
3. the Chinese medicine composition that one of claim 1-2 is described, is characterized in that described compositions is pill, capsule, tablet, granule or oral liquid.
4. the preparation method of the Chinese medicine composition of the described treatment bacillary dysentery of one of claim 1-2, comprise the steps: that the Herba Andrographis second alcohol and water getting recipe quantity extracts, be condensed into extractum, the Ramulus Et Folium Picrasmae of the recipe quantity of recipe quantity, Pericarpium Citri Reticulatae, Radix Glycyrrhizae percolation are extracted, be condensed into extractum, then by two kinds of extractum mixings, add different auxiliary material according to the process requirements making different dosage form and make preparation.
5. the preparation method of claim 4, the Herba Andrographis comprising the steps: to get recipe quantity adds ethanol 12 times of Soakage extraction twice, each 12 hours, filters, merging filtrate, reclaims ethanol and is concentrated into the extractum I of relative density 1.30 ~ 1.35 (50 DEG C); Get the Ramulus Et Folium Picrasmae of recipe quantity, Pericarpium Citri Reticulatae, Radix Glycyrrhizae powder be broken into coarse powder, add ethanol 10 doubly slowly percolation, diacolation liquid recycling ethanol, is concentrated into the extractum II of relative density 1.30 ~ 1.35 (50 DEG C); By above-mentioned two kinds of extractum mixing, add different auxiliary material according to the process requirements making different dosage form and make preparation.
6. the application of the Chinese medicine composition that one of claim 1-2 is described in the medicine for the preparation for the treatment of bacillary dysentery, acute enteritis.
7. the method for quality control of the Chinese medicine composition that one of claim 1-2 is described, it is characterized in that using chromatograph of liquid to detect andrographolide in the Chinese medicine composition of one of claim 1-2 and Determination of Dehydroandrographoliin sum, wherein chromatographic column filler is octadecyl silane, mobile phase is methanol-water (54 ︰ 46), andrographolide determined wavelength is 225nm, dehydrorographolide determined wavelength is 254nm, the preparation method detecting sample is: precision takes compositions fine powder 1g, add 70% methanol 20ml, leave standstill 2 hours, supersound extraction 30 minutes, be cooled to room temperature, add methanol constant volume to 25ml measuring bottle, shake up, filter and get final product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106177210A (en) * | 2016-08-04 | 2016-12-07 | 郭贤卿 | A kind of Chinese medicinal capsule treating enteritis |
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Application publication date: 20160316 |