CN106620498A - Preparation method, quality control and use of traditional Chinese medicine composition for treating postinfectious cough - Google Patents

Preparation method, quality control and use of traditional Chinese medicine composition for treating postinfectious cough Download PDF

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CN106620498A
CN106620498A CN201510708038.9A CN201510708038A CN106620498A CN 106620498 A CN106620498 A CN 106620498A CN 201510708038 A CN201510708038 A CN 201510708038A CN 106620498 A CN106620498 A CN 106620498A
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chinese medicine
chinese
medicine composition
medicinal material
solution
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李慧
冯学功
吴宏伟
杨洪军
刘宇灵
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Institute of Materia Medica of CAMS
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Abstract

The invention provides a traditional Chinese medicine composition for treating postinfectious cough. The traditional Chinese medicine composition is composed of the following raw material medicines in parts by weight: 6-20g of radix clematidis, 6-20g of radix curcumae, 3-10g of rhizoma acori graminei and 3-6g of mint. A preparation method comprises the steps: adding water which is 6-12 times of total weight of the medicinal materials into radix clematidis, mint, rhizoma acori graminei and radix curcumae, extracting volatile oil for 5-9 hours by a water vapor distillation method, collecting the volatile oil, and adding tween-80 to solubilize or adding ethanol to dissolve for later use; filtering a water vapor distillation extracting solution to obtain oil extraction mother liquor and filter dregs; adding 6-10 times of water into the filter dregs and decocting the mixture for 1-3 times, 1-3 hours every time, combining the decocting liquid and the oil extraction mother liquor, adding 75-95% ethanol after concentrating the supernate, wherein the alcohol content reaches 65-85%, freezing and leaving the mixture to stand and take out, performing filtration, and recovering the filtrate at a reduced pressure till ethanol is free of alcohol odor; adding the solubilized volatile oil and conventional pharmaceutic adjuvants, and preparing a proper form by adopting a conventional preparation method in traditional Chinese medicine pharmacy. The invention also provides an application of the traditional Chinese medicine composition in preparing medicines for treating infectious cough and various chronic cough.

Description

A kind of preparation method of the Chinese medicine composition for treating cough after common cold, quality control and purposes
Technical field
The invention belongs to the field of Chinese medicines, is related to a kind of Chinese medicine composition, and in particular to a kind of to treat Chinese medicine composition of cough after common cold and preparation method thereof and purposes.
Background technology
Flu is also called acute upper respiratory infection, is one of modal infectious diseases of the mankind, and adult catches a cold 2-4 time every year on average, and acute cough is the adjoint most common symptom of flu, is one of medical most common symptom of primary care mechanism.
According to statistics, the patient of annual about 11%-25% can occur cough after common cold (PIC), in epidemic season, cough after common cold incidence may be up to 25%-50%, such crowd is after flu acute stage symptom itself disappears, cough still protracted course of disease, show as excitant dry cough more or cough a small amount of white mucus phlegm, can be with continued for several weeks, even longer time frequent violent cough usually has a strong impact on study, work and the life of patient, normal life to people has stronger negative effect, and this disease of Chinese medicine is with some superiority.
PIC belongs to traditional Chinese medicine " exogenous cough's disease " category.Traditional Chinese medicine thinks lung governing qi, and department's breathing, upper even air flue is had one's ideas straightened out in nose, and throat is its door, intolerant to fever and chills, is easily invaded by heresy.The heresy of the diseases caused by external factors six external factors which cause diseases, again based on ailment said due to cold or exposure, can be mingled with cold, hot, dry, wet etc. simultaneously, fail timely table to dissipate, or the miscellaneous throwing of relieving cough and reducing sputum medicine or bitter-cold herbs expelling heat medicine blindly use or astringe the lung astringent medicinal misuse, cause exopathogen to be reluctant to leave, inside lie prostrate in lung, impairment of dispersing and descending function of the lung, superinverse and cough, so one of TCM Syndrome Features of cough after common cold are that table is evil not to the greatest extent.
Another feature of PIC is deficient vital QI leading to lingering of pathogen, and the state of an illness is touching.With the passing of time cough after common cold does not heal, and can be transformed into endogenous cough.《Plain Questions coughs opinion》In then point out that " vital organs of the human body all make us coughing, non-only lung." in addition to lung is coughed, still intentionally cough, cough due to the disorder of the Liver Channel, cough related to the spleen channel, kidney are coughed, course of disease length of now coughing, sick locating depth, then more refractory.Guan Qiuhong etc. think to adjust mend it is inappropriate be also cough after common cold common disease because, cross and mend or improper diet, disorder of the spleen and stomach caused by internal damage, retention of water-damp in the body, above store in lung, the respectful drop of lung qi is unfavorable and cough.What is had thinks that this disease is more because of wind-heat affecting lung, and with the passing of time the violent rage impariment of the liver, feelings hinder, and movement of QI being out of order feels again exopathogen, changes hot vehement Tianjin；Or Kidney-Yin loss, the fire of unrooted, parading without system, visitor is caused by throat.Separately have think the disease be because stagnation of liver qi, the dysfunction of the spleen in transport, stomach Qi are weak, with bringing about the spread of body fluid can not on hold throat and cause.Also many doctors opinion in terms of pathological product controls, opinion is controlled from phlegm-blood stasis opinion, it is believed that in chronic pharyngitis pathogenic process, and " phlegm " and " stasis of blood " is modal pathological factor, and phlegm-blood stasis are mutual and deposit.There is just PIC point of research to be 5 types：Ailment said due to cold or exposure love pulmonary type is controlled based on eliminating evil, and cold drink volt pulmonary type is controlled with Wenfei of drink cold dispelling, and phlegm-heat accumulated in the lung type is controlled based on clearing lung and eliminating phlegm, liver-fire attacking lung then removing heat from the lung to relieve cough, soft liver emergency, and asthenia of pulmonosplenic qi type is then based on help lung spleen.《Tcm clinical practice diagnosis and treatment term syndrome part》Then cough after common cold is divided into into type of YIN-deficiency and interior-heat, deficiency of vital energy phlegm-damp type, the type of caused by hepatic stagnation qi stagnation 3.
The Chinese medicine composition of the present invention is from clinical effective experience side, substantial amounts of clinical case is have accumulated in long-term clinical practice, for the little compound of a 4 taste Chinese medicines composition, compatibility is precise and appropriate, change sanction degree of having, the quality control of advantageously combined thing preparation and technical study.Wherein：
The root of Chinese clematis：Property it is pungent, into, temperature.Return bladder warp.With wines used as antirheumatic, degrading the channel effect, for arthralgia due to wind-dampness, extremity numbness, muscle arteries and veins contraction, joint stuffiness.For the monarch drug in a prescription in this side, because the wines used as antirheumatic of the root of Chinese clematis is acted on, for modal wind result index type is extremely suited the medicine to the illness in cough after common cold, the effect that dispelling wind declares lung is played.
Grass-leaved sweetflag：Property pungent, hardship, temperature.The thoughts of returning home, stomach.With slit phlegm of having one's ideas straightened out, inducing resuscitation intelligence development, dampness elimination appetizing effect.For coma epilepsy, forgetful insomnia, Hiccough and deaf, gastral cavity ruffian is not hungry, a mouthful diarrhea of keeping silent.For the adjutant in this side, no matter grass-leaved sweetflag which kind of type in treatment cough after common cold has the effect of resolving sputum profit pharynx.
Root tuber of aromatic turmeric：Property pungent, hardship, tremble with fear.Return liver, the heart, lung channel.With promoting blood circulation and stopping pain, promoting qi circulation and removing obstruction in the collateral, clear away heart-fire cool blood, normalizing gallbladder to cure jaundice effect.For chest side of body shouting pain, chest impediment and cardialgia.For the ministerial drug in this side.Root tuber of aromatic turmeric in the treatment coughed to caused by hepatic stagnation qi stagnation, the effect of promoting qi circulation and removing obstruction in the collateral can be played very well.
Peppermint：Property is pungent, cool.Return lung, Liver Channel.With dispelling wind and heat from the body, head clearing, profit pharynx, promoting eruption, soothing the liver promoting the circulation of qi effect.For anemopyretic cold, from the beginning of, headache, hot eyes, larynx numbness, aphtha, rubella, measles, Breast bilges frowsty about is to make medicine in this side to wind-warm syndrome.
The content of the invention
It is an object of the invention to provide a kind of Chinese medicine composition；
The present invention also aims to provide the preparation method of said composition；
The present invention also aims to provide the purposes of the Chinese medicine composition；
The present invention also aims to provide the method for quality control of the Chinese medicine composition.
The purpose of the present invention is achieved in the following ways：
A kind of Chinese medicine composition for treating cough after common cold, is made up of the bulk drug of following weight ratio：6-20 gram of the root of Chinese clematis, 6-20 gram of root tuber of aromatic turmeric, 3-10 gram of grass-leaved sweetflag, 3-10 gram of peppermint.
Above-mentioned raw materials, the root of Chinese clematis is dried root and rhizome from ranunculaceae plant root of Chinese clematis Clematis chinensis Osbeck, Clematis hexapetala Clematis hexapetala Pall. or northeast clematis Clematis manshurica Rupr.'s；Root tuber of aromatic turmeric derives from zingiberaceous plant RADIX CURCUMAE Curcuma wenyujin Y.H.Chen et C.Ling, turmeric Curcuma longa L., the dried root of Guangxi zedoary Curcuma kwangsiensis S.G.Lee et C.F.Liang or zedoary Curcuma phaeocaulis Val..The above two practise respectively title " RADIX CURCUMAE " and " Radix Curcuma ", and remaining claims " osmanthus root tuber of aromatic turmeric " or " green silk root tuber of aromatic turmeric " by different habit of proterties；Dry rhizome of the grass-leaved sweetflag from acorus gramineus araceae plant Acorus tatarinowii Schott.Dry aerial parts of the peppermint from labiate peppermint Metha haplocalyx Briq..
The Chinese medicine composition is preferably made up of the bulk drug of following weight ratio：10 grams of the root of Chinese clematis, 10 grams of root tuber of aromatic turmeric, 6 grams of grass-leaved sweetflag, 6 grams of peppermint.
The Chinese medicine composition is preferably made up of the bulk drug of following weight ratio：6 grams of the root of Chinese clematis, 15 grams of root tuber of aromatic turmeric, 6 grams of grass-leaved sweetflag, 9 grams of peppermint.
The Chinese medicine composition is preferably made up of the bulk drug of following weight ratio：12 grams of the root of Chinese clematis, 10 grams of root tuber of aromatic turmeric, 6 grams of grass-leaved sweetflag, 6 grams of peppermint.
The Chinese medicine composition is preferably made up of the bulk drug of following weight ratio：15 grams of the root of Chinese clematis, 12 grams of root tuber of aromatic turmeric, 9 grams of grass-leaved sweetflag, 3 grams of peppermint.
The Chinese medicine composition is preferably made up of the bulk drug of following weight ratio：20 grams of the root of Chinese clematis, 15 grams of root tuber of aromatic turmeric, 3 grams of grass-leaved sweetflag, 9 grams of peppermint.
The preparation method of above-mentioned Chinese medicine composition is：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material total amount 6-12 times water, with extraction by steam distillation volatile oil 5-9 hours, collect volatile oil, add Tween-80 solubilising, standby；Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 6-10 times of decocting to boil 1-3 time, each 1-3 hours, merges decoction liquor and carries oily mother liquor, and 75-95% ethanol will be added to make alcohol content up to 65-85% after supernatant concentration, and refrigeration is taken out after standing, and is filtered, and decompression filtrate recycling ethanol is to without alcohol taste；Volatile oil and conventional pharmaceutical adjuvants after solubilising are added, using formulation method conventional in pharmacy of Chinese materia medica, suitable dosage forms is made.
Above-mentioned preparation method is preferably：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, collect volatile oil, and mother liquor is filtered, and add Tween-80 solubilising, standby；Steam distillation extract is filtered, and must carry oily mother liquor and filter residue；Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, merges decoction liquor and carries oily mother liquor, and 95% ethanol will be added to make alcohol content up to 65% after supernatant concentration, and refrigeration stands and taken out after 15h, filtration, and decompression filtrate recycling ethanol is extremely without alcohol taste；Volatile oil and conventional pharmaceutical adjuvants after solubilising are added, using formulation method conventional in pharmacy of Chinese materia medica, granule, oral tablet, buccal tablet, dispersible tablet, hard capsule, soft capsule, oral liquid, spray, powder-type spray is made.
The preferred formulation of Chinese medicine composition of the present invention is oral liquid, and its preparation method is：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, collect volatile oil, add Tween-80 solubilising, standby；Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, merges decoction liquor and carries oily mother liquor, and 95% ethanol will be added to make alcohol content up to 65% after supernatant concentration, and refrigeration stands and taken out after 15h, filtration, and decompression filtrate recycling ethanol is extremely without alcohol taste；Volatile oil and simple syrup, stevioside and Sodium Benzoate, constant volume after solubilising are added, in being sub-packed in oral liquid bottle, is obtained final product.
The Chinese medicine composition of the present invention can also be adopted and prepared with the following method：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, the 50-80% alcohol refluxs for adding medicinal material total amount 5-15 times are extracted, extraction time 1-4 time, every time 0.5-4 hours, alcohol extract merging, filter, filtrate concentrates, conventional pharmaceutical adjuvants are added, using formulation method conventional in pharmacy of Chinese materia medica, suitable dosage forms is made.
Above-mentioned preparation method is preferably：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, plus 70% alcohol reflux extract 2 times, 3 hours every time, alcohol extract merges, filter, concentration adds conventional pharmaceutical adjuvants, using formulation method conventional in pharmacy of Chinese materia medica, granule, oral tablet, buccal tablet, dispersible tablet, hard capsule, soft capsule, oral liquid, spray, powder-type spray are made.
The preferred formulation of Chinese medicine composition of the present invention is oral liquid, and its preparation method is：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, plus 70% alcohol reflux extracts 2 times, 3 hours every time, alcohol extract merged, and filtered, and concentration adds simple syrup, stevioside and Sodium Benzoate, constant volume, in being sub-packed in oral liquid bottle, obtains final product.
The Chinese medicine composition of the present invention can also be adopted and prepared with the following method：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material total amount 6-12 times water, with extraction by steam distillation volatile oil 5-9 hours, collect volatile oil, and beta-cyclodextrin inclusion compound obtains inclusion compound standby：Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 6-10 times of decocting to boil 1-3 time, and each 1-3 hours merge decoction liquor and carry oily mother liquor, 75-95% ethanol will be added after supernatant concentration to make alcohol content reach 65-85%, refrigeration is taken out after standing, filtration, and decompression filtrate recycling ethanol is to without alcohol taste, then proceed to be concentrated into thick paste, it is dried, gained dried object is well mixed with volatile oil clathrate compound, adds conventional pharmaceutical adjuvants, using formulation method conventional in pharmacy of Chinese materia medica, suitable dosage forms are made.
Above-mentioned preparation method is preferably：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, collect volatile oil, and beta-cyclodextrin inclusion compound, refrigerated overnight, filtration, low temperature drying obtains Benexate Hydrochloride standby；Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, merge decoction liquor and carry oily mother liquor, by 95% ethanol is added after supernatant concentration alcohol content is made up to 65%, refrigeration stands and taken out after 15h, filtration, decompression filtrate recycling ethanol is to without alcohol taste, then proceed to be concentrated into thick paste, it is dried, gained dried object is well mixed with volatile oil clathrate compound, adds conventional pharmaceutical adjuvants, using formulation method conventional in pharmacy of Chinese materia medica, granule, oral tablet, buccal tablet, dispersible tablet, hard capsule, soft capsule, oral liquid, spray, powder-type spray are made.
The preferred formulation of Chinese medicine composition of the present invention also has buccal tablet, and its preparation method is：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, collect volatile oil, and beta-cyclodextrin inclusion compound, refrigerated overnight, filtration, low temperature drying obtains Benexate Hydrochloride standby；Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, merges decoction liquor and carries oily mother liquor, 95% ethanol will be added after supernatant concentration to make alcohol content up to 65%, refrigeration stands and taken out after 15h, filtration, decompression filtrate recycling ethanol then proceedes to be concentrated into thick paste to without alcohol taste, is dried, gained dried object is well mixed with volatile oil clathrate compound, adds dextrin, cane sugar powder, stevioside, essence, wet granulation, whole grain after drying, 0.5% magnesium stearate is added, is well mixed, be pressed into buccal tablet and obtain final product.
The Chinese medicine composition method of quality control of the present invention includes one or more of following discrimination method and/or assay：
Differentiate：
The Chinese medicinal composition preparation content 2-10mL for taking the present invention is placed in round bottom sesame seed cake, add the HCl30-100mL of 2mol/L, water-bath backflow 1-3 hours, it is placed in after cooling in separatory funnel, ethyl acetate is added to extract 1-3 time, each 15-30mL, combining extraction liquid pressurization is evaporated, methanol constant volume to 5-10mL, as need testing solution.Separately take oleanolic acid and the normal aglycon reference substance of ivy soap plus methyl alcohol makes every 1mL containing 1mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-ethyl acetate-formic acid (5-20: 1-10: 0.1-1) as solvent, lamellae puts presaturation 30 minutes in expansion cylinder, launches, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear.In test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color.
The Chinese medicinal composition preparation content 2-10mL for taking the present invention is placed in separatory funnel, and addition petroleum ether extraction 1-3 time, each 5-15mL merges ether, 2-10mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.Peppermint control medicinal material is separately taken, 40 mesh sieves were crushed, 0.5g plus 5-15mL petroleum ethers ultrasound 30min is taken, after filtration, filtrate is evaporated and is settled to 1mL, as control medicinal material solution.Separately take menthol reference substance plus methyl alcohol makes every 1ml containing 2mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (5-20: 1-5) as solvent, after presaturation 30min, launch, take out, dry, spray with 2% vanillin-sulfuric acid-ethanol (1: 4) developer, 105 DEG C to be heated to spot development clear.In test sample chromatogram, on position corresponding with reference substance, control medicinal material chromatogram, show the spot of same color.
The Chinese medicinal composition preparation content 2-10mL of the present invention is taken, absolute ethyl alcohol 25-50mL ultrasound 15-30min are added, filtration, decompression and solvent recovery, residue 1mL ethanol dissolves, used as need testing solution.Root tuber of aromatic turmeric control medicinal material is separately taken, 40 mesh sieves were crushed, 0.5-2g, plus 5-50mL EtOH Sonicate 30min is taken, is filtered, be settled to 1mL as control medicinal material solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-ethyl acetate (10-30: 5-10) as solvent, after presaturation 30min, launch, taking-up is dried, with 10% concentrated sulfuric acid ethanol developer, 105 DEG C to be heated to spot development clear for spray.In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the spot of same color.
The Chinese medicinal composition preparation content 2-10mL for taking the present invention is placed in separatory funnel, and addition petroleum ether extraction 1-3 time, each 5-15mL merges ether, 2-10mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.Grass-leaved sweetflag control medicinal material is separately taken, 40 mesh sieves were crushed, 0.5-2g, plus 10-40mL ether ultrasound 30min is taken, after filtration, filtrate is evaporated and is settled to 1mL, used as need testing solution.Separately take α-asarone reference substance plus methyl alcohol is prepared into every mL containing 2mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-ethyl acetate (5-20: 2-20) as solvent, after presaturation 30min, launch, take out, dry, put and inspected under ultraviolet lamp (365nm).In test sample chromatogram, on position corresponding with reference substance solution chromatogram, show the spot of same color.
Assay：
Chromatographic condition：Octadecylsilane chemically bonded silica is filler；Mobile phase be acetonitrile (A) -0.1-0.5% phosphoric acid (B), gradient elution (0～15min：70%A, 15～20min：70% → 90%A, 20～30min：90%A, 30～35：90% → 70%)；30 DEG C of column temperature；Flow velocity 1.0mlmin-1, Detection wavelength 205nm.External standard method peak area quantification.
It is prepared by reference substance solution：Hederagenin, the oleanolic acid reference substance in 60 DEG C of drying under reduced pressure 3-5 hours is weighed, plus methyl alcohol is made concentration of every 1ml containing 20ug and is obtained final product.
It is prepared by need testing solution：Measure Chinese medicinal composition preparation content 1-5ml, plus 2mol/L hydrochloric acid solution 10-50ml, 1-3 hours are heated to reflux, cool down immediately, in moving into separatory funnel, plus ethyl acetate shaking is extracted 1-3 time, each 10-30ml, combined ethyl acetate liquid, it is evaporated, plus methyl alcohol dissolving, in being transferred to 5ml measuring bottles, constant volume is obtained final product.
Determination method：Reference substance solution and each 10ul of need testing solution are drawn respectively, liquid chromatograph is injected, is determined, obtain final product.
Per milliliter gram must not be less than 0.60-1.00mg containing the root of Chinese clematis in terms of hederagenin in the oral liquid of Chinese medicine composition of the present invention, and 0.10-0.40mg must not be less than in terms of oleanolic acid.
The Chinese medicine composition method of quality control of the present invention is preferably one or more of following discrimination method and/or assay：
Differentiate：
Chinese medicinal composition preparation 2mL for taking the present invention is placed in round bottom sesame seed cake, adds the HCl 30mL of 2mol/L, water-bath to flow back 2 hours, it is placed in after cooling in separatory funnel, adds ethyl acetate to extract 3 times, each 15mL, combining extraction liquid pressurization is evaporated, methanol constant volume to 10mL, as need testing solution.Separately take oleanolic acid and the normal aglycon reference substance of ivy soap plus methyl alcohol makes every 1mL containing 1mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-ethyl acetate-formic acid (10: 3: 0.1) as solvent, lamellae puts presaturation 30 minutes in expansion cylinder, launches, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear.In test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color.
Chinese medicinal composition preparation 2mL for taking the present invention is placed in separatory funnel, and addition petroleum ether extraction 3 times, each 5mL merges ether, 2mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.Peppermint control medicinal material is separately taken, 40 mesh sieves were crushed, 0.5g plus 10mL petroleum ethers ultrasound 30min is taken, after filtration, filtrate is evaporated and is settled to 1mL, used as control medicinal material solution.Separately take menthol reference substance plus methyl alcohol makes every 1ml containing 2mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 2 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (8: 18) as solvent, after presaturation 30min, launch, take out, dry, spray with 2% vanillin-sulfuric acid-ethanol (1: 4) developer, 105 DEG C to be heated to spot development clear.In test sample chromatogram, on position corresponding with reference substance, control medicinal material chromatogram, show the spot of same color.
Chinese medicinal composition preparation 2mL of the present invention is taken, absolute ethyl alcohol 25mL ultrasound 15min are added, filtration, decompression and solvent recovery, residue 1mL ethanol dissolves, used as need testing solution.Root tuber of aromatic turmeric control medicinal material is separately taken, 40 mesh sieves were crushed, 2g, plus 25mL EtOH Sonicate 30min is taken, is filtered, be settled to 1mL as control medicinal material solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-Ethyl formate (15: 5) as solvent, after presaturation 30min, launch, taking-up is dried, with 10% concentrated sulfuric acid ethanol developer, 105 DEG C to be heated to spot development clear for spray.In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the spot of same color.
Chinese medicinal composition preparation 5mL for taking the present invention is placed in separatory funnel, and addition petroleum ether extraction 3 times, each 5mL merges ether, 5mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.Grass-leaved sweetflag control medicinal material is separately taken, 40 mesh sieves were crushed, 1g, plus 10mL ether ultrasound 30min is taken, after filtration, filtrate is evaporated and is settled to 1mL, used as need testing solution.Separately take α-asarone reference substance plus methyl alcohol is prepared into every mL containing 2mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-ethyl acetate (6: 4) as solvent, after presaturation 30min, launch, take out, dry, put and inspected under ultraviolet lamp (365nm).In test sample chromatogram, on position corresponding with reference substance solution chromatogram, show the spot of same color.
Assay：
Chromatographic condition：Octadecylsilane chemically bonded silica is filler；Mobile phase be the phosphoric acid (B) of acetonitrile (A) -0.1%, gradient elution (0～15min：70%A, 15～20min：70% → 90%A, 20～30min：90%A, 30～35：90% → 70%)；30 DEG C of column temperature；Flow velocity 1.0mlmin-1, Detection wavelength 205nm.External standard method peak area quantification.
It is prepared by reference substance solution：Weigh and make every 1ml in 60 DEG C of drying under reduced pressure hederagenin of 4 hours, oleanolic acid reference substance, plus methyl alcohol and obtain final product containing the concentration of 20ug.
It is prepared by need testing solution：Chinese medicinal composition preparation content 1ml, plus 2mol/L hydrochloric acid solution 30ml are measured, is heated to reflux 3 hours, cooled down immediately, in moving into separatory funnel, plus ethyl acetate shaking is extracted 3 times, each 15ml, combined ethyl acetate liquid, it is evaporated, plus methyl alcohol dissolving, in being transferred to 5ml measuring bottles, constant volume is obtained final product.
Determination method：Reference substance solution and each 10ul of need testing solution are drawn respectively, liquid chromatograph is injected, is determined, obtain final product.
Per milliliter gram must not be less than 0.70mg containing the root of Chinese clematis in terms of hederagenin in Chinese medicine composition oral liquid of the present invention, and 0.25mg must not be less than in terms of oleanolic acid.
The content assaying method of the claims, it is characterised in that wherein methyl alcohol can be substituted with 70% ethanol or ethyl acetate.
The content assaying method of the claims, it is characterised in that wherein ultrasonic processing method can be substituted with reflux extraction method.
The content assaying method of the claims, it is characterised in that wherein ultrasonic processing method can be substituted with reflux extraction method.
The content assaying method of the claims, it is characterised in that the wherein phosphoric acid of mobile phase acetonitrile -0.1% can be substituted with acetonitrile-water.
Application of the Chinese medicine composition in the infectious cough medicine for the treatment of is prepared.
Application of the Chinese medicine composition in all kinds of chronic cough medicines are prepared.
Following pharmaceutical test example is used to further illustrating but being not limited to the present invention.
Experimental example 1：Carry and whether need before oil immersion investigation
Totally 2 parts of medicinal material 170g is weighed by prescription, 10 times of water are added, with extraction by steam distillation volatile oil, portion immersion, another does not soak.The volatilization oil mass collected after 10h see the table below, it can be seen that it is 0.56ml that volatile oil total amount is collected in medicinal material immersion from table 1 below, and it is 0.48ml not soak collection volatile oil total amount.Therefore, medicinal material is carried and need before oil immersion.
Whether table 1 soaks the impact to oil mass of volatilizing
Experimental example 2：The multiple that adds water is investigated
Totally 4 parts of medicinal material 170g is weighed by prescription, 8,10,12,14 times of water are separately added into, volatile oil is extracted with steam distillation, add up to extract volatilization oil mass in observation 10h.Table 2 for difference add water multiple when volatile oil extracted amount.
Table 2 add water multiple to volatilize oil mass impact
In the total amount of oil extract of volatilizing from table, add water 12 times not soaking and put forward volatilization oil mass for 0.51ml, oil mass is put forward better than remaining multiple that adds water, and after extracting 7 hours, volatilization oil mass is 0.51ml or so, does not increase substantially, therefore the optimum process of extraction volatile oil is defined as plus 12 times of water of medicinal material amount, do not soak, carry the oily time 7 hours.
Experimental example 3：Optimal extraction technology is studied
After determining prescription medicinal material extract volatile oil, the dregs of a decoction carry out again decocting and boil.Decocting process parameter optimizing adopts orthogonal design, with hederagenin, the rate of transform of oleanolic acid and paste-forming rate as index, selects water extraction time, water extraction number of times, the multiple that adds water to carry out extraction process by water investigation.The results are shown in Table 3, table 4.
The factor level of the extraction process by water of table 3
Table2-6 Factors and levels of water extraction of compound radix clematidis sprays
The orthonormal design of experiments result table of table 4
Analyzed by orthogonal experiment data result, it is found that water extracts the factor primary and secondary order of the hederagenin rate of transform in the impact root of Chinese clematis in experiment and is：Number of times ＞ amount of water ＞ times, i.e. impact of the extraction time to the hederagenin rate of transform in the root of Chinese clematis is most notable, and amount of water takes second place, and extraction time affects minimum.Change of three factors in 3 levels is investigated, the average of 3 levels of 3 levels, the level of number of times factor 3 and amount of water of time factor is maximum, is optimal conditions, therefore determine that optimum process condition, to add water to cook 3 times, 2 hours every time, adds water 10 times and measures.
Experimental example 4：Alcohol precipitation process is studied
Using orthogonal design, with hederagenin as index, concentrate concentration, alcohol deposition fraction, time of repose is selected to carry out alcohol precipitation process investigation, factor level is shown in Table 5, table 6.
The factor level of the alcohol precipitation experimental study of table 5
The orthonormal design of experiments result table of table 6
Analyzed by orthogonal experiment data result, the factor primary and secondary order for finding the hederagenin rate of transform in the impact root of Chinese clematis in alcohol precipitation experiment is：Concentrate concentration ＞ time of repose ＞ alcohol precipitation volume fractions, i.e. impact of the concentrate concentration to the hederagenin rate of transform in the root of Chinese clematis is most notable, and time of repose takes second place, and alcohol precipitation volume fraction affects minimum.Investigate change of three factors in 3 levels, the average of 1 level of 2 levels, the level of alcohol precipitation volume fraction factor 1 and time of repose of concentrate concentration factor is maximum, for optimal conditions, therefore determine that optimum process condition is that concentrate concentration (g/ml) is 1.0, determining alcohol is 60%, and time of repose is 12 hours.
Experimental example 5：The selection of flavouring and consumption
Because this Traditional Chinese medicine composition liquid medicine taste bitterness is difficult to swallow, and tongue has obvious thick and heavy sense after pharynx clothes, therefore need to consider to add appropriate flavouring, to improve preparation mouthfeel, improves patient medication degree of complying with.In the selection of flavouring, mouthfeel is slightly worse after the flavoring such as sucrose and honey, brown sugar, Aspartame, final choice stevioside, and many people of Jing taste, and its consumption is screened.It is convenient prescription that final choice adds 0.33% stevioside.The results are shown in Table 7.
The stevioside consumption the selection result of table 7
Experimental example 6：The screening of preservative
For avoid microorganism pollution cause it is rotten, become sour, Chinese medicine extract often needs to add appropriate preservative.Sodium Benzoate has no toxic side effect, good in taste, is the preferable preservative of liquid preparation of Chinese medicine.According to by Sodium Benzoate as anti-corrosion Liu common dose, Jing trial tests determine its consumption be 0.30%.
Experimental example 7：The Qualitive test of main component contained by the root of Chinese clematis
Chinese medicinal composition preparation 2mL for taking the present invention is placed in round bottom sesame seed cake, adds the HCl 30mL of 2mol/L, water-bath to flow back 2 hours, it is placed in after cooling in separatory funnel, adds ethyl acetate to extract 3 times, each 15mL, combining extraction liquid pressurization is evaporated, methanol constant volume to 10mL, as need testing solution.
Separately take oleanolic acid and the normal aglycon reference substance of ivy soap plus methyl alcohol makes every 1mL containing 1mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether-ethyl acetate-formic acid (10: 3: 0.1) as solvent, lamellae puts presaturation 30 minutes in expansion cylinder, launches, take out, dry, spray with 10% ethanol solution of sulfuric acid, be heated to spot development at 105 DEG C clear.In test sample chromatogram, on position corresponding with reference substance chromatogram, show the spot of same color.
Experimental example 8：The discriminating of main component contained by peppermint
Chinese medicinal composition preparation 2mL for taking the present invention is placed in separatory funnel, and addition petroleum ether extraction 3 times, each 5mL merges ether, 2mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.
Peppermint control medicinal material is separately taken, 40 mesh sieves were crushed, 0.5g plus 10mL petroleum ethers ultrasound 30min is taken, after filtration, filtrate is evaporated and is settled to 1mL, used as control medicinal material solution.
Separately take menthol reference substance plus methyl alcohol makes every 1ml containing 2mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 2 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (8: 18) as solvent, after presaturation 30min, launch, take out, dry, spray with 2% vanillin-sulfuric acid-ethanol (1: 4) developer, 105 DEG C to be heated to spot development clear.In test sample chromatogram, on position corresponding with reference substance, control medicinal material chromatogram, show the spot of same color.
Experimental example 9：The discriminating of main component contained by root tuber of aromatic turmeric
Chinese medicinal composition preparation 2mL of the present invention is taken, absolute ethyl alcohol 25mL ultrasound 15min are added, filtration, decompression and solvent recovery, residue 1mL ethanol dissolves, used as need testing solution.
Root tuber of aromatic turmeric control medicinal material is separately taken, 40 mesh sieves were crushed, 2g, plus 25mL EtOH Sonicate 30min is taken, is filtered, be settled to 1mL as control medicinal material solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-Ethyl formate (15: 5) as solvent, after presaturation 30min, launch, taking-up is dried, with 10% concentrated sulfuric acid ethanol developer, 105 DEG C to be heated to spot development clear for spray.In test sample chromatogram, on position corresponding with control medicinal material chromatogram, show the spot of same color.
Experimental example 10：The discriminating of main component contained by grass-leaved sweetflag
Chinese medicinal composition preparation 5mL for taking the present invention is placed in separatory funnel, and addition petroleum ether extraction 3 times, each 5mL merges ether, 5mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.
Grass-leaved sweetflag control medicinal material is separately taken, 40 mesh sieves were crushed, 1g, plus 10mL ether ultrasound 30min is taken, after filtration, filtrate is evaporated and is settled to 1mL, used as need testing solution.
Separately take α-asarone reference substance plus methyl alcohol is prepared into every mL containing 2mg, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, draw each 1-5 μ l of above two solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-ethyl acetate (6: 4) as solvent, after presaturation 30min, launch, take out, dry, put and inspected under ultraviolet lamp (365nm).In test sample chromatogram, on position corresponding with reference substance solution chromatogram, show the spot of same color.
Experimental example 11：Hederagenin, content of oleanolic acid determination experiment in Chinese medicinal composition preparation
The selection of Detection wavelength：Take mixed reference substance solution appropriate, in 200-400nm wavelength UV scanning is carried out, three compositions have characteristic absorption at 205nm wavelength, therefore select 205nm as Detection wavelength.
Chromatographic determination condition：The phosphoric acid (B) of acetonitrile (A) -0.1%, gradient elution (0～15min：70%A, 15～20min：70% → 90%A, 20～30min：90%A, 30～35：90% → 70%)；30 DEG C of column temperature；Flow velocity 1.0mlmin-1；Sample size 10uL；Flow velocity 1ml/min, 30 DEG C of column temperature, theoretical cam curve must not be less than 1000 based on hederagenin, oleanolic acid.
Linear relationship is investigated：
Precision weighs hederagenin, oleanolic acid reference substance 5.73mg, in 25ml volumetric flasks, chromatogram methanol constant volume, it is accurate respectively to draw 8ml, 6ml, 4ml, 2ml, 1ml, in 10ml volumetric flasks, chromatogram methanol constant volume to scale crosses 0.22 μm of organic filter membrane, peak area is determined by above-mentioned chromatographic condition with 10 μ l injection high performance liquid chromatographs, with integrating peak areas value as ordinate, respectively with hederagenin, oleanolic acid sample size (ug) as abscissa, calibration curve is drawn, regression equation is calculated, 8 are the results are shown in Table.
The hederagenin of table 8, oleanolic acid linear relationship are investigated
Calibration curve：Hederagenin Y=6E+0.6X+40997, R2=0.9999；Calibration curve：Oleanolic acid Y=6E+0.6X+61056, R2=0.9996；
Reappearance test：
Precision draws the Chinese medicinal composition preparation sample 2ml of the present invention, parallel 8 parts, is separately added into 2mol/L 30mlHCL, it is heated to reflux 2h, separatory funnel is transferred to after cooling, 5 times is extracted with ethyl acetate, combining extraction liquid, recycling design, decompression receives dry, and residue chromatogram methyl alcohol dissolves, and transfer is settled to 10ml, 0.22 μm of organic filter membrane is crossed, peak area is determined by above-mentioned chromatographic condition with 10 μ l injection high performance liquid chromatographs.
The hederagenin of table 9, oleanolic acid repeatability are investigated
Conclusion：Hederagenin, the RSD values of oleanolic acid are respectively less than 5%, illustrate that the method repeatability is good.
Precision test：
Precision draws the above-mentioned μ L of 8 solution of reappearance laboratory sample 10, repeats sample introduction 6 times, tries to achieve hederagenin, oleanolic acid peak area relative standard deviation RSD ＜ 1%.The results are shown in Table 10.
The hederagenin Precision test result of table 10
Stability test
Precision draws the above-mentioned μ L of reappearance laboratory sample 10, respectively at 0,2,4,6,10,12 sample introductions 1 time, and common sample introduction 6 times, measurement result is shown in Table 11, and with hederagenin and oleanolic acid peak area sample stability is investigated.
The hederagenin of table 11, oleanolic acid stability test
Conclusion：In 12h, RSD values are less than 1% to hederagenin, the oleanolic acid peak area of same sample, illustrate that need testing solution is stable in 12 hours.
Recovery test：
Result is investigated by repeatability, the content of hederagenin is 0.90mg/ml；Content of oleanolic acid is 0.40mg/ml.Therefore, precision weighs hederagenin 9.40mg and oleanolic acid 4.00mg in 10ml volumetric flasks, chromatogram methanol constant volume so as to fully dissolving, must mix mark solution.
Precision draws above-mentioned mixed mark solution 1ml in triangular flask, parallel 7 parts, adds test agent in the accurate 1ml for drawing, 2mol/L 30mlHCL are added, 2h is heated to reflux, separatory funnel is transferred to after cooling, it is extracted with ethyl acetate 5 times, every time 15ml, combining extraction liquid, reduce pressure and receive dry solvent, residue chromatogram methyl alcohol dissolves, 10ml is settled to, 0.22 μm of organic filter membrane is crossed, peak area is determined by above-mentioned chromatographic condition with 10 μ l injection high performance liquid chromatographs.
Average recovery is calculated as follows：
The hederagenin of table 12, the oleanolic acid rate of recovery
Conclusion：Between 95%-105%, RSD values are respectively less than 5% to the average recovery of 6 parts of samples, illustrate that the method is reliable and stable, can be used for the assay of hederagenin and oleanolic acid in Chinese medicine composition of the present invention.
Below pharmacodynamic experiment result is used to further illustrating but being not limited to the present invention.
Experimental example 11：Cough-relieving drug effect Germicidal efficacy
1st, experiment purpose：Cause to cough test by ammonia spraying, compare its antitussive action.
2nd, experiment material
The technique one of 2.1 test medicine pectoral, technique two, technique three, are provided by centers for making of pharmaceutical preparations of Institute Of Chinese Materia Medica Of China Academy of Chinese Medical Sciences, and content is 1.0g crude drugs/ml.
2.2 animal CD-1 (ICR) mouse, 18-22g is provided by Beijing Vital River Experimental Animals Technology Co., Ltd., and quality certification number is SCXK (capital) 2012-0001.
2.3 reagent ammoniacal liquor, Chemical Reagent Co., Ltd., Sinopharm Group, lot number：20120918.
2.4 instrument 402A ultrasonic atomizers, Yuyue Medical Apparatus Co., Ltd., Jiangsu produces.
2.5 animal packet
Take healthy mice and be randomly divided into 10 groups by body weight, respectively model control group, the high, medium and low dosage group of the medicine of embodiment 1, the high, medium and low dosage group of embodiment 2, the high, medium and low dosage group of embodiment 3,10 per group, male and female half and half.
3rd, experimental technique
Cause to cough method using ammonia spraying, embodiment 1, embodiment 2, the medicine of embodiment 3 give mouse with 12.54,6.27,3.14g crude drugs/kg gavages respectively, test by antibechic, compare its antitussive action.Each group gives relative medicine by only gavage, gavage volume is 20ml/kg, model control group gavage gives the distilled water of same volume, 1 hour after administration, by mouse by being only put in the glass beaker of 1000ml specifications, add a cover above, contain in atomizing cup into 12.5% ammoniacal liquor 40ml, atomizer pipe connects atomizer and glass beaker, certain power of mist amount is sent to start shooting with moderate air-supply and maximum, spraying stops for 5 seconds, observes and records and causes (cough latent period) and number of times of coughing in 2 minutes the time required to mouse cough, carries out comparing between group with t inspections.
4th, experimental result
The ammonia spraying of table 13 causes the impact of mouse cough
Note：The * P ＜ 0.05 compared with control group；* P ＜ 0.01
5th, cough-relieving drug effect observation experiment conclusion
Result of the test is visible, and high, medium and low three dosage groups of Chinese medicine composition embodiment 1 of the present invention and height, the middle dose group of embodiment 2,3 can be obviously prolonged mouse cough incubation period；The high, medium and low dosage group of embodiment 1, the height of the high dose group of embodiment 2 and embodiment 3, middle dose group can obviously reduce mouse cough number of times, with significant difference compared with model control group.
Specific embodiment：
Embodiment 1：The preparation of oral liquid
Medicinal material root of Chinese clematis 300g, root tuber of aromatic turmeric 250g, grass-leaved sweetflag 150g, peppermint 150g, add 10 times of water, volatile oil is extracted with steam distillation, volatile oil is collected after 8h standby, oily mother liquor will be carried and leached, the dregs of a decoction add 10 times of amount decoctings to boil 1h, filtration, filtrate merges with oily mother liquor is carried, and 20min is centrifuged with 3500r/min, removes precipitation.95% ethanol is added to make alcohol content up to 65% after concentration, refrigeration is taken out after standing overnight, filtration, decompression filtrate recycling ethanol, plus Tween 80 solubilising volatile oil, and be well mixed with flavouring (such as sucrose, honey, xylitol, stevioside one or more), preservative (such as sodium sorbate or sylvite, benzoic acid one or more) and liquid, 1000ml is settled to, it is filling to obtain final product.
Embodiment 2：The preparation of conventional tablet
Medicinal material root of Chinese clematis 150g, root tuber of aromatic turmeric 375g, grass-leaved sweetflag 150g, peppermint 225g, add 10 times of amount water, with extraction by steam distillation volatile oil, collect within 7 hours volatile oil standby, oily mother liquor will be carried and leached, the dregs of a decoction add 8 times of 60% ethanol of amount, backflow 2 times, every time 1h, alcohol extract merging, reclaim ethanol to without alcohol taste, after standing overnight, suction filtration will be precipitated and removed, and is concentrated to dryness, and be crushed.Volatile oil is included with beta cyclodextrin, refrigerated overnight, filtration, and low temperature drying adds dextrin, Icing Sugar and magnesium stearate, mixes with extract powder, and granulation is pressed into 1000 and obtains final product.
Embodiment 3：The preparation of spray
Medicinal material grass-leaved sweetflag 225g, peppermint 75g add 14 times of water, with extraction by steam distillation volatile oil, collect volatile oil within 7 hours standby, oily mother liquor will be carried to leach, the dregs of a decoction add 10 times of water, decoct 1 hour, after decoction liquor is filtered with carry oily mother liquor and merge, precipitation is removed with 3500r/min centrifugation 20min, 95% ethanol is added to make alcohol content up to 65% after supernatant concentration, refrigeration is taken out after standing overnight, filtration, decompression filtrate recycling ethanol, refrigerates standby.
Root of Chinese clematis 375g, root tuber of aromatic turmeric 300g add 6 times of 70% ethanol of amount, and twice, each 1h merges alcohol extract, reclaims ethanol for backflow.And merge with liquid after grass-leaved sweetflag, peppermint water extract-alcohol precipitation, reduced pressure concentration.Plus be well mixed with liquid after Tween 80 solubilising volatile oil, 1000ml is settled to, it is filling to obtain final product
Embodiment 4：The preparation of spray
Root of Chinese clematis 500g, root tuber of aromatic turmeric 375g, grass-leaved sweetflag 75g, peppermint 225g, plus 10 times amount 70% alcohol refluxs extract 3 times, every time 3 hours, extract merges, and filters, and filtrate adds 0.05% ethylparaben, 1.5% stevioside, 1000ml is settled to, in being sub-packed in spray bottle, sterilizing, thus obtaining the product.
Embodiment 5：The preparation of buccal tablet
Medicinal material root of Chinese clematis 150g, root tuber of aromatic turmeric 375g, grass-leaved sweetflag 150g, peppermint 225g, add 10 times of amount water, with extraction by steam distillation volatile oil, collect volatile oil within 7 hours, dissolve standby with a small amount of ethanol；Oily mother liquor will be carried to leach, the dregs of a decoction add 8 times of 60% ethanol of amount, flow back 2 times, each 1h, alcohol extract merges, and reclaims ethanol to concentrate without alcohol taste, is obtained, and adds appropriate mannitol, Aspartame, magnesium stearate and volatile oil ethanol solution, mix, granulation is pressed into 1000 and obtains final product.
Embodiment 6：The application 1 of Chinese medicine inventive composition
Root of Chinese clematis 500g, root tuber of aromatic turmeric 375g, grass-leaved sweetflag 75g, peppermint 225g, dextrin 110g, superfine silica gel powder 15g make capsule 1000, for the treatment of various acute and chronics cough.
Embodiment 7：The application 2 of Chinese medicine inventive composition
Medicinal material root of Chinese clematis 300g, root tuber of aromatic turmeric 250g, grass-leaved sweetflag 150g, peppermint 150g, sucrose 90g, stevioside 5g, benzoic acid 10g, make oral liquid 1000ml, for the treatment of infectious cough.

Claims (25)

1. a kind of Chinese medicine composition for treating cough after common cold, is made up of the bulk drug of following weight portion：6-20 gram of the root of Chinese clematis, 6-20 gram of root tuber of aromatic turmeric, 3-10 gram of grass-leaved sweetflag, 3-10 gram of peppermint.
2. Chinese medicine composition according to claim 1, it is characterised in that the Chinese medicine composition by following weight portion bulk drug Composition：10 grams of the root of Chinese clematis, 10 grams of root tuber of aromatic turmeric, 6 grams of grass-leaved sweetflag, 6 grams of peppermint.
3. Chinese medicine composition according to claim 1, it is characterised in that the Chinese medicine composition by following weight portion bulk drug Composition：6 grams of the root of Chinese clematis, 15 grams of root tuber of aromatic turmeric, 6 grams of grass-leaved sweetflag, 9 grams of peppermint.
4. Chinese medicine composition according to claim 1, it is characterised in that the Chinese medicine composition by following weight portion bulk drug Composition：12 grams of the root of Chinese clematis, 10 grams of root tuber of aromatic turmeric, 6 grams of grass-leaved sweetflag, 6 grams of peppermint.
5. Chinese medicine composition according to claim 1, it is characterised in that the Chinese medicine composition by following weight portion bulk drug Composition：15 grams of the root of Chinese clematis, 12 grams of root tuber of aromatic turmeric, 9 grams of grass-leaved sweetflag, 3 grams of peppermint.
6. Chinese medicine composition according to claim 1, it is characterised in that the Chinese medicine composition by following weight portion bulk drug Composition：20 grams of the root of Chinese clematis, 15 grams of root tuber of aromatic turmeric, 3 grams of grass-leaved sweetflag, 9 grams of peppermint.
7. the Chinese medicine composition according to any claim in claim 1 to 6, it is characterised in that the Chinese medicine composition Preparation method be：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material total amount 6-12 times water, with steam distillation Method extracts volatile oil 5-9 hours, collects volatile oil, adds Tween-80 solubilising, standby；Steam distillation extract is filtered, Oily mother liquor and filter residue must be carried；Filter residue adds 6-10 times of decocting to boil 1-3 time, and each 1-3 hours merge decoction liquor and carry oily mother liquor, 75-95% ethanol will be added after supernatant concentration to make alcohol content up to 65-85%, refrigeration is taken out after standing, and is filtered, and filtrate decompression is reclaimed Ethanol is to without alcohol taste；Volatile oil and conventional pharmaceutical adjuvants after solubilising are added, using formulation method conventional in pharmacy of Chinese materia medica, Make suitable dosage forms.
8. Chinese medicine composition according to claim 7, it is characterised in that the preparation method of the Chinese medicine composition is：The root of Chinese clematis, Peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, collect Volatile oil, mother liquor is filtered, and adds Tween-80 solubilising, standby；Steam distillation extract is filtered, and must carry oily mother liquor and filter residue： Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, merges decoction liquor and carries oily mother liquor, will Jia 95% after supernatant concentration Ethanol makes alcohol content up to 65%, and refrigeration stands and taken out after 15h, filtration, and decompression filtrate recycling ethanol is to without alcohol taste；Add solubilising Volatile oil afterwards and conventional pharmaceutical adjuvants, using formulation method conventional in pharmacy of Chinese materia medica, make granule, oral tablet, Buccal tablet, dispersible tablet, hard capsule, soft capsule, oral liquid, spray, powder-type spray.
9. Chinese medicine composition oral liquid according to claim 8, it is characterised in that the preparation method of the Chinese medicine composition is： The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, little with extraction by steam distillation volatile oil 7 When, volatile oil is collected, Tween-80 solubilising is added, it is standby；Steam distillation extract is filtered, oily mother liquor and filter residue must be carried； Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, merges decoction liquor and carries oily mother liquor, will Jia 95% after supernatant concentration Ethanol makes alcohol content up to 65%, and refrigeration stands and taken out after 15h, filtration, and decompression filtrate recycling ethanol is to without alcohol taste；Add solubilising Volatile oil afterwards and simple syrup, stevioside and Sodium Benzoate, constant volume in being sub-packed in oral liquid bottle, is obtained final product.
10. the Chinese medicine composition according to any claim in claim 1 to 6, it is characterised in that the Chinese medicine composition Preparation method be：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, the 50-80% ethanol for adding medicinal material total amount 5-15 times is returned Stream is extracted, extraction time 1-4 time, each 0.5-4 hours, and alcohol extract merges, and is filtered, filtrate concentration, is added conventional medicinal auxiliary Material, using formulation method conventional in pharmacy of Chinese materia medica, makes suitable dosage forms.
11. Chinese medicine compositions according to claim 10, it is characterised in that the preparation method of the Chinese medicine composition is：Wheeling Celestial being, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, plus 70% alcohol reflux extract 2 times, 3 hours every time, alcohol extract merge, filter, Concentration, adds conventional pharmaceutical adjuvants, using formulation method conventional in pharmacy of Chinese materia medica, makes granule, oral tablet, mouth containing Piece, dispersible tablet, hard capsule, soft capsule, oral liquid, spray, powder-type spray.
12. Chinese medicine composition oral liquids according to claim 11, it is characterised in that the preparation method of the Chinese medicine composition is： The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, plus 70% alcohol reflux extract 2 times, 3 hours every time, alcohol extract merge, Filter, concentration adds simple syrup, stevioside and Sodium Benzoate, constant volume, in being sub-packed in oral liquid bottle, obtains final product.
13. Chinese medicine compositions according to any claim in claim 1 to 6, it is characterised in that the Chinese medicine composition Preparation method be：The root of Chinese clematis, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material total amount 6-12 times water, with steam distillation Method extracts volatile oil 5-9 hours, collects volatile oil, and beta-cyclodextrin inclusion compound obtains inclusion compound standby；Steam distillation is extracted Liquid is filtered, and must carry oily mother liquor and filter residue；Filter residue add 6-10 times of decocting boil 1-3 time, each 1-3 hours, merge decoction liquor and Oily mother liquor is carried, 75-95% ethanol will be added to make alcohol content up to 65-85% after supernatant concentration, refrigeration is taken out after standing, and is filtered, filter Liquid decompression recycling ethanol then proceedes to be concentrated into thick paste to without alcohol taste, is dried, and gained dried object mixes with volatile oil clathrate compound It is even, conventional pharmaceutical adjuvants are added, using formulation method conventional in pharmacy of Chinese materia medica, make suitable dosage forms.
14. Chinese medicine compositions according to claim 13, it is characterised in that the preparation method of the Chinese medicine composition is：Wheeling Celestial being, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, Volatile oil is collected, beta-cyclodextrin inclusion compound, refrigerated overnight, filtration, low temperature drying obtains Benexate Hydrochloride standby； Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, closes And decoction liquor with carry oily mother liquor, will be after supernatant concentration plus 95% ethanol makes alcohol content up to 65%, refrigeration stands and taken out after 15h, Filtration, decompression filtrate recycling ethanol then proceedes to be concentrated into thick paste to without alcohol taste, is dried, gained dried object and inclusion essential oil Thing is well mixed, and adds conventional pharmaceutical adjuvants, using formulation method conventional in pharmacy of Chinese materia medica, make granule, oral tablet, Buccal tablet, dispersible tablet, hard capsule, soft capsule, oral liquid, spray, powder-type spray.
15. Chinese medicine compositions according to claim 14, it is characterised in that the preparation method of the Chinese medicine composition is：Wheeling Celestial being, peppermint, grass-leaved sweetflag and root tuber of aromatic turmeric medicinal material, add medicinal material 12 times of water of total amount, with extraction by steam distillation volatile oil 7 hours, Volatile oil is collected, beta-cyclodextrin inclusion compound, refrigerated overnight, filtration, low temperature drying obtains Benexate Hydrochloride standby； Steam distillation extract is filtered, oily mother liquor and filter residue must be carried；Filter residue adds 10 times of decoctings to boil 3 times, 2 hours every time, closes And decoction liquor with carry oily mother liquor, will be after supernatant concentration plus 95% ethanol makes alcohol content up to 65%, refrigeration stands and taken out after 15h, Filtration, decompression filtrate recycling ethanol then proceedes to be concentrated into thick paste to without alcohol taste, is dried, gained dried object and inclusion essential oil Thing is well mixed, and adds dextrin, cane sugar powder, stevioside, essence, wet granulation, whole grain after being dried to add 0.5% stearic acid Magnesium, is mixed, and is pressed into buccal tablet and obtains final product.
The 16. Chinese medicine composition method of quality control according to any claim in claim 1 to 6, it is characterised in that The discrimination method of the Chinese medicine composition includes one or more in following method：
(1) Chinese medicinal composition preparation 2-10mL for taking the present invention is placed in round bottom sesame seed cake, adds the HCl 30-100mL of 2mol/L, Water-bath backflow 1-3 hours, are placed in separatory funnel after cooling, and add ethyl acetate to extract 1-3 time, and each 15-30mL merges Extract pressurization is evaporated, methanol constant volume to 5-10mL, as need testing solution.Separately take oleanolic acid and the normal aglycon pair of ivy soap Every 1mL is made containing 1mg, according to product plus methyl alcohol as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, each 1-5 μ l of above two solution are drawn, put respectively on same silica gel g thin-layer plate, with petroleum ether-ethyl acetate - formic acid (5-20: 1-10: 0.1-1) is solvent, and lamellae puts presaturation 30 minutes in expansion cylinder, is launched, and is taken out, and is dried, Spray is heated to spot development clear with 10% ethanol solution of sulfuric acid at 105 DEG C.In test sample chromatogram, with reference substance chromatogram phase On the position answered, show the spot of same color.
(2) Chinese medicinal composition preparation 2-10mL for taking the present invention is placed in separatory funnel, addition petroleum ether extraction 1-3 time, every time 5-15mL, merges ether, 2-10mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.Separately take peppermint comparison medicine Material, crushed 40 mesh sieves, took 0.5g plus 5-15mL petroleum ethers ultrasound 30min, and after filtration, filtrate is evaporated and is settled to 1mL, As control medicinal material solution.Separately take menthol reference substance plus methyl alcohol makes every 1ml containing 2mg, as reference substance solution.According to thin layer Chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, each 1-5 μ l of above two solution are drawn, put respectively in same silica gel On G lamellaes, with toluene-ethyl acetate (5-20: 1-5) as solvent, after presaturation 30min, launch, take out, dry, With 2% vanillin-sulfuric acid-ethanol (1: 4) developer, 105 DEG C to be heated to spot development clear for spray.In test sample chromatogram, with On reference substance, the corresponding position of control medicinal material chromatogram, show the spot of same color.
(3) Chinese medicinal composition preparation 2-10mL of the present invention is taken, absolute ethyl alcohol 25-50mL ultrasound 15-30min are added, is filtered, Decompression and solvent recovery, residue 1mL ethanol dissolves, used as need testing solution.Root tuber of aromatic turmeric control medicinal material is separately taken, 40 mesh were crushed Sieve, takes 0.5-2g, plus 5-50mL EtOH Sonicate 30min, filters, and is settled to 1mL as control medicinal material solution.According to thin layer color Spectrometry (《Chinese Pharmacopoeia》2010 editions annex VI B) test, each 1-5 μ l of above two solution are drawn, put respectively in same silica G On lamellae, with petroleum ether (60-90 DEG C)-ethyl acetate (10-30: 5-10) as solvent, after presaturation 30min, exhibition Open, taking-up is dried, spray with 10% concentrated sulfuric acid ethanol developer, 105 DEG C to be heated to spot development clear.In test sample chromatogram, On position corresponding with control medicinal material chromatogram, show the spot of same color.
(4) Chinese medicinal composition preparation 2-10mL for taking the present invention is placed in separatory funnel, addition petroleum ether extraction 1-3 time, every time 5-15mL, merges ether, 2-10mL methanol constant volumes is added after evaporated under reduced pressure, as need testing solution.Separately take grass-leaved sweetflag control Medicinal material, crushed 40 mesh sieves, took 0.5-2g, plus 10-40mL ether ultrasound 30min, and after filtration, filtrate is evaporated and is settled to 1mL, as need testing solution.Separately take α-asarone reference substance plus methyl alcohol is prepared into every mL containing 2mg, as reference substance solution. According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, each 1-5 μ l of above two solution are drawn, put in same respectively On one silica gel g thin-layer plate, with petroleum ether (60-90 DEG C)-ethyl acetate (5-20: 2-20) as solvent, presaturation 30min Afterwards, launch, take out, dry, put and inspected under ultraviolet lamp (365nm).In test sample chromatogram, with reference substance solution chromatogram phase On the position answered, show the spot of same color.
17. Chinese medicine composition method of quality control according to claim 16, it is characterised in that the discriminating of the Chinese medicine composition Method includes one or more in following method：
(1) Chinese medicinal composition preparation 2mL for taking the present invention is placed in round bottom sesame seed cake, adds the HCl 30mL of 2mol/L, water-bath Backflow 2 hours, is placed in separatory funnel after cooling, and adds ethyl acetate to extract 3 times, each 15mL, combining extraction liquid pressurization It is evaporated, methanol constant volume to 10mL, as need testing solution.Separately take oleanolic acid and the normal aglycon reference substance of ivy soap plus methyl alcohol system Contain 1mg into every 1mL, as reference substance solution.According to thin-layered chromatography (《Chinese Pharmacopoeia》2010 editions annex VI B) test, inhale The each 5 μ l of above two solution are taken, is put respectively on same silica gel g thin-layer plate, with petroleum ether-ethyl acetate-formic acid (10: 3: 0.1) For solvent, lamellae puts presaturation 30 minutes in expansion cylinder, launches, and takes out, and dries, and sprays with 10% ethanol solution of sulfuric acid, It is clear spot development to be heated at 105 DEG C.In test sample chromatogram, on position corresponding with reference substance chromatogram, show same color Spot.
(2) Chinese medicinal composition preparation 2mL for taking the present invention is placed in separatory funnel, addition petroleum ether extraction 3 times, each 5mL, Merge ether, 2mL methanol constant volumes are added after evaporated under reduced pressure, as need testing solution.Peppermint control medicinal material is separately taken, 40 were crushed Mesh sieve, takes 0.5g plus 10mL petroleum ethers ultrasound 30min, and after filtration, filtrate is evaporated and is settled to 1mL, used as control medicinal material Solution.Separately take menthol reference substance plus methyl alcohol makes every 1ml containing 2mg, as reference substance solution.According to thin-layered chromatography (《China Pharmacopeia》2010 editions annex VI B) test, each 2 μ l of above two solution are drawn, put respectively on same silica gel g thin-layer plate, with Toluene-ethyl acetate (8: 18) is solvent, after presaturation 30mmin, is launched, and is taken out, and is dried, and is sprayed with 2% vanillic aldehyde sulphur Acid-ethanol (1: 4) developer, 105 DEG C to be heated to spot development clear.In test sample chromatogram, with reference substance, control medicinal material On the corresponding position of chromatogram, show the spot of same color.
(3) Chinese medicinal composition preparation 2mL of the present invention is taken, adds absolute ethyl alcohol 25mL ultrasound 15min, filtration to reduce pressure back Solvent is received, residue 1mL ethanol dissolves, used as need testing solution.Root tuber of aromatic turmeric control medicinal material is separately taken, 40 mesh sieves were crushed, is taken 2g, plus 25mL EtOH Sonicate 30min, filter, and are settled to 1mL as control medicinal material solution.According to thin-layered chromatography (《China Pharmacopeia》2010 editions annex VI B) test, each 1-5 μ l of above two solution are drawn, put respectively on same silica gel g thin-layer plate, With petroleum ether (60-90 DEG C)-Ethyl formate (15: 5) as solvent, after presaturation 30min, launch, taking-up is dried, and is sprayed With 10% concentrated sulfuric acid ethanol developer, 105 DEG C to be heated to spot development clear.In test sample chromatogram, with control medicinal material chromatogram phase On the position answered, show the spot of same color.
(4) Chinese medicinal composition preparation 5mL for taking the present invention is placed in separatory funnel, addition petroleum ether extraction 3 times, each 5mL, Merge ether, 5mL methanol constant volumes are added after evaporated under reduced pressure, as need testing solution.Grass-leaved sweetflag control medicinal material is separately taken, was crushed 40 mesh sieves, take 1g, plus 10mL ether ultrasound 30min, and after filtration, filtrate is evaporated and is settled to 1mL, molten as test sample Liquid.Separately take α-asarone reference substance plus methyl alcohol is prepared into every mL containing 2mg, as reference substance solution.According to thin-layered chromatography (《In State's pharmacopeia》2010 editions annex VI B) test, each 1-5 μ l of above two solution are drawn, put respectively on same silica gel g thin-layer plate, With petroleum ether (60-90 DEG C)-ethyl acetate (6: 4) as solvent, after presaturation 30min, launch, take out, dry, Put and inspected under ultraviolet lamp (365nm).In test sample chromatogram, on position corresponding with reference substance solution chromatogram, show same color Spot.
The 18. Chinese medicine composition method of quality control according to any claim in claim 1 to 6, it is characterised in that The assay of the Chinese medicine composition include following assay method:
Chromatographic condition：Octadecylsilane chemically bonded silica is filler；Mobile phase is acetonitrile (A) -0.1-0.5% phosphoric acid (B), Gradient elution (0～15min：70%A, 15～20min：70% → 90%A, 20～30min：90%A, 30～35：90% → 70%)； 30 DEG C of column temperature；Flow velocity 1.0mlmin-1, Detection wavelength 205nm.External standard method peak area quantification.
It is prepared by reference substance solution：Hederagenin, the oleanolic acid reference substance in 60 DEG C of drying under reduced pressure 3-5 hours is weighed, plus Methyl alcohol is made concentration of every 1ml containing 20ug and is obtained final product.
It is prepared by need testing solution：Chinese medicinal composition preparation content 1-5ml, plus 2mol/L hydrochloric acid solution 10-50ml are measured, plus Heat backflow 1-3 hours, cool down immediately, and in moving into separatory funnel, plus ethyl acetate shaking is extracted 1-3 time, each 10-30ml, Combined ethyl acetate liquid, is evaporated, plus methyl alcohol dissolving, and in being transferred to 5ml measuring bottles, constant volume is obtained final product.
Determination method：Reference substance solution and each 10ul of need testing solution are drawn respectively, liquid chromatograph is injected, is determined, obtain final product.
Per milliliter gram must not be less than containing the root of Chinese clematis in terms of hederagenin in the oral liquid of Chinese medicine composition of the present invention 0.60-1.00mg, must not be less than 0.10-0.40mg in terms of oleanolic acid.
19. content assaying methods according to claim 18, it is characterised in that the method includes following assay method：
Chromatographic condition：Octadecylsilane chemically bonded silica is filler；Mobile phase be the phosphoric acid (B) of acetonitrile (A) -0.1%, gradient Wash-out (0～15min：70%A, 15～20min：70% → 90%A, 20～30min：90%A, 30～35：90% → 70%)；Post 30 DEG C of temperature；Flow velocity 1.0mlmin-1, Detection wavelength 205nm.External standard method peak area quantification.
It is prepared by reference substance solution：Weigh in 60 DEG C of drying under reduced pressure hederagenin of 4 hours, oleanolic acid reference substance, plus first Alcohol is made concentration of every 1m1 containing 20ug and is obtained final product.
It is prepared by need testing solution：Chinese medicinal composition preparation content 1ml, plus 2mol/L hydrochloric acid solution 30ml are measured, is heated back Stream 3 hours, cools down immediately, and in moving into separatory funnel, plus ethyl acetate shaking is extracted 3 times, and each 15ml merges acetic acid second Ester liquid, is evaporated, plus methyl alcohol dissolving, and in being transferred to 5ml measuring bottles, constant volume is obtained final product.
Determination method：Reference substance solution and each 10ul of need testing solution are drawn respectively, liquid chromatograph is injected, is determined, obtain final product.
Per milliliter gram must not be less than 0.70mg containing the root of Chinese clematis in terms of hederagenin in the oral liquid of Chinese medicine composition of the present invention, with Oleanolic acid meter must not be less than 0.25mg.
20. content assaying methods as described in claim 18 or 19, it is characterised in that wherein methyl alcohol can with 70% ethanol or Ethyl acetate is substituted.
21. content assaying methods as described in claim 18 or 19, it is characterised in that wherein ultrasonic processing method can be used back Stream extracting method is substituted.
22. content assaying methods as described in claim 18 or 19, it is characterised in that wherein mobile phase ultrasonic processing method can To be substituted with reflux extraction method.
23. content assaying methods as described in claim 18 or 19, it is characterised in that the wherein phosphoric acid of mobile phase acetonitrile -0.1% Can be substituted with acetonitrile-water.
24. Chinese medicine compositions according to any claim in claim 1 to 6, it is characterised in that the Chinese medicine composition exists Prepare the application in the infectious cough medicine for the treatment of.
25. Chinese medicine compositions according to any claim in claim 1 to 6, it is characterised in that the Chinese medicine composition Application in all kinds of chronic cough medicines for the treatment of are prepared.
CN201510708038.9A 2015-10-28 2015-10-28 Preparation method, quality control and use of traditional Chinese medicine composition for treating postinfectious cough Pending CN106620498A (en)

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