CN107782838A - A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing - Google Patents

A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing Download PDF

Info

Publication number
CN107782838A
CN107782838A CN201610770575.0A CN201610770575A CN107782838A CN 107782838 A CN107782838 A CN 107782838A CN 201610770575 A CN201610770575 A CN 201610770575A CN 107782838 A CN107782838 A CN 107782838A
Authority
CN
China
Prior art keywords
solution
medicine
coughing
medicinal material
eliminating phlegm
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610770575.0A
Other languages
Chinese (zh)
Inventor
闫晓楠
潘勤
王祎
孙律衡
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
ZHONGXIN INNOVA LABORATORIES
Original Assignee
ZHONGXIN INNOVA LABORATORIES
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by ZHONGXIN INNOVA LABORATORIES filed Critical ZHONGXIN INNOVA LABORATORIES
Priority to CN201610770575.0A priority Critical patent/CN107782838A/en
Publication of CN107782838A publication Critical patent/CN107782838A/en
Pending legal-status Critical Current

Links

Classifications

    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/90Plate chromatography, e.g. thin layer or paper chromatography

Landscapes

  • Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Investigating Or Analysing Biological Materials (AREA)

Abstract

The invention discloses the method for quality control that a kind of clearing lung and eliminating phlegm stops medicine of coughing, belong to pharmaceutical field.A kind of clearing lung and eliminating phlegm stops the quality determining method for medicine of coughing, and step is:1st, need testing solution is prepared:Candidate drug is taken as need testing solution;2nd, control medicinal material solution is prepared:Fritillaria thunbergii medicinal material is taken, control medicinal material solution is made;3rd, reference substance solution is prepared;4th, thin-layer chromatography:Each 4 μ l of above two solution are drawn respectively, puts on same silica gel g thin-layer plate, is deployed with solvent respectively, are taken out, are dried, spray with dilute bismuth potassium iodide test solution;5th, result judgement.The present invention is in lung clearing cough suppressing phlegm transforming medicinal ball on the basis of primary standard, establish the thin-layer identification method of fritillaria thunbergii, filter out revised quality standard in the method inclusive criteria that favorable reproducibility, specificity are strong, spot development is clear, result easily judges, improve the quality control of medicine, make the qualitative detection of medicine more accurate, quality is more prone to control.

Description

A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing
Technical field
The present invention relates to the method for quality control that a kind of clearing lung and eliminating phlegm stops medicine of coughing, belong to pharmaceutical field.
Background technology
The lung clearing cough suppressing phlegm transforming medicinal ball prescription is using radix scutellariae, root of Chinese trichosanthes as main ingredient, the clear dry heat-phlegm syndrome of purging the lung of pathogenic fire intestines and internal organs of the body internal organs;With the root of purple-flowered peucedanum, Abundant expectoration due to lung-heat cough is controlled supplemented by balloonflower root, fritillaria thunbergii;To be relievingd asthma with semen armeniacae amarae, the root bark of white mulberry, stemona root cough relieving, the tuber of dwarf lilyturf, the wind-weed nourish lung yin, Rheum officinale is equipped with root of Chinese trichosanthes and rushes down big internal organs heat, with Exocarpium Citri Grandis, Fructus Aurantii regulating qi-flowing for eliminating phlegm, and prevents rheum officinale, radix scutellariae from rushing down clearly too, for assistant Medicine;Radix glycyrrhizae coordinating the drug actions of a prescription.The ten four traditional Chinese medicines collaboration of full side works, and is exclusively used in treating the yellow phlegm of cough caused by abundant expectoration due to lung-heat, chest diaphragm is not Freely, sound of having sore throat is mute, is hard and dry.For bronchitis, the pneumonia person that occurs above-mentioned symptom.
Lung clearing cough suppressing phlegm transforming medicinal ball prescription:Radix scutellariae 96g, root of Chinese trichosanthes 48g, fritillaria thunbergii 24g, Fructus Aurantii (going flesh bran to fry) 24g, balloonflower root It is 24g, the root bark of white mulberry (honey is processed) 24g, prepared RADIX ET RHIZOMA RHEI 12g, wind-weed 12g, tuber of dwarf lilyturf 12g, Exocarpium Citri Grandis 12g, semen armeniacae amarae (peeling fry) 12g, preceding Hu 12g, tuber of stemona 12g, radix glycyrrhizae 3g.
Lung clearing cough suppressing phlegm transforming medicinal ball preparation method:14 tastes by more than, are ground into fine powder, sieve, and mix, and with water pill, dry, i.e., .
Major function:Clearing lung-heat, resolving sputum, only cough.For the yellow phlegm of cough caused by lung heat phlegm, chest diaphragm is not smooth, and laryngalgia sound is mute, greatly Just dry.
Existing standard record in《Drug Standard of Ministry of Public Health of the Peoples Republic of China》The 7th (Chinese traditional patent formulation of in 1993 version Preparation) page 172 (WS3-B-1433-93).Appearance character, microscopical characters and rhubarb medicinal material are only defined in its quality standard Thin-layer identification method, can not fundamentally qualitative, quantitative control product inherent quality.Through retrieval, find no Guan Qingjin and stop The patent document for phlegm-resolving pill detection method of coughing.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of clear gold that is simple, being capable of accurate qualitative detection drug ingedient to stop Cough the method for quality control of phlegm-resolving pill.
To achieve the above object, the present invention uses following technical scheme:
A kind of clearing lung and eliminating phlegm stops the quality determining method for medicine of coughing, and step is:
(1) need testing solution is prepared:Candidate drug 3~10g is taken, it is finely ground, add 20~40ml of water to make dissolving, water-bath to 70~ 90 DEG C, 0.5~2% hydrochloric acid is adjusted to pH value as 1~3, centrifugation, takes supernatant, with 3~10% sodium hydroxides be adjusted to pH value for 9~ 12, with extracted by ether 2~3 times, 10~30ml, merges extract solution, is evaporated every time, and residue adds 2~5ml of methanol to make dissolving, as Need testing solution;
(2) reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made Contain 1~3mg solution per 1ml, as reference substance solution;
(3) control medicinal material solution is prepared:Fritillaria thunbergii medicinal material 1~5g is taken, it is finely ground, add 10~50ml of water to make dissolving, water-bath is extremely 70~90 DEG C, it is 1~3 that 0.5~2% hydrochloric acid, which is adjusted to pH value, centrifugation, takes supernatant, being adjusted to pH value with 3~10% sodium hydroxides is 8~12, with extracted by ether 2~3 times, 10~30ml, merges extract solution, is evaporated every time, and residue adds 2~5ml of methanol to make dissolving, makees For need testing solution;
(4) thin-layer chromatography:Each 3~5 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with Ethyl acetate-methanol-conc. aq. ammonia is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;
(5) result judgement.
Preferably, the step (1) prepares need testing solution:Candidate drug 5g is taken, it is finely ground, add water 30ml to make dissolving, water To 80 DEG C, it is 2 that 1% hydrochloric acid, which is adjusted to pH value, centrifugation, takes supernatant for bath, and it is 11 to be adjusted to pH value with 5% sodium hydroxide, is carried with ether Take 3 times, each 20ml, merge extract solution, be evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
Preferably, the step (2) prepares reference substance solution:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively Add chloroform that solution of every 1ml containing 2mg is made, as reference substance solution;
Preferably, the step (3) prepares control medicinal material solution:Fritillaria thunbergii medicinal material 2g is taken, it is finely ground, add water 30ml to make molten Solution, to 80 DEG C, it is 2 that 1% hydrochloric acid, which is adjusted to pH value, centrifugation, takes supernatant for water-bath, and it is 11 to be adjusted to pH value with 5% sodium hydroxide, uses second Ether extracts 3 times, each 20ml, merges extract solution, is evaporated, residue adds methanol 3ml to make dissolving, as need testing solution;
Preferably, step (4) thin-layer chromatography:Each 4 μ l of above two solution are drawn respectively, are put respectively in same silica gel On G lamellaes, using ethyl acetate-methanol-conc. aq. ammonia as solvent, deploy, take out, dry, spray with dilute bismuth potassium iodide test solution;Institute State ethyl acetate in solvent:Methanol:The volume ratio of concentrated ammonia liquor is 15~20:3~1:3~1.
Preferably, ethyl acetate in the solvent:Methanol:The volume ratio of concentrated ammonia liquor is 18:2:1.
Step (5) result judgement refers to:Contrast the chromatogram of test sample, reference substance and control medicinal material;Wherein test sample In chromatogram, on position corresponding with reference substance and control medicinal material chromatogram, the spot person for showing same color is qualified.
It is lung clearing cough suppressing phlegm transforming medicinal ball that clearing lung and eliminating phlegm of the present invention, which stops medicine of coughing,.
The prescription of the lung clearing cough suppressing phlegm transforming medicinal ball is:Radix scutellariae 96g, root of Chinese trichosanthes 48g, fritillaria thunbergii 24g, Fructus Aurantii (going flesh bran to fry) 24g, balloonflower root 24g, the root bark of white mulberry (honey is processed) 24g, prepared RADIX ET RHIZOMA RHEI 12g, wind-weed 12g, tuber of dwarf lilyturf 12g, Exocarpium Citri Grandis 12g, semen armeniacae amarae (peeling Fry) 12g, root of purple-flowered peucedanum 12g, tuber of stemona 12g, radix glycyrrhizae 3g.
The preparation method of the lung clearing cough suppressing phlegm transforming medicinal ball is:14 tastes by more than, are ground into fine powder, sieve, and mix, general with water Ball, dry, produce.
A kind of clearing lung and eliminating phlegm stops the quality determining method for medicine of coughing:
1st, need testing solution is prepared:Candidate drug 5g is taken, it is finely ground, add water 30ml to make dissolving, water-bath is to 80 DEG C, 1% hydrochloric acid PH value is adjusted to as 2, centrifugation, takes supernatant, pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, each 20ml, is closed And extract solution, it is evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
2nd, reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made often Solution of the 1ml containing 2mg, as reference substance solution;
3rd, control medicinal material solution is prepared:Fritillaria thunbergii medicinal material 2g is taken, it is finely ground, add water 30ml to make dissolving, water-bath is to 80 DEG C, 1% Hydrochloric acid is adjusted to pH value as 2, centrifugation, takes supernatant, and pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, every time 20ml, merge extract solution, be evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
3rd, thin-layer chromatography:Each 4 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with acetic acid Ethyl ester-methanol-conc. aq. ammonia (﹕ 1 of 18 ﹕ 2) is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution.
4th, result judgement:Contrast the chromatogram of test sample, reference substance and control medicinal material;Wherein in test sample chromatogram, with it is right According on product and the corresponding position of control medicinal material chromatogram, the spot person of aobvious same color is qualified.
Step 4 thin-layer chromatography, according to thin-layered chromatography (《Chinese Pharmacopoeia》Four annex general rules 0502 of version in 2015) Experiment is carried out.
It is an advantage of the invention that:The present invention on the basis of primary standard, establishes the thin of fritillaria thunbergii in lung clearing cough suppressing phlegm transforming medicinal ball Layer discrimination method, filters out and is repaiied in the method inclusive criteria that favorable reproducibility, specificity are strong, spot development is clear, result easily judges Quality standard after ordering, the quality control of medicine is improved, make the qualitative detection of medicine more accurate, quality is more prone to control System.
The present invention is elaborated with reference to the accompanying drawings and detailed description, not to the limitation of invention.It is all according to This area equivalent substitution that the disclosure of invention is carried out, belongs to protection scope of the present invention.
Brief description of the drawings
Fig. 1 is the measurement result figure of embodiment 1
Embodiment
Embodiment 1
First, material
Test sample:Lung clearing cough suppressing phlegm transforming medicinal ball, Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj, lot number: 160801、160802、160803。
Reference substance:Peimine reference substance, National Institute for Food and Drugs Control, lot number 110750-201311,
Peininine reference substance, National Institute for Food and Drugs Control, lot number 110751-201110
Control medicinal material:Fritillaria thunbergii medicinal material, National Institute for Food and Drugs Control, lot number 120972-201405.
It is prepared by negative controls:The technique and prescription announced according to pharmacopeia prepare the drug sample without fritillaria thunbergii.
2nd, detect
1st, need testing solution is prepared:Candidate drug 5g is taken, it is finely ground, add water 30ml to make dissolving, water-bath is to 80 DEG C, with 1% salt Acid is adjusted to pH value as 2, centrifuges 10 minutes, takes supernatant, and pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, often Secondary 20ml, merge extract solution, be evaporated, residue adds methanol 3ml to make dissolving, produces;
2nd, reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made often Solution of the 1ml containing 2mg, is produced;
3rd, control medicinal material solution is prepared:Fritillaria thunbergii medicinal material 2g is taken, it is finely ground, add water 30ml to make dissolving, water-bath is to 80 DEG C, 1% Hydrochloric acid is adjusted to pH value as 2, centrifugation, takes supernatant, and pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, every time 20ml, merge extract solution, be evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
4th, negative controls solution is prepared:Negative controls 5g is taken, is carried out by need testing solution same method is prepared.
5th, thin-layer chromatography:Each 4 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with acetic acid Ethyl ester-methanol-conc. aq. ammonia (volume ratio 18:2:1) it is solvent, deploys, takes out, dry, spray with dilute bismuth potassium iodide test solution.
6th, result judgement:Contrast test sample, reference substance and control medicinal material, the chromatogram of negative controls;Wherein test sample color In spectrum, on position corresponding with reference substance and control medicinal material chromatogram, the spot person for showing same color is qualified.
3rd, result
Three batches of test samples differentiate as stated above.As a result Fig. 1 is seen, 1-7 is followed successively by from left to right:Peimine reference substance, Peininine reference substance, fritillaria thunbergii medicinal material, lung clearing cough suppressing phlegm transforming medicinal ball 160801, lung clearing cough suppressing phlegm transforming medicinal ball 160802, lung clearing cough suppressing Phlegm-resolving pill 160803, negative controls.
It is being in phase with fritillaria Su Jia ﹑ Peininines reference substances and fritillaria thunbergii medicinal material chromatogram relevant position in test sample chromatogram With colored speckles spot, and feminine gender is noiseless.
Embodiment 2
First, material
Test sample:Lung clearing cough suppressing phlegm transforming medicinal ball, Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj, lot number: 160801、160802、160803。
Reference substance:Peimine reference substance, National Institute for Food and Drugs Control, lot number 110750-201311,
Peininine reference substance, National Institute for Food and Drugs Control, lot number 110751-201110
Control medicinal material:Fritillaria thunbergii medicinal material, National Institute for Food and Drugs Control, lot number 120972-201405.
2nd, detect
1st, need testing solution is prepared:Candidate drug 5g is taken, it is finely ground, add water 30ml to make dissolving, water-bath is to 80 DEG C, with 1% salt Acid is adjusted to pH value as 2, centrifuges 10 minutes, takes supernatant, and pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, often Secondary 20ml, merge extract solution, be evaporated, residue adds methanol 3ml to make dissolving, produces;
2nd, reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made often Solution of the 1ml containing 2mg, is produced;
3rd, control medicinal material solution is prepared:Fritillaria thunbergii medicinal material 2g is taken, it is finely ground, add water 30ml to make dissolving, water-bath is to 80 DEG C, 1% Hydrochloric acid is adjusted to pH value as 2, centrifugation, takes supernatant, and pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, every time 20ml, merge extract solution, be evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
4th, thin-layer chromatography:Each 4 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with acetic acid Ethyl ester-methanol-conc. aq. ammonia (volume ratio 18:2:1) it is solvent, deploys, takes out, dry, spray with dilute bismuth potassium iodide test solution.
5th, result judgement:Contrast test sample, reference substance and control medicinal material, the chromatogram of negative controls;Wherein test sample color In spectrum, on position corresponding with reference substance and control medicinal material chromatogram, the spot person for showing same color is qualified.
3rd, result
Three batches of test samples differentiate as stated above.In test sample chromatogram, with fritillaria Su Jia ﹑ Peininines reference substances and Zhejiang Fritillaria medicinal material chromatogram relevant position is in same color spot spot.
Embodiment 3
First, material
Test sample:Lung clearing cough suppressing phlegm transforming medicinal ball, Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj, lot number: 160801、160802、160803。
Reference substance:Peimine reference substance, National Institute for Food and Drugs Control, lot number 110750-201311
Peininine reference substance, National Institute for Food and Drugs Control, lot number 110751-201110
Control medicinal material:Fritillaria thunbergii medicinal material, National Institute for Food and Drugs Control, lot number 120972-201405
2nd, detect
1st, need testing solution is prepared:Candidate drug 3g is taken, it is finely ground, add water 20ml to make dissolving, water-bath is to 70 DEG C, 0.5% salt Acid is adjusted to pH value as 3, centrifugation, takes supernatant, and pH value is adjusted to as 9 with 3% sodium hydroxide, with extracted by ether 2 times, each 10ml, Merge extract solution, be evaporated, residue adds methanol 2ml to make dissolving, as need testing solution.
2nd, reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made often Solution of the 1ml containing 1mg, as reference substance solution;
3rd, control medicinal material solution is prepared:Take fritillaria thunbergii medicinal material 1g, it is finely ground, add water 10ml to make dissolving, water-bath to 70 DEG C, 0.5% hydrochloric acid is adjusted to pH value as 1, centrifugation, takes supernatant, and pH value is adjusted to as 12 with 3% sodium hydroxide, with extracted by ether 2 times, often Secondary 10ml, merge extract solution, be evaporated, residue adds methanol 2ml to make dissolving, as need testing solution;
4th, thin-layer chromatography:Each 3 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with acetic acid Ethyl ester-methanol-conc. aq. ammonia is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;Ethyl acetate in solvent: Methanol:The volume ratio of concentrated ammonia liquor is 20:3:3.
5th, result judgement:Contrast the chromatogram of test sample, reference substance and control medicinal material;Wherein in test sample chromatogram, with it is right According on product and the corresponding position of control medicinal material chromatogram, the spot person of aobvious same color is qualified.
Embodiment 4
First, material
Test sample:Lung clearing cough suppressing phlegm transforming medicinal ball, Lerentang Pharmaceutical Factory, Zhongxin Pharmaceutical Group Co., Ltd., Tianj, lot number: 160801、160802、160803。
Reference substance:Peimine reference substance, National Institute for Food and Drugs Control, lot number 110750-201311,
Peininine reference substance, National Institute for Food and Drugs Control, lot number 110751-201110
Control medicinal material:Fritillaria thunbergii medicinal material, National Institute for Food and Drugs Control, lot number 120972-201405.
2nd, detect
1st, need testing solution is prepared:Candidate drug 10g is taken, it is finely ground, add water 40ml to make dissolving, water-bath is to 90 DEG C, 2% hydrochloric acid PH value is adjusted to as 1, centrifugation, takes supernatant, pH value is adjusted to as 9 with 10% sodium hydroxide, with extracted by ether 3 times, each 30ml, is closed And extract solution, it is evaporated, residue adds methanol 5ml to make dissolving, as need testing solution.
2nd, reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made often Solution of the 1ml containing 3mg, as reference substance solution;
3rd, control medicinal material solution is prepared:Fritillaria thunbergii medicinal material 5g is taken, it is finely ground, add water 50ml to make dissolving, water-bath is to 90 DEG C, 2% Hydrochloric acid is adjusted to pH value as 1, centrifugation, takes supernatant, and pH value is adjusted to as 8 with 10% sodium hydroxide, with extracted by ether 3 times, every time 30ml, merge extract solution, be evaporated, residue adds methanol 5ml to make dissolving, as need testing solution;
4th, thin-layer chromatography:Each 5 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with acetic acid Ethyl ester-methanol-conc. aq. ammonia is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;Ethyl acetate in solvent: Methanol:The volume ratio of concentrated ammonia liquor is 15:1:1.
5th, result judgement:Contrast the chromatogram of test sample, reference substance and control medicinal material;Wherein in test sample chromatogram, with it is right According on product and the corresponding position of control medicinal material chromatogram, the spot person of aobvious same color is qualified.

Claims (10)

1. a kind of quality determining method of clearing lung and eliminating phlegm cough suppressing medicine, it is characterised in that step is:
(1) need testing solution is prepared:Candidate drug 3~10g is taken, it is finely ground, add 20~40ml of water to make dissolving, water-bath to 70~90 DEG C, it is 1~3 that 0.5~2% hydrochloric acid, which is adjusted to pH value, centrifugation, takes supernatant, and it is 9~12 to be adjusted to pH value with 3~10% sodium hydroxides, With extracted by ether 2~3 times, 10~30ml, merges extract solution, is evaporated every time, and residue adds 2~5ml of methanol to make dissolving, as trying Product solution;
(2) reference substance solution is prepared:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus every 1ml is made in chloroform Solution containing 1~3mg, as reference substance solution;
(3) control medicinal material solution is prepared:Fritillaria thunbergii medicinal material 1~5g is taken, it is finely ground, add 10~50ml of water to make dissolving, water-bath to 70~ 90 DEG C, 0.5~2% hydrochloric acid is adjusted to pH value as 1~3, centrifugation, takes supernatant, with 3~10% sodium hydroxides be adjusted to pH value for 8~ 12, with extracted by ether 2~3 times, 10~30ml, merges extract solution, is evaporated every time, and residue adds 2~5ml of methanol to make dissolving, as Need testing solution;
(4) thin-layer chromatography:Each 3~5 μ l of above two solution are drawn respectively, are put respectively on same silica gel g thin-layer plate, with acetic acid Ethyl ester-methanol-conc. aq. ammonia is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;
(5) result judgement.
2. a kind of clearing lung and eliminating phlegm according to claim 1 stops the quality determining method for medicine of coughing, it is characterised in that:The step Suddenly (1) prepares need testing solution:Candidate drug 5g is taken, it is finely ground, add water 30ml to make dissolving, to 80 DEG C, 1% hydrochloric acid is adjusted to PH for water-bath It is worth for 2, centrifugation, takes supernatant, pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, each 20ml, merges extraction Liquid, it is evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
3. a kind of clearing lung and eliminating phlegm according to claim 1 stops the quality determining method for medicine of coughing, it is characterised in that:The step Suddenly (2) prepare reference substance solution:Peimine Dui Zhao Pin ﹑ Peininine reference substances are taken, respectively plus chloroform is made every 1ml and contained 2mg solution, as reference substance solution.
4. a kind of clearing lung and eliminating phlegm according to claim 1 stops the quality determining method for medicine of coughing, it is characterised in that:The step Suddenly (3) prepare control medicinal material solution:Fritillaria thunbergii medicinal material 2g is taken, it is finely ground, add water 30ml to make dissolving, to 80 DEG C, 1% hydrochloric acid is adjusted for water-bath It is 2 to pH value, centrifugation, takes supernatant, pH value is adjusted to as 11 with 5% sodium hydroxide, with extracted by ether 3 times, each 20ml, closes And extract solution, it is evaporated, residue adds methanol 3ml to make dissolving, as need testing solution.
5. a kind of clearing lung and eliminating phlegm according to claim 1 stops the quality determining method for medicine of coughing, it is characterised in that:The step Suddenly (4) thin-layer chromatography:Draw each 4 μ l of above two solution respectively, put respectively on same silica gel g thin-layer plate, with ethyl acetate- Methanol-conc. aq. ammonia is solvent, is deployed, and takes out, dries, spray with dilute bismuth potassium iodide test solution;Ethyl acetate in the solvent:First Alcohol:The volume ratio of concentrated ammonia liquor is 15~20:3~1:3~1.
6. a kind of clearing lung and eliminating phlegm according to claim 5 stops the quality determining method for medicine of coughing, it is characterised in that:The exhibition Open ethyl acetate in agent:Methanol:The volume ratio of concentrated ammonia liquor is 18:2:1.
7. a kind of clearing lung and eliminating phlegm according to claim 1 stops the quality determining method for medicine of coughing, it is characterised in that:The step Suddenly (5) result judgement refers to:Contrast the chromatogram of test sample, reference substance and control medicinal material;Wherein in test sample chromatogram, with compareing On product and the corresponding position of control medicinal material chromatogram, the spot person for showing same color is qualified.
8. a kind of clearing lung and eliminating phlegm according to any one of claim 1 to 7 stops the quality determining method for medicine of coughing, it is special Sign is:It is lung clearing cough suppressing phlegm transforming medicinal ball that the clearing lung and eliminating phlegm, which stops medicine of coughing,.
9. a kind of clearing lung and eliminating phlegm according to claim 8 stops the quality determining method for medicine of coughing, it is characterised in that:It is described clear The prescription of golden Zhisou-Huatan tablet is:Radix scutellariae 96g, root of Chinese trichosanthes 48g, fritillaria thunbergii 24g, Fructus Aurantii (going flesh bran to fry) 24g, balloonflower root 24g, mulberry White skin (honey is processed) 24g, prepared RADIX ET RHIZOMA RHEI 12g, wind-weed 12g, tuber of dwarf lilyturf 12g, Exocarpium Citri Grandis 12g, semen armeniacae amarae (peeling is fried) 12g, root of purple-flowered peucedanum 12g, Tuber of stemona 12g, radix glycyrrhizae 3g.
10. a kind of clearing lung and eliminating phlegm according to claim 9 stops the quality determining method for medicine of coughing, it is characterised in that:It is described The preparation method of lung clearing cough suppressing phlegm transforming medicinal ball is:14 tastes by more than, are ground into fine powder, sieve, and mix, and with water pill, dry, produce.
CN201610770575.0A 2016-08-30 2016-08-30 A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing Pending CN107782838A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610770575.0A CN107782838A (en) 2016-08-30 2016-08-30 A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610770575.0A CN107782838A (en) 2016-08-30 2016-08-30 A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing

Publications (1)

Publication Number Publication Date
CN107782838A true CN107782838A (en) 2018-03-09

Family

ID=61450004

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610770575.0A Pending CN107782838A (en) 2016-08-30 2016-08-30 A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing

Country Status (1)

Country Link
CN (1) CN107782838A (en)

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
中华人民共和国卫生部药典委员会: "《卫生部颁药品标准(中药成方制剂第七册)》", 31 December 1993 *
中国药典委员会: "《中国药典1995版一部》", 31 December 1995 *
刘志辉等: "润喉开音片有效成分的定性定量研究 ", 《中成药》 *

Similar Documents

Publication Publication Date Title
CN1925864B (en) Plant-based medicament for the treatment of hepatitis c
CN101396544A (en) Traditional Chinese medicine composition capable of ventilating the lung and relieving asthma and preparation and quality control method thereof
CN106198837A (en) The quality determining method of old cough with asthma sheet
CN102749401B (en) Inspection method of traditional Chinese medicine composition twenty-five-ingredient lung disease preparation
CN102120015A (en) Traditional Chinese medicine for soothing liver and dispersing depressed vital energy and soothing nerves and sedating mind, and preparation method and quality standard thereof
Nazir et al. Qualitative phytochemical analysis of Allium sativum (Garlic) and Curcuma longa (Turmeric)
CN101829216B (en) Preparation method and quality control method of traditional Chinese medicine preparation for treating bronchitis and bronchial asthma
CN101396486B (en) Traditional Chinese medicine composition for treating cough and asthma and preparation and quality control method thereof
Guo et al. Progress in the design and quality control of placeboes for clinical trials of traditional Chinese medicine
CN107782838A (en) A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing
Zhong et al. Co-existing polysaccharides affect the systemic exposure of major bioactive ingredients in Chang-Kang-Fang, a multi-herb prescription for treatment of irritable bowel syndrome
CN108743893A (en) The preparation method and applications of clearing lung-heat soup side's Chinese medical extract
CN107782839A (en) A kind of clearing lung and eliminating phlegm stops the method for quality control for medicine of coughing
CN104771451B (en) A kind of Chinese medical extract and its application with antidepressant effect
CN102258665B (en) Inspection method of Chinese medicinal composition for treating cough and asthma
CN103760271B (en) The detection method of brain heart clearing capsule
Niaz Application of Natural Products in SARS-CoV-2
CN107173763A (en) It is a kind of to treat Chinese herbal medicine jelly of recurrent oral ulceration and preparation method thereof
CN106248859A (en) A kind of method of quality control of removing heat from the lung and dissipating phlegm antitussive medicine
CN106198842A (en) A kind of method of quality control of removing heat from the lung and dissipating phlegm antitussive medicine
CN106226453A (en) A kind of method of quality control of removing heat from the lung and dissipating phlegm antitussive medicine
CN106038577A (en) Medicine composition with cough relieving effect, and preparation method and application thereof
CN102225144A (en) Traditional Chinese medicine compound for treating cough and asthma and preparation method thereof
CN106124686A (en) A kind of method of quality control of removing heat from the lung and dissipating phlegm antitussive medicine
CN106324176A (en) Quality control method of medicine for clearing lung, eliminating phlegm and relieving coughs

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20180309

RJ01 Rejection of invention patent application after publication