CN109692291A - Lung power cough mixture medicinal extract and application thereof and method of quality control - Google Patents

Lung power cough mixture medicinal extract and application thereof and method of quality control Download PDF

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CN109692291A
CN109692291A CN201910165137.5A CN201910165137A CN109692291A CN 109692291 A CN109692291 A CN 109692291A CN 201910165137 A CN201910165137 A CN 201910165137A CN 109692291 A CN109692291 A CN 109692291A
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solution
medicinal extract
lung power
cough mixture
medicinal material
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孙小鸚
廖萍
廖伟
廖忠
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JIANXING MEDICAL INDUSTRY Co Ltd GUIZHOU
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JIANXING MEDICAL INDUSTRY Co Ltd GUIZHOU
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Abstract

The present invention relates to lung power cough mixture medicinal extract and application thereof and method of quality control, a kind of lung power cough mixture medicinal extract, it is specific the preparation method comprises the following steps: taking radix scutellariae by prescription, the root of purple-flowered peucedanum, the tuber of stemona, red gentian, phoenix tree root, oldenlandia diffusa, aster, radix scutellariae be crushed into 16mm sieve plate, then boiling water is added to decoct with other 6 taste medicines secondary, the boiling water that addition for the first time is equivalent to 7 times of medicinal material weight decocts 2 hours, the boiling water that second of addition is equivalent to 4 times of medicinal material weight decocts 1.5 hours, merge decoction liquor, filtering, filtrate is concentrated into the clear cream that relative density is 1.03~1.05 (80 DEG C), to obtain the final product, this method can be sufficiently reserved effective component；The invention also discloses the method for quality control of lung power cough mixture medicinal extract, can preferably control product quality.

Description

Lung power cough mixture medicinal extract and application thereof and method of quality control
Technical field
The invention belongs to pharmaceutical fields, are related to lung power cough mixture medicinal extract and application thereof and pharmaceutical composition, and lung power cough The method of quality control of mixture medicinal extract.
Background technique
Respiratory disease is a kind of common disease, and frequently-occurring disease, disease incidence is relatively high in old, children, is shown as after the onset It coughs, breathe, unsmooth breath, abundant expectoration, some meetings are lain awake all night, and the health of patient is influenced, and some also jeopardizes patient vitals. Lung power cough mixture medicinal extract is using prescription as radix scutellariae 29g, root of purple-flowered peucedanum 28g, tuber of stemona 28g, red gentian 28g, phoenix tree root 26g, agkistrodon Tongue grass 25g, aster 23g, are concentrated after extracted and are made, have a better effect to above-mentioned illness tool.But lung power cough is closed at present The preparation method disunity of agent medicinal extract, and the rate of transform of scutelloside is low, with 1g containing radix scutellariae with scutelloside (C21H18O11) meter, it is less than 3.5mg, also massless standard of perfection.
Therefore, secondary development is carried out to it to obtain curative effect stable lung power cough mixture medicinal extract urgent need, obtains a kind of quality Stable lung power cough mixture medicinal extract, and establish the method controlled lung power cough mixture medicinal extract quality.
Summary of the invention
In view of this, one of the objects of the present invention is to provide lung power cough mixture medicinal extract；The second object of the present invention is The purposes and its pharmaceutical composition of lung power cough mixture medicinal extract are provided；The third object of the present invention is to provide lung power cough mixture medicinal extract Preparation method；The fourth object of the present invention is to provide the method for quality control of lung power cough mixture medicinal extract.
For achieving the above object, the invention provides the following technical scheme:
A kind of lung power cough mixture medicinal extract, is prepared by including the following steps: taking radix scutellariae, the root of purple-flowered peucedanum, the tuber of stemona, safflower dragon by prescription Radix scutellariae crushed 16mm sieve plate by gallbladder, phoenix tree root, oldenlandia diffusa, aster, and boiling water is then added to decoct two with other 6 taste medicines Secondary, the boiling water that addition for the first time is equivalent to 7 times of medicinal material weight decocts 2 hours, and second of addition is equivalent to 4 times of medicinal material weight of boiling Water decocts 1.5 hours, merges decoction liquor, filtering, and filtrate is concentrated into the clear cream that relative density is 1.03~1.05 (80 DEG C), i.e., ?.In a preferred technical solution, radix scutellariae 29g, root of purple-flowered peucedanum 28g, tuber of stemona 28g, red gentian 28g, phoenix tree root 26g, agkistrodon Tongue grass 25g, aster 23g.
A kind of lung power cough composition medicine composition, it includes previously described lung power cough mixture medicinal extract and pharmaceutically acceptable auxiliaries.
Previously described lung power cough mixture medicinal extract is used to prepare the purposes of lung power cough mixture.
The preparation method of lung power cough mixture medicinal extract includes the following steps: to take radix scutellariae, the root of purple-flowered peucedanum, the tuber of stemona, safflower dragon by prescription Radix scutellariae crushed 16mm sieve plate by gallbladder, phoenix tree root, oldenlandia diffusa, aster, and boiling water is then added to decoct two with other 6 taste medicines Secondary, the boiling water that addition for the first time is equivalent to 7 times of medicinal material weight decocts 2 hours, and second of addition is equivalent to 4 times of medicinal material weight of boiling Water decocts 1.5 hours, merges decoction liquor, filters, and filtrate is concentrated into the clear cream that relative density is 1.03~1.05 (80 DEG C), i.e., ?.Preferably, wherein radix scutellariae 29g, root of purple-flowered peucedanum 28g, tuber of stemona 28g, red gentian 28g, phoenix tree root 26g, oldenlandia diffusa 25g, red Pipe medicine 23g.
The lung power cough mixture medicinal extract as made from above-mentioned preparation method.
The method of quality control of above-mentioned lung power cough mixture medicinal extract, including root of purple-flowered peucedanum identification, tuber of stemona identification and content of baicalin inspection It surveys:
The root of purple-flowered peucedanum identification specifically: take lung power cough mixture medicinal extract to be diluted with water, then with extracted by ether at least 2 times, close And ether solution, it is evaporated, residue adds ethyl acetate to dissolve, as test solution；Root of purple-flowered peucedanum control medicinal material separately is taken, adds diethyl ether and heats back Stream extracts, and filters, and filtrate is evaporated, and residue adds ethyl acetate to make to dissolve, as control medicinal material solution；Draw test solution and Control medicinal material solution is put respectively on same silica gel g thin-layer plate, using toluene-ethyl acetate as solvent, is unfolded, takes out, dry in the air Sodium hydroxide solution dry, that spray is 10% with mass fraction, sets and inspects under 365nm ultraviolet lamp, in sample chromatogram, with compare On the corresponding position of medicinal material chromatography, the fluorescence spot of same color is shown；
The tuber of stemona identification specifically: take lung power cough mixture medicinal extract to be diluted with water, adjust pH value to 10, with two with ammonia solution Chloromethanes shaking is extracted at least 2 times, is merged dichloromethane solution, is evaporated, residue adds methanol to dissolve, as test solution；Separately take Tuber of stemona control medicinal material, ammonification test solution make to moisten, place, add methylene chloride, be ultrasonically treated, filter, and filtrate is evaporated, and residue adds first Alcohol dissolution, as control medicinal material solution；Test solution and control medicinal material solution are drawn, is put respectively on same silicon G lamellae, It is solvent with toluene-acetone-methanol-, sets in the pre-saturated expansion cylinder of ammonia steam, presaturation 30 minutes, is unfolded, takes out, dry in the air Dry, spray in sample chromatogram, on position corresponding with reference medicine chromatography, shows same color with dilute bismuth potassium iodide test solution Spot；
The content of baicalin detection are as follows: take lung power cough mixture medicinal extract, add ethanol solution, be ultrasonically treated, let cool, add second Alcoholic solution shakes up, and filtering takes subsequent filtrate；Accurately weighed scutelloside reference substance, adds methanol to dissolve, and is configured to every 1ml and contains The reference substance solution of 0.070mg；It is accurate respectively to draw reference substance solution and test solution, liquid chromatograph is injected, with ten Eight alkyl silane bonded silica gels are the chromatographic column of filler；Methanol-water-phosphoric acid is mobile phase；It is surveyed under the conditions of wavelength is 280nm It is fixed.
Preferably, the root of purple-flowered peucedanum identification specifically: taking lung power cough mixture medicinal extract to be diluted with water to concentration is 1mg/ml, uses second Ether proposes 2 times, each 25ml, merges ether solution, is evaporated, residue adds ethyl acetate 1ml to make to dissolve, as test solution；Separately Root of purple-flowered peucedanum control medicinal material 1g is taken, add diethyl ether 20ml, is heated to reflux 30 minutes, filters, and filtrate is evaporated, and residue adds ethyl acetate 1ml to make Dissolution, as control medicinal material solution；Test solution and each 5~10 μ l of control medicinal material solution are drawn, is put respectively in same silica G It is 3:2 toluene-ethyl acetate as solvent using volume ratio on lamellae, is unfolded, taking out, drying, spray is with mass fraction for 10% Sodium hydroxide solution, set and inspected under 365nm ultraviolet lamp, in sample chromatogram, on position corresponding with reference medicine chromatography, The fluorescence spot of aobvious same color.
Preferably, the tuber of stemona identification specifically: taking lung power cough mixture medicinal extract to be diluted with water to concentration is 1mg/ml, uses ammonia Test solution adjusts pH value to 10, is extracted 2 times, each 25ml with methylene chloride shaking, merges dichloromethane solution, be evaporated, residue adds first Alcohol 1ml makes to dissolve, as test solution；Tuber of stemona control medicinal material 2g is separately taken, ammonification test solution makes to moisten, places 10 minutes, add two Chloromethanes 20ml is ultrasonically treated 30 minutes, and filtering, filtrate is evaporated, and residue adds methanol 1ml to make to dissolve, as control medicinal material solution； Test solution and each 10 μ l of control medicinal material solution are drawn, is put respectively on same silica gel g thin-layer plate, with toluene: acetone: methanol Volume ratio is that 8:3:0.5 is solvent, is set in the pre-saturated expansion cylinder of ammonia steam, presaturation 30 minutes, is unfolded, takes out, dry, Spray is with dilute bismuth potassium iodide test solution, in sample chromatogram, on position corresponding with reference medicine chromatography, shows the spot of same color Point.
Preferably, the content of baicalin detection method is specific as follows:
(1) prepared by test sample: taking lung power cough mixture medicinal extract 0.5g, sets in 25ml volumetric flask, adds the appropriate volume score to be 75% ethanol solution is ultrasonically treated 10 minutes, lets cool, and adds 75% ethanol solution to scale, shakes up, filter, take subsequent filtrate；
(2) preparation of reference substance solution: taking scutelloside reference substance, accurately weighed, adds methanol that every 1ml is made containing the molten of 70 μ g Liquid；
(3) accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, chromatographic column is with ten Eight alkyl silane bonded silica gels are filler；The mixed liquor that methanol-water-phosphoric acid volume ratio is 55: 45:0.2 is mobile phase；Wavelength To be measured under the conditions of 280nm.
The beneficial effects of the present invention are: the invention discloses lung power cough mixture medicinal extract, preparation method and its quality controls Method processed, preparation process add water to cook the bulk pharmaceutical chemicals of recipe quantity secondary, 2 hours first times, second 1.5 hours, merge and decoct Boil liquid, filtering, filtrate are concentrated into 80 DEG C of relative density as 1.03~1.05 clear cream, and this method extracting method is simple, does not make With organic solvent, it can be sufficiently reserved each effective component, improve content of baicalin, content of baicalin is higher than 3.5mg/g in product；This Invention also discloses the method for quality control of lung power cough mixture medicinal extract, can preferably control product quality, soaks to lung power cough mixture The processing of cream and quality control are of great significance.
Detailed description of the invention
Fig. 1 is root of purple-flowered peucedanum thin-layer chromatography qualification result (1: root of purple-flowered peucedanum control medicinal material；2: negative (with the medicinal extract of root of purple-flowered peucedanum medicinal material by confession Test product processing)；3-5: different lung power cough mixture medicinal extract).
Fig. 2 is tuber of stemona thin-layer chromatography qualification result (1: tuber of stemona control medicinal material；2: negative (medicinal extract of tuber of stemona medicinal material is pressed for examination Product processing)；3-5: different lung power cough mixture medicinal extract).
Specific embodiment
Below by a preferred embodiment of the present invention will be described in detail.
The preparation method of embodiment 1, lung power cough mixture medicinal extract
The preparation method of lung power cough mixture medicinal extract, includes the following steps: to take radix scutellariae 29g, root of purple-flowered peucedanum 28g, the tuber of stemona by prescription 28g, red gentian 28g, phoenix tree root 26g, oldenlandia diffusa 25g, aster 23g, add water to cook secondary, are added for the first time suitable It being decocted 2 hours in 7 times of medicinal material weight of boiling water, the yu boiling water that second of addition is equivalent to 4 times of medicinal material weight decocts 1.5 hours, Merge decoction liquor, filtering, filtrate be concentrated into relative density be 1.03~1.05 (80 DEG C) clear cream to get.The clear cream of acquisition is Brown.Every 1g is containing radix scutellariae with scutelloside (C21H18O11) meter, it is higher than 3.5mg.Boiling water is directly added into preparation process to help to improve The conversion ratio of scutelloside.
Control group: the radix scutellariae of recipe quantity, the root of purple-flowered peucedanum, the tuber of stemona, red gentian, phoenix tree root, oldenlandia diffusa, aster are pressed The method of Publication No. CN1415324A prepares lung power cough mixture, and scutelloside is 3.1mg/ml in product.
Embodiment 2, lung power cough mixture medicinal extract method of quality control
(1) root of purple-flowered peucedanum is identified: being taken lung power cough mixture medicinal extract 3ml made from 3 parts of embodiments 1 to be diluted with water to 30ml, is used ether It proposes 2 times, each 25ml, merges ether solution, be evaporated, residue adds ethyl acetate 1ml to make to dissolve, as test solution.
Root of purple-flowered peucedanum control medicinal material (lot number: 120951-200704, source: Nat'l Pharmaceutical & Biological Products Control Institute) 1g separately is taken, is added Ether 20ml is heated to reflux 30 minutes, and filtering, filtrate is evaporated, and residue adds ethyl acetate 1ml to make to dissolve, molten as control medicinal material Liquid.
And it is handled using the medicinal extract of root of purple-flowered peucedanum medicinal material by test sample as negative control solution.
It is tested according to thin-layered chromatography (one annex VI B of " Chinese Pharmacopoeia " version in 2010), it is each to draw above two solution 5~10 μ l put respectively on same silica gel g thin-layer plate, with toluene-ethyl acetate (3:2) for solvent, are unfolded, take out, dry in the air It is dry, it sprays with 10% sodium hydroxide solution, sets and inspected under ultraviolet lamp (365nm).In sample chromatogram, with reference medicine chromatography On corresponding position, the fluorescence spot of same color, negative noiseless (Fig. 1) are shown.
(2) tuber of stemona is identified:
Take lung power cough mixture medicinal extract 3ml made from 3 parts of embodiments 1 to be diluted with water to 30ml, with ammonia solution adjust pH value to 10, it is extracted 2 times, each 25ml with methylene chloride shaking, merges dichloromethane solution, be evaporated, residue adds methanol 1ml to make to dissolve, and makees For test solution.
Tuber of stemona control medicinal material (lot number: 121221-200402, source: Chinese pharmaceutical biological product inspection institute) 2g separately is taken, is added Ammonia solution makes to moisten, and places 10 minutes, and add methylene chloride 20ml, is ultrasonically treated 30 minutes, and filtering, filtrate is evaporated, and residue adds first Alcohol 1ml makes to dissolve, as control medicinal material solution.
And it is handled using the medicinal extract of tuber of stemona medicinal material by test sample as negative control solution.
It is tested according to thin-layered chromatography (one annex VI B of " Chinese Pharmacopoeia " version in 2010), it is each to draw above two solution 10 μ l put respectively on same silicon G lamellae, with toluene-acetone-methanol (volume ratio 8:3:0.5) for solvent, set ammonia steaming In the pre-saturated expansion cylinder of gas, presaturation 30 minutes, it is unfolded, takes out, dry, spray with dilute bismuth potassium iodide test solution.Sample chromatogram In, on position corresponding with reference medicine chromatography, show the spot of same color, negative noiseless (Fig. 2).
(3) lung power cough mixture medicinal extract content determination of Baicalin method
Assay is carried out according to high performance liquid chromatography (one VI D of annex of " Chinese Pharmacopoeia " version in 2010), Shimadzu liquid Chromatography；Ethyl alcohol, phosphoric acid are that analysis is pure；Methanol is chromatography alcohol；(lot number: 110715-200811 comes scutelloside reference substance Source: Nat'l Pharmaceutical & Biological Products Control Institute).
Chromatographic condition and system suitability: being filler with octadecylsilane chemically bonded silica；Methanol-quality point It is mobile phase that number, which is 0.4% phosphoric acid (55: 45),；Detection wavelength is 280nm.Theoretical cam curve should be not less than based on scutelloside peak 2000。
The preparation of reference substance solution: accurately weighed scutelloside reference substance 17.68mg (content 94%) sets the capacity of 50ml In bottle plus methanol dissolves and is diluted to stock solution of the scale to get every 1ml containing 0.3324mg/ml.It is molten that precision measures 5ml reserve Liquid is set in the volumetric flask of 25ml plus methanol dissolves and be diluted to scale, shakes up the reference substance to get every 1ml containing 0.06648mg/ml Solution.
The preparation of test solution: it referring to lung power cough mixture content assaying method, takes as made from 1 method of embodiment for examination 8 parts of product, every part of 0.5g is set in 25ml volumetric flask, 2 parts plus 95% appropriate amount of ethanol, 2 parts plus 85% appropriate amount of ethanol, 2 parts plus 75% second Appropriate alcohol, 2 parts plus 65% appropriate amount of ethanol are ultrasonically treated 10 minutes, let cool, add corresponding solvent to be diluted to scale, shake up, mistake Filter, take subsequent filtrate to get.
Measuring method: accurate absorption reference substance solution and each 10 μ l of test solution respectively, injection liquid chromatograph, measurement, The results are shown in Table 1.
Table 1, lung power cough mixture medicinal extract assay result
It can be seen that 75% alcohol treatment sample size highest, average value 7.6mg/ml.
Embodiment 3, detection method reliability
(1) specificity
The preparation of negative solution；It takes the medicinal extract 0.5g of scarce radix scutellariae medicinal materials to set in 25ml volumetric flask, adds 75% appropriate amount of ethanol, press According to test solution processing to get negative solution.
Measuring method: pressing above-mentioned chromatographic condition, accurate respectively to draw reference substance solution and test solution, negative solution each 10 μ l, injects liquid chromatograph, and measurement result shows that sample peak is consistent with scutelloside reference substance peak retention time, and separating degree meets It is required that number of theoretical plate is greater than 2000 in terms of scutelloside, negative sample solution is noiseless, and specificity is strong.
(2) linear relationship
(1ml, 2.5ml, 5ml, 8ml, 20ml) is drawn through precision with scutelloside reference substance stock solution (0.3324mg/ml), It is set in the volumetric flask of 25ml respectively plus methanol dissolves and be diluted to scale, shaken up, prepare the reference substance of 5 concentration, be injected separately into Liquid chromatograph the results are shown in Table 2:
Table 2, difference sampling volume peak area
NO 1 2 3 4 5
Peak area 318480 649251 1314931 2301133 5905160
The result shows that: for scutelloside reference substance concentration within the scope of 13.296 μ of μ g/ml -265.92 g/ml, linear relationship is good Good (regression equation: Y=2E+07X-76934 related coefficient: R2Value: 0.999).
(3) durability
Reference substance solution is drawn, at room temperature every 2 hours sample introductions, 10 μ l, measurement calculates peak area RSD, and experiment shows Huang A kind of reed mentioned in ancient books glycosides is stablized in 8 hours surveyed, the results are shown in Table 3:
Table 3, Detection of Stability result
(4) precision
6 parts of test sample (lung power cough mixture medicinal extract is made by 1 method of embodiment) is taken, every part of 0.5g is set in 25ml volumetric flask, Add 75% appropriate amount of ethanol, be ultrasonically treated 10 minutes, let cool, add 75% ethyl alcohol to be diluted to scale, shake up, filters, it is accurate respectively to inhale Each 10 μ l of subsequent filtrate solution is taken, liquid chromatograph is injected, is measured to get the results are shown in Table 4:
Table 4, precision measurement result
(5) accuracy
6 parts of test sample (lung power cough mixture medicinal extract is made by 1 method of embodiment) is taken, every part of 0.25g sets 25ml volumetric flask In, it is accurately weighed, it is accurate respectively that scutelloside stock solution (0.3324mg/ml) 9ml is added, add 75% appropriate amount of ethanol, at ultrasound Reason 10 minutes, lets cool, adds 75% ethyl alcohol to be diluted to scale, shake up, and filters, accurate respectively to draw each 10 μ l of subsequent filtrate solution, note Enter liquid chromatograph, measurement to get.The results are shown in Table 5:
Table 5, accuracy determination result
(6) sample measurement and the determination of content limit
10 batches of lung power cough mixture medicinal extract samples (being made by 1 method of embodiment) are taken to handle by test solution preparation, respectively Precision draw each 10 μ l of subsequent filtrate solution, inject liquid chromatograph, measurement to get.The results are shown in Table 6:
The determination of table 6, content limit
As seen from the above table, content of baicalin value in 10 batches of medicinal extract, it is contemplated that had differences between difference batch medicinal material, by radix scutellariae Glycosides content limit, which is fixed tentatively, must not be less than 3.5mg for every 1ml.
Embodiment 4, the verifying of lung power cough mixture medicinal extract drug effect
For the drug effect for proving lung power cough mixture medicinal extract, to lung power cough mixture medicinal extract in anti-oxidant, immunoglobulin concentrations and Antibacterial aspect is tested, and the specific method is as follows:
By bacterial bronchopneumonia mouse model 120, it is randomly divided into treatment group, control group and positive controls.It controls Treatment method: lung power cough mixture medicinal extract is taken by treatment group, each 125mg, 3 times a day, the 2 Monday courses for the treatment of；Control group takes equivalent Lung power cough mixture disclosed in CN1415324A.Simultaneously to take penicillin as positive control, takes front and back and blood is carried out to mouse Clear superoxide dismutase (SOD), the testing result such as table 7 of lipid peroxidation (LPO) and Immunoglobulin IgG, IgA, IgM With shown in table 8.
The variation of SOD and LPO before and after table 7, the medication of lung power cough mixture medicinal extract
As can be seen from Table 7, the equal indifference of SOD and LPO before medication, treatment group SOD and LPO and control group and sun after medication Property control group compare, treatment group SOD in rising by a relatively large margin, and LPO is on a declining curve, and effect is better than control group.
Table 8, lung power cough mixture medicinal extract observe result to humoral immunity
As shown in Table 8, treatment group Ig G, Ig M, Ig E are above control group and positive controls after 15 days, show to exempt from Epidemic disease function is improved.
Bacteriostatic experiment is specific as follows, by lung power cough mixture medicinal extract respectively to staphylococcus, streptococcus, Candida albicans, lung Scorching diplococcus, Klebsiella Pneumoniae, carries out bacteriostatic experiment to chlamydia pneumoniae, influenza Alphavirus at haemophilus influenzae, antibacterial It is as shown in table 9 to enclose size.
Table 9, lung power cough mixture medicinal extract are to sensitive bacteria inhibition zone size (unit mm)
Bacterial species Experimental group Control group Positive controls
Staphylococcus 21.32 19.28 -
Streptococcus 21.47 20.72 -
Candida albicans 19.65 17.83 -
Diplococcus pneumopniae 19.89 17.56 -
Haemophilus influenzae 18.56 17.44 -
Klebsiella Pneumoniae 20.17 18.34 -
To chlamydia pneumoniae 21.49 19.56 -
Influenza Alphavirus 18.95 17.41 -
The results show that lung power cough capsule medicinal extract is thermophilic to staphylococcus, streptococcus, Candida albicans, Diplococcus pneumopniae, influenza G+, the G- such as blood bacillus, Klebsiella Pneumoniae have inhibiting effect；There is significant suppression to chlamydia pneumoniae, influenza Alphavirus Production is used.
Finally, it is stated that preferred embodiment above is only used to illustrate the technical scheme of the present invention and not to limit it, although logical It crosses above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be Various changes are made to it in form and in details, without departing from claims of the present invention limited range.

Claims (10)

1. a kind of lung power cough mixture medicinal extract, which is characterized in that prepared by including the following steps: taking radix scutellariae, the root of purple-flowered peucedanum, hundred by prescription Radix scutellariae crushed 16mm sieve plate by portion, red gentian, phoenix tree root, oldenlandia diffusa, aster, then add boiling with other 6 taste medicines Water decoction is secondary, and the boiling water that addition for the first time is equivalent to 7 times of medicinal material weight decocts 2 hours, and second of addition is equivalent to medicinal material weight The boiling water of 4 times of amount decocts 1.5 hours, merges decoction liquor, filtering, it is 1.03~1.05 (80 DEG C) that filtrate, which is concentrated into relative density, Clear cream to get.
2. lung power cough mixture medicinal extract according to claim 1, it is characterised in that: the prescription each component is as follows: radix scutellariae 29g, Root of purple-flowered peucedanum 28g, tuber of stemona 28g, red gentian 28g, phoenix tree root 26g, oldenlandia diffusa 25g, aster 23g.
3. a kind of lung power cough composition medicine composition, it includes the lung power cough mixture medicinal extract of claims 1 or 2 and pharmaceutically acceptable auxiliary Material.
4. the lung power cough mixture medicinal extract of claims 1 or 2 is used to prepare the purposes of lung power cough mixture.
5. a kind of preparation method of lung power cough mixture medicinal extract, which comprises the steps of: by prescription take radix scutellariae, the root of purple-flowered peucedanum, Radix scutellariae crushed 16mm sieve plate by the tuber of stemona, red gentian, phoenix tree root, oldenlandia diffusa, aster, then add with other 6 taste medicines Boiling water decoction is secondary, and the boiling water that addition for the first time is equivalent to 7 times of medicinal material weight decocts 2 hours, and second of addition is equivalent to medicinal material The boiling water that 4 times of weight decocts 1.5 hours, merges decoction liquor, filtering, it is 1.03~1.05 (80 DEG C) that filtrate, which is concentrated into relative density, Clear cream to get.
6. the preparation method of lung power cough mixture medicinal extract according to claim 5, it is characterised in that: the prescription each component is such as Under: radix scutellariae 29g, root of purple-flowered peucedanum 28g, tuber of stemona 28g, red gentian 28g, phoenix tree root 26g, oldenlandia diffusa 25g, aster 23g.
7. the method for quality control of lung power cough mixture medicinal extract as claimed in claim 1 or 2, which is characterized in that including root of purple-flowered peucedanum identification, hundred Portion's identification and content of baicalin detection:
The root of purple-flowered peucedanum identification specifically: take lung power cough mixture medicinal extract to be diluted with water, then with extracted by ether at least 2 times, merge second Ether liquid, is evaporated, and residue adds ethyl acetate to dissolve, as test solution；Root of purple-flowered peucedanum control medicinal material separately is taken, adding diethyl ether to be heated to reflux mentions It takes, filters, filtrate is evaporated, and residue adds ethyl acetate to make to dissolve, as control medicinal material solution；Draw test solution and comparison medicine Material solution is put respectively on same silica gel g thin-layer plate, using toluene-ethyl acetate as solvent, is unfolded, is taken out, dry, spray with Mass fraction be 10% sodium hydroxide solution, set and inspected under 365nm ultraviolet lamp, in sample chromatogram, with comparison medicine wood color It composes on corresponding position, shows the fluorescence spot of same color；
The tuber of stemona identification specifically: take lung power cough mixture medicinal extract to be diluted with water, adjust pH value to 10 with ammonia solution, use dichloromethane Alkane shaking is extracted at least 2 times, is merged dichloromethane solution, is evaporated, residue adds methanol to dissolve, as test solution；Separately take the tuber of stemona Control medicinal material, ammonification test solution make to moisten, place, add methylene chloride, be ultrasonically treated, and filtering, filtrate is evaporated, and residue adds methanol molten Solution, as control medicinal material solution；Test solution and control medicinal material solution are drawn, is put respectively on same silica gel g thin-layer plate, with Toluene-acetone-methanol-is solvent, is set in the pre-saturated expansion cylinder of ammonia steam, presaturation 30 minutes, is unfolded, and takes out, dries, Spray is with dilute bismuth potassium iodide test solution, in sample chromatogram, on position corresponding with reference medicine chromatography, shows the spot of same color Point；
The content of baicalin detection are as follows: take lung power cough mixture medicinal extract, add ethanol solution, be ultrasonically treated, let cool, it is molten to add ethyl alcohol Liquid shakes up, and filtering takes subsequent filtrate；Accurately weighed scutelloside reference substance, adds methanol to dissolve, and is configured to every 1ml containing 0.070mg's Reference substance solution；It is accurate respectively to draw reference substance solution and test solution, liquid chromatograph is injected, with octadecylsilane Bonded silica gel is the chromatographic column of filler；Methanol-water-phosphoric acid is mobile phase；It is measured under the conditions of wavelength is 280nm.
8. the method for quality control of lung power cough mixture medicinal extract according to claim 7, which is characterized in that the root of purple-flowered peucedanum identification tool Body are as follows: it takes lung power cough mixture medicinal extract 3ml to be diluted with water 30ml, is proposed 2 times, each 25ml with ether, merge ether solution, be evaporated, Residue adds ethyl acetate 1ml to make to dissolve, as test solution；Root of purple-flowered peucedanum control medicinal material 1g separately is taken, add diethyl ether 20ml, is heated to reflux 30 minutes, filtering, filtrate was evaporated, and residue adds ethyl acetate 1ml to make to dissolve, as control medicinal material solution；Draw test solution With each 5~10 μ l of control medicinal material solution, put respectively on same silica gel g thin-layer plate, with volume ratio for 3:2 toluene-ethyl acetate For solvent, it is unfolded, takes out, dry, spray, for 10% sodium hydroxide solution, is set and inspected under 365nm ultraviolet lamp with mass fraction, supplies In test product chromatography, on position corresponding with reference medicine chromatography, the fluorescence spot of same color is shown.
9. the method for quality control of lung power cough mixture medicinal extract according to claim 7, which is characterized in that the tuber of stemona identification tool Body are as follows: take lung power cough mixture medicinal extract 3ml to be diluted with water 30ml, adjust pH value to 10 with ammonia solution, extract 2 with methylene chloride shaking Secondary, each 25ml merges dichloromethane solution, is evaporated, residue adds methanol 1ml to make to dissolve, as test solution；Separately take the tuber of stemona pair According to medicinal material 2g, ammoniating test solution makes to moisten, and places 10 minutes, and add methylene chloride 20ml, is ultrasonically treated 30 minutes, and filtering, filtrate is steamed Dry, residue adds methanol 1ml to make to dissolve, as control medicinal material solution；Test solution and each 10 μ l of control medicinal material solution are drawn, point Other point is on same silicon G lamellae, and using toluene: acetone: the mixed liquor that methanol volume ratio is 8:3:0.5 sets ammonia steaming as solvent In the pre-saturated expansion cylinder of gas, presaturation 30 minutes, it is unfolded, takes out, dry, spray with dilute bismuth potassium iodide test solution, sample chromatogram In, on position corresponding with reference medicine chromatography, show the spot of same color.
10. the method for quality control of lung power cough mixture medicinal extract according to claim 7, which is characterized in that the scutelloside contains Quantity measuring method is specific as follows:
(1) prepared by test sample: taking lung power cough mixture medicinal extract 0.5g, sets in 25ml volumetric flask, adding appropriate volume score is 75% Ethanol solution is ultrasonically treated 10 minutes, lets cool, and adding volume fraction is 75% ethanol solution to scale, shakes up, filters, take Subsequent filtrate；
(2) preparation of reference substance solution: taking scutelloside reference substance, accurately weighed, adds methanol that the solution that every 1ml contains 70 μ g is made；
(3) accurate respectively to draw reference substance solution and each 10 μ l of test solution, inject liquid chromatograph, chromatographic column octadecane Base silane bonded silica gel is filler；The solution that methanol-water-phosphoric acid volume ratio is 55: 45:0.2 is mobile phase；Wavelength is It is measured under the conditions of 280nm.
CN201910165137.5A 2019-03-05 2019-03-05 Lung power cough mixture medicinal extract and application thereof and method of quality control Pending CN109692291A (en)

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Publication number Priority date Publication date Assignee Title
CN112603973A (en) * 2020-12-22 2021-04-06 贵州健兴药业有限公司 Improved preparation method of pharmaceutical composition for treating lung cough
CN114869977A (en) * 2022-03-28 2022-08-09 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) Application of lung cough in preparation of product for preventing and treating breast cancer
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CN115837063A (en) * 2022-12-27 2023-03-24 贵州健兴药业有限公司 Preparation and detection method of improved lung-strength cough medicine composition
CN115837063B (en) * 2022-12-27 2023-12-08 贵州健兴药业有限公司 Preparation and detection methods of lung force cough pharmaceutical composition

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Application publication date: 20190430