CN101708274A - Quality control method of pill preparation for treating chest impediment and cardialgia - Google Patents
Quality control method of pill preparation for treating chest impediment and cardialgia Download PDFInfo
- Publication number
- CN101708274A CN101708274A CN 200910312108 CN200910312108A CN101708274A CN 101708274 A CN101708274 A CN 101708274A CN 200910312108 CN200910312108 CN 200910312108 CN 200910312108 A CN200910312108 A CN 200910312108A CN 101708274 A CN101708274 A CN 101708274A
- Authority
- CN
- China
- Prior art keywords
- solution
- reference substance
- quality control
- eucalyptol
- cardialgia
- 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.)
- Granted
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a quality control method of a pill preparation for treating chest impediment and cardialgia. The quality control method of the pill preparation comprises the following steps of property research, identification, inspection and content determination, wherein the identification refers to identifying megalocarpous pungent litsea fruit and szechuan lovage rhizome; and the content determination refers to determining the contents of eucalyptol and borneol in the pill preparation respectively by using gas chromatography. The quality control method of a Migao Xinle dropping pill preparation for treating the chest impediment and the cardialgia is provided for researching and screening properties, the identification, the inspection and the content determination of the Migao Xinle dropping pill preparation. The adopted quality control method has the advantages of scientificity, rationality, high accuracy, good reproducibility, comprehensive and effective quality control of the Migao Xinle dropping pill preparation and guaranteed clinical curative effect of the preparation.
Description
Technical field
The present invention relates to the method for quality control of medicine, particularly treat the method for quality control of the happy dropping pill formulation of the Cinnamomum Migao H.W.Li. heart of obstruction of qi in the chest and cardialgia, belong to technical field of medicaments.
Background technology
Obstruction of qi in the chest and cardialgia is one of important diseases of the heart system that threatens the middle-aged and elderly people life and health, and along with the change of modern society's life style and dietary structure, morbidity has the trend that increases gradually, thereby causes that increasing people payes attention to.Obstruction of qi in the chest and cardialgia is called angina pectoris again, is mostly that expectorant is turbid because healthy energy is lost emptyly, blood stasis, the stagnation of QI, cold coagulation and cause that blockage of the cardiac vessels is not smooth, clinically with Danzhong or left chest ictally feel oppressed, pain serve as a kind of disease that mainly shows.The lighter accidental of short duration slight chest oppressiveness or dull pain, or be ictal Danzhong or the unclean sense of discomfort of left breast; Weight person's sharp ache, or be the squeezing sexual anhedonia.Often, breathe hard with cardiopalmus, hypopnea, even dyspnea with rapid and short breath, terrified uneasy, pale complexion, cold spontaneous sweating etc.How by fatigue, heavy meal, cold and excited and bring out, also can not have obvious inducement or when peace and quiet, fall ill.The happy drop pill of the Cinnamomum Migao H.W.Li. heart has hot temperature cold expelling, and the effect of vital energy regualting and blood circulation-promoting pain relieving cures mainly deficiency of heart-YANG, the obstruction of qi in the chest and cardialgia (angina pectoris) due to the stagnation of heart-blood.Disease is seen uncomfortable in chest, chest pain, and cardiopalmus is breathed hard, and very then chest pain radiating to the back is felt cold pain very, hypopnea, pale tongue or dark, tongue fur is white, deep-thready pulse.Because this medicine is a kind of new drug, does not also have the effective quality control method at present.The applicant studies this medicine, to guarantee the clinical efficacy of this medicine.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method of quality control for the treatment of the dropping pill formulation of obstruction of qi in the chest and cardialgia, comprises character, discriminating, inspection and assay.This method of quality control can be controlled the quality of the happy dropping pill formulation of the Cinnamomum Migao H.W.Li. heart of treatment obstruction of qi in the chest and cardialgia fully and effectively, thereby guarantees the clinical efficacy of this medicine.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme: the method for quality control of the dropping pill formulation of treatment obstruction of qi in the chest and cardialgia.This drop pill prepares like this: Fructus cinnamomi camphorae 4500g, Blumeae preparatum Tabellae (left-handed Borneolum Syntheticum) 90g, Rhizoma Chuanxiong 3600g, Bulbus Allii Macrostemonis 360g, more than four flavors, by recipe quantity Fructus cinnamomi camphorae is extracted volatile oil, Rhizoma Chuanxiong extracts extractum, Bulbus Allii Macrostemonis extracts extractum; Fructus cinnamomi camphorae volatile oil, Blumeae preparatum Tabellae, Rhizoma Chuanxiong extractum and Bulbus Allii Macrostemonis extractum are mixed, slight fever makes mixing, add in the fused Polyethylene Glycol (420g Macrogol 4000,280g polyethylene glycol 6000), stir evenly, move in the drop pill machine liquid reservoir, drip and make 1000g, this method of quality control do as one likes shape, discriminating, inspection and assay are formed, wherein differentiate it is discriminating to Fructus cinnamomi camphorae, Rhizoma Chuanxiong, assay be respectively according to gas chromatography among appendix VIE of Chinese Pharmacopoeia version in 2005 to the assay of eucalyptol in the drop pill and Borneolum Syntheticum.
The method of quality control of the dropping pill formulation of above-mentioned treatment obstruction of qi in the chest and cardialgia is specially:
Character: this product is the yellowish-brown drop pill, special fragrance is arranged, mildly bitter flavor;
Differentiate: be contrast, be developing solvent with the eucalyptol reference substance, according to thin layer chromatography discriminating Fructus cinnamomi camphorae with cyclohexane extraction-ethyl acetate; Be contrast, be developing solvent with the Rhizoma Chuanxiong control medicinal material, differentiate Rhizoma Chuanxiong according to thin layer chromatography with normal hexane-ethyl acetate;
Check: according to residual solvent algoscopy second method among two appendix VIIIP of Chinese Pharmacopoeia version in 2005, promptly capillary column headspace sampling system program temperature-raising method is measured the chloroform residual quantity; Other should meet among an appendix I of Chinese Pharmacopoeia version in 2005 K relevant every regulation under the drop pill item;
Assay: with the eucalyptol reference substance is contrast, is immobile phase with the SE-30 methyl silicone rubber, according to the content of eucalyptol in the gas chromatography determination drop pill among appendix VIE of Chinese Pharmacopoeia version in 2005; With the Borneolum Syntheticum reference substance is contrast, is immobile phase with the PEG-20M Polyethylene Glycol, according to the content of Borneolum Syntheticum in the gas chromatography determination drop pill among appendix VIE of Chinese Pharmacopoeia version in 2005.
The method of quality control of the dropping pill formulation of aforesaid treatment obstruction of qi in the chest and cardialgia, described discriminating is formed by following:
(1) Fructus cinnamomi camphorae is differentiated: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution; Other gets eucalyptol reference substance 20 μ l, adds dehydrated alcohol 1ml, in contrast product solution; According to thin layer chromatography test among appendix VIB of Chinese Pharmacopoeia version in 2005, drawing each 6 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, is that cyclohexane extraction-ethyl acetate of 9: 1 is developing solvent with volume ratio, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, 80 ℃ of bakings 5～10 minutes, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) Rhizoma Chuanxiong is differentiated: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution; Get Rhizoma Chuanxiong control medicinal material 0.5g, the 10ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and filtering residue adds ethyl acetate 1ml dissolving, medical material solution in contrast; According to thin layer chromatography test among appendix VIB of Chinese Pharmacopoeia version in 2005, draw each 5 μ l of need testing solution and control medicinal material solution, putting respectively on same silica gel g thin-layer plate, is that normal hexane-ethyl acetate of 9: 1 is developing solvent with volume ratio, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The method of quality control of the dropping pill formulation of aforementioned therapies obstruction of qi in the chest and cardialgia, described inspection is:
Chromatographic condition and system suitability experiment: fixative is the fused-silica capillary column of 5% phenyl-crosslinked methyl polysiloxane of 95%SE-54, column length 30m, internal diameter 0.53mm, film thickness 1.0 μ m; Temperature programming, 30 ℃ of initial temperatures keep 8min, and the heating rate with 35 ℃/min rises to 200 ℃ again, keeps 5min; Injector temperature is 230 ℃; Detector is the FID flame ionization ditector, and detector temperature is 250 ℃; Split sampling not; Headspace sampling, head space bottle equilibrium temperature is 70 ℃, and equilibration time is 40min, and sampling volume is 1.0ml; Carrier gas is a nitrogen, presses before the post to be 25kPa, and head space device pressure is 40kPa; Theoretical cam curve is calculated by the chloroform peak and is not less than 5000, and the separating degree of chloroform and two chromatographic peaks of internal standard substance should be greater than 1.5;
Correction factor is measured: get 1, the 2-dichloroethanes is an amount of, and accurate the title decides, and adds methanol and makes the inner mark solution that every 1ml contains 1,2 dichloroethanes 2.0mg; It is an amount of that other gets chloroform, and accurate the title decides, and adds methanol and makes the standard solution that every 1ml contains chloroform 3.0mg; 10ml is in 20ml head space bottle in water intaking, accurate chloroform 30 μ g and the internal standard substance 20 μ g of adding, and sealing, 70 ℃ of balances 40 minutes are got 1.0ml head space gas sampling, repeat the sample introduction secondary, use the mean value calculation correction factor;
Test sample is measured: get and be milled to pulverous test sample 0.5g, the accurate title, decide, and puts in the 20ml head space bottle, adds water 10ml and 1,2-dichloroethanes 20 μ g, sealing, 70 ℃ of balances 40 minutes are got 1.0ml head space gas sampling, repeat the sample introduction secondary, measure, use mean value calculation, should be up to specification.
The method of quality control of the dropping pill formulation of aforesaid treatment obstruction of qi in the chest and cardialgia, the assay of eucalyptol, Borneolum Syntheticum is in the described drop pill:
(1) assay of eucalyptol
Chromatographic condition and system suitability test: with the SE-30 methyl silicone rubber is immobile phase; Carrier is 60～80 whitish eye color kieselguhr, and coating concentration is 5%; 2.0m * 3.0mm, 80 ℃ of column temperatures; Flame ionization ditector, 140 ℃ of detected temperatures; Number of theoretical plate calculates by the eucalyptol peak should be not less than 1000;
The preparation of reference substance solution: it is an amount of to get the eucalyptol reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 3mg, promptly;
The preparation of need testing solution: get the about 0.5g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 3 μ l of need testing solution of drawing, inject gas chromatograph is measured, promptly;
(2) Borneolum Syntheticum assay
Chromatographic condition and system suitability test: with the PEG-20M Polyethylene Glycol is immobile phase; Carrier is 60～80 whitish eye color kieselguhr, and coating concentration is 10%; 2.0m * 3.0mm, 135 ℃ of column temperatures; Flame ionization ditector, 170 ℃ of detected temperatures; Number of theoretical plate is pressed the Borneolum Syntheticum peak and is calculated, and should be not less than 1700;
The preparation of reference substance solution: it is an amount of to get the Borneolum Syntheticum reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 5mg, promptly;
The preparation of need testing solution: get the about 0.4g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 3 μ l of need testing solution of drawing, inject gas chromatograph is measured, promptly
The method of quality control of the dropping pill formulation of aforesaid treatment obstruction of qi in the chest and cardialgia, the every ball of this product contains Fructus cinnamomi camphorae in eucalyptol, must not be less than 0.5mg; Every ball contains Blumeae preparatum Tabellae in Borneolum Syntheticum, must not be less than 1.6mg.
In order to study the method for quality control of the happy dropping pill formulation of the Cinnamomum Migao H.W.Li. heart for the treatment of obstruction of qi in the chest and cardialgia, the applicant has carried out a large amount of experiments with screening preferred plan, and is specific as follows:
One, the research of character
All meet according to many batch samples character: " this product is the yellowish-brown drop pill, special fragrance is arranged, mildly bitter flavor ", list the method for quality control text in.
Two, the research of discrimination method
Carry out the research of thin layer chromatography discrimination test at the crude drug in the prescription, the result is as follows:
Instrument and reagent: constant temperature electric heating baking oven; Vertical chromatography cylinder etc.
Reference substance or control medicinal material: eucalyptol reference substance (assay with) lot number is 110788-9202, Borneolum Syntheticum reference substance (assay with) lot number is 110881-200504, the Rhizoma Chuanxiong control medicinal material, lot number is 120918-200406, all purchase in Nat'l Pharmaceutical ﹠ Biological Products Control Institute, reagent is analytical pure in fact.
(1) effective site of Fructus cinnamomi camphorae is its volatile oil, the Fructus cinnamomi camphorae volatile oil that gets with the steam distillation extraction, light yellow, tool the spy smell, with capillary chromatography-mass spectrum-computer coupling, capillary chromatography-infrared spectrum-computer coupling, the capillary chromatography retention index and the standard substance addition method, analyzed the chemical constituent of volatile oil, identify 46 compositions, wherein main component is eucalyptol (23.75%), fragrant juniperin (10.63%), limonene (8.77%) and alpha-terpineol (6.36%) etc.Also adopt its volatile oil of extraction to feed intake when the preparation finished product, main component is an eucalyptol, can be with its composition as quality control.It is carried out TLC research.
The preparation of need testing solution: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution.
The preparation of negative control solution: get 0.5g negative control (feminine gender that lacks Fructus cinnamomi camphorae volatile oil), add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as negative control solution.Other gets eucalyptol reference substance 20 μ l, adds dehydrated alcohol 1ml dissolving, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 6 μ l of need testing solution, negative control solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (9: 1) is developing solvent, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, 80 ℃ of bakings 5～10 minutes, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, the speckle that shows same color, feminine gender is noiseless, lists the discriminating item of this product method of quality control in.
(2) with reference to a Chinese Pharmacopoeia Rhizoma Chuanxiong medical material [discriminating] (3) in 2005 item down, the Rhizoma Chuanxiong in this product is carried out TLC research.
The preparation of need testing solution: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution.
The preparation of negative control solution: get 0.5g negative control (feminine gender that lacks the Rhizoma Chuanxiong medical material), add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as negative control solution.
The preparation of reference substance solution: get Rhizoma Chuanxiong control medicinal material 0.5g, the 10ml that adds diethyl ether, ultrasonic extraction 20 minutes filters, and filtrate volatilizes, and filtering residue adds ethyl acetate 1ml dissolving, medical material solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 5 μ l of need testing solution, negative control solution and control medicinal material solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9: 1) is developing solvent, launch, take out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color, negative noiseless.List the discriminating item of this product method of quality control in.
(3) in this product quality standard formulation process, adopt " 2005 editions one Chinese crude drug Bulbus Allii Macrostemonis TLC of Chinese pharmacopoeia discrimination method, Bulbus Allii Macrostemonis in this product is carried out Study on Identification:
Need testing solution preparation: get this product 20 balls, add dehydrated alcohol (or normal hexane) 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution.
The preparation of negative control solution: get negative sample 0.5g, add dehydrated alcohol (or normal hexane) 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution.
The preparation of control medicinal material solution: get Bulbus Allii Macrostemonis control medicinal material 4g, add normal hexane 20ml, supersound process 20 minutes filters, and filtrate volatilizes, and filtering residue adds normal hexane 1ml dissolving, medical material solution in contrast.According to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 10 μ l of need testing solution, negative control solution and control medicinal material solution, put respectively on same silica gel H lamellae, with normal hexane-ethyl acetate (10: 1) is developing solvent, launch, take out, dry.Smoked clear with iodine vapor to the speckle colour developing, or spray is with 5% vanillin sulfuric acid solution, 80 ℃ of bakings 5～10 minutes.Owing to lack Bulbus Allii Macrostemonis negative control product interference is arranged, promptly negative test sample with control medicinal material and the corresponding position of test sample on the speckle of same color is arranged, should not list the TLC of Bulbus Allii Macrostemonis in quality standard as the discrimination method of this product, so do not adopt TLC method discriminating Bulbus Allii Macrostemonis.
Three, the research of Jian Chaing
(1) weight differential: this product is according to the regulation check down of (2005 editions one appendix I K of Chinese Pharmacopoeia) drop pill weight differential item, result such as table 1.
Table 1
| Lot number | Weight differential | Lot number | Weight differential |
| ??20060301 | Up to specification | ??20060406 | Up to specification |
| Lot number | Weight differential | Lot number | Weight differential |
| ??20060302 | Up to specification | ??20060501 | Up to specification |
| ??20060401 | Up to specification | ??20060502 | Up to specification |
| ??20060402 | Up to specification | ??20060503 | Up to specification |
| ??20060403 | Up to specification | ??20071001 | Up to specification |
| ??20060404 | Up to specification | ??20071002 | Up to specification |
| ??20060405 | Up to specification | ??20071003 | Up to specification |
| Lot number | Dissolve scattered time limit (min) | Lot number | Dissolve scattered time limit (min) |
| ????20060301 | 15 | ????20060406 | 15 |
| ????20060302 | 15 | ????20060501 | 15 |
| ????20060401 | 15 | ????20060502 | 15 |
| ????20060402 | 15 | ????20060503 | 15 |
| ????20060403 | 15 | ????20071001 | 15 |
| ????20060404 | 15 | ????20071002 | 15 |
| ????20060405 | 15 | ????20071003 | 15 |
4, system suitability test
4.1 system suitability experiment: result such as table 4.
Table 4 system suitability result of the test
Water intaking 10.0ml, add in the head space bottle, add chloroform 30 μ g and 1 respectively, 2-dichloroethanes 20 μ g get 1ml head space gas sampling at 70 ℃ of balance 30min, 40min, 50min, 60min, the record chromatogram, chloroform peak area and 1,2-dichloroethanes peak area changes little at 40min, 50min peak area, adopt 40min as head space bottle equilibration time.The results are shown in Table 6.
The selection of table 6 head space equilibration time
Table 8 linear relationship result of the test
| Sequence number | Add chloroform amount (μ g) | Retention time (min) | Peak area (A) |
| 1 | 12.500 | ??3.663 | ????10692 |
| 2 | 21.875 | ??3.677 | ????14412 |
| 3 | 31.250 | ??3.685 | ????21511 |
| 4 | 40.625 | ??3.583 | ????26694 |
| 5 | 50.000 | ??3.692 | ????32865 |
| 6 | 59.375 | ??3.691 | ????39804 |
Four, the research of assay
The assay of the happy drop pill of the Cinnamomum Migao H.W.Li. heart is to be quantitative target with Borneolum Syntheticum in main component of essential oil eucalyptol in the monarch drug Fructus cinnamomi camphorae and the ministerial drug Blumeae preparatum Tabellae, controls the quality of this product.
(1), the assay of eucalyptol
1, instrument and reagent
Gas chromatograph: Tianjin, island GC-14C, fid detector, Sepu3000 chromatographic work station, Tianjin, island AUW220D type (scale division value 0.01mg) electronic balance.
Eucalyptol reference substance (using) for assay, lot number 110788-9202 purchases in Nat'l Pharmaceutical ﹠ Biological Products Control Institute, and dehydrated alcohol, dichloromethane are analytical pure, sample (our company's self-control, lot number is 20060301).
2, sample treatment
(1) preparation of reference substance solution: it is an amount of to get the eucalyptol reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 3mg, promptly.
(2) preparation of need testing solution: get the about 0.5g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
(3) negative control solution (lacking Fructus cinnamomi camphorae volatile oil negative control) preparation.Get the about 0.5g of negative control product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
3, chromatographic condition
With methyl silicone rubber (SE-30) is fixative, and carrier is white diatomite (60～80 order), and coating concentration is 5%, and 2.0m * φ 3mm, column temperature are 80 ℃, flame ionization ditector, 140 ℃ of detected temperatures, N2 pressure: 100kpa; H2 pressure: 50kpa; Air pressure: 50kpa, theoretical cam curve is calculated with the eucalyptol peak, should be not less than 1000.
4, system suitability test
Take by weighing scarce Fructus cinnamomi camphorae volatile oil negative sample 0.5g, prepare negative sample solution by above definite need testing solution preparation method.Draw solvent (dehydrated alcohol), negative sample solution, reference substance solution, each 3 μ l of need testing solution respectively, inject gas chromatograph, record chromatogram, result such as table 14.
Table 14 system suitability result of the test table
| Sequence number | Sample size (μ g) | Retention time (min) | Peak area (A) |
| ????1 | ????3.0136 | ???10.027 | ????360782 |
| ????2 | ????6.0272 | ???10.039 | ????706242 |
| ????3 | ????9.0408 | ???10.060 | ????1065727 |
| ????4 | ????12.0544 | ???10.075 | ????1417329 |
| ????5 | ????15.0680 | ???10.089 | ????1757272 |
, record chromatogram, result such as table 17.
Table 17 stability experiment is table as a result
Table 22 system suitability result of the test table
6, stability test
Press method under the need testing solution preparation, prepare need testing solution, need testing solution is put under the room temperature placed, drew 3 μ l sample introductions respectively at 0,2,4,6,8 hour and measure, record chromatogram, result such as table 25.
Table 25 stability test is table as a result
9, average recovery test
Precision takes by weighing 6 parts of this product (content is 83.94mg/g), every part of 0.2g puts in the 10ml measuring bottle, the about 1ml of drip dichloromethane, add Borneolum Syntheticum reference substance solution (concentration: 5.330mg/ml) an amount of respectively, add dehydrated alcohol again and be diluted to scale, shake up, filter, get subsequent filtrate, measure record chromatogram, result such as table 28.
Table 28 average recovery result of the test
Differentiate: (1) Fructus cinnamomi camphorae is differentiated: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution; Other gets eucalyptol reference substance 20 μ l, adds dehydrated alcohol 1ml, in contrast product solution; According to thin layer chromatography test among appendix VIB of Chinese Pharmacopoeia version in 2005, drawing each 6 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, is that cyclohexane extraction-ethyl acetate of 9: 1 is developing solvent with volume ratio, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, 80 ℃ of bakings 5～10 minutes, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) Rhizoma Chuanxiong is differentiated: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution; Get Rhizoma Chuanxiong control medicinal material 0.5g, the 10ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and filtering residue adds ethyl acetate 1ml dissolving, medical material solution in contrast; According to thin layer chromatography test among appendix VIB of Chinese Pharmacopoeia version in 2005, draw each 5 μ l of need testing solution and control medicinal material solution, putting respectively on same silica gel g thin-layer plate, is that normal hexane-ethyl acetate of 9: 1 is developing solvent with volume ratio, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Check: according to residual solvent algoscopy second method among two appendix VIIIP of Chinese Pharmacopoeia version in 2005, promptly capillary column headspace sampling system program temperature-raising method is measured the chloroform residual quantity:
Chromatographic condition and system suitability experiment: fixative is the fused-silica capillary column of 5% phenyl-crosslinked methyl polysiloxane of 95%SE-54, column length 30m, internal diameter 0.53mm, film thickness 1.0 μ m; Temperature programming, 30 ℃ of initial temperatures keep 8min, and the heating rate with 35 ℃/min rises to 200 ℃ again, keeps 5min; Injector temperature is 230 ℃; Detector is the FID flame ionization ditector, and detector temperature is 250 ℃; Split sampling not; Headspace sampling, head space bottle equilibrium temperature is 70 ℃, and equilibration time is 40min, and sampling volume is 1.0ml; Carrier gas is a nitrogen, presses before the post to be 25kPa, and head space device pressure is 40kPa; Theoretical cam curve is calculated by the chloroform peak and is not less than 5000, and the separating degree of chloroform and two chromatographic peaks of internal standard substance should be greater than 1.5
Correction factor is measured: get 1, the 2-dichloroethanes is an amount of, and accurate the title decides, and adds methanol and makes the inner mark solution that every 1ml contains 1,2 dichloroethanes 2.0mg; It is an amount of that other gets chloroform, and accurate the title decides, and adds methanol and makes the standard solution that every 1ml contains chloroform 3.0mg; 10ml is in 20ml head space bottle in water intaking, accurate chloroform 30 μ g and the internal standard substance 20 μ g of adding, and sealing, 70 ℃ of balances 40 minutes are got 1.0ml head space gas sampling, repeat the sample introduction secondary, use the mean value calculation correction factor;
Test sample is measured: get and be milled to pulverous test sample 0.5g, the accurate title, decide, and puts in the 20ml head space bottle, adds water 10ml and 1,2-dichloroethanes 20 μ g, sealing, 70 ℃ of balances 40 minutes are got 1.0ml head space gas sampling, repeat the sample introduction secondary, measure, use mean value calculation, should be up to specification.
Other should meet among an appendix I of Chinese Pharmacopoeia version in 2005 K relevant every regulation under the drop pill item.
Assay:
(1) assay of eucalyptol
Chromatographic condition and system suitability test: with the SE-30 methyl silicone rubber is immobile phase; Carrier is 60～80 whitish eye color kieselguhr, and coating concentration is 5%; 2.0m * 3.0mm, 80 ℃ of column temperatures; Flame ionization ditector, 140 ℃ of detected temperatures; Number of theoretical plate calculates by the eucalyptol peak should be not less than 1000;
The preparation of reference substance solution: it is an amount of to get the eucalyptol reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 3mg, promptly;
The preparation of need testing solution: get the about 0.5g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 3 μ l of need testing solution of drawing, inject gas chromatograph is measured, promptly;
(2) Borneolum Syntheticum assay
Chromatographic condition and system suitability test: with the PEG-20M Polyethylene Glycol is immobile phase; Carrier is 60～80 whitish eye color kieselguhr, and coating concentration is 10%; 2.0m * 3.0mm, 135 ℃ of column temperatures; Flame ionization ditector, 170 ℃ of detected temperatures; Number of theoretical plate is pressed the Borneolum Syntheticum peak and is calculated, and should be not less than 1700;
The preparation of reference substance solution: it is an amount of to get the Borneolum Syntheticum reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 5mg, promptly;
The preparation of need testing solution: get the about 0.4g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 3 μ l of need testing solution of drawing, inject gas chromatograph is measured, promptly
The every ball of this product contains Fructus cinnamomi camphorae in eucalyptol (C10H18O), must not be less than 0.5mg; Every ball contains Blumeae preparatum Tabellae in Borneolum Syntheticum (C10H18O), must not be less than 1.6mg.
This product function cures mainly: hot temperature cold expelling, vital energy regualting and blood circulation-promoting pain relieving.Cure mainly deficiency of heart-YANG, the obstruction of qi in the chest and cardialgia (angina pectoris) due to the stagnation of heart-blood.Disease is seen uncomfortable in chest, chest pain, and cardiopalmus is breathed hard, and very then chest pain radiating to the back is felt cold pain very, hypopnea, pale tongue or dark, tongue fur is white, deep-thready pulse.Usage and dosage: oral.One time 10 ball, 3 times on the one.
Specification: the heavy 25mg of every ball.
Storage: sealing, shading, put shady and cool place (being no more than 20 ℃).
Claims (6)
1. method of quality control for the treatment of the dropping pill formulation of obstruction of qi in the chest and cardialgia, this drop pill prepares like this: Fructus cinnamomi camphorae 4500g, Blumeae preparatum Tabellae 90g, Rhizoma Chuanxiong 3600g, Bulbus Allii Macrostemonis 360g, more than four the flavor, by recipe quantity Fructus cinnamomi camphorae is extracted volatile oil, Rhizoma Chuanxiong extracts extractum, and Bulbus Allii Macrostemonis extracts extractum; Fructus cinnamomi camphorae volatile oil, Blumeae preparatum Tabellae, Rhizoma Chuanxiong extractum and Bulbus Allii Macrostemonis extractum are mixed, slight fever makes mixing, add in the fused Polyethylene Glycol, stir evenly, move in the drop pill machine liquid reservoir, drip and make 1000g, it is characterized in that: this method of quality control do as one likes shape, discriminating, inspection and assay are formed, wherein differentiate it is discriminating to Fructus cinnamomi camphorae, Rhizoma Chuanxiong, assay be respectively according to gas chromatography among an appendix VI of Chinese Pharmacopoeia version in 2005 E to the assay of eucalyptol in the drop pill and Borneolum Syntheticum.
2. the method for quality control of the dropping pill formulation of treatment obstruction of qi in the chest and cardialgia according to claim 1 is characterized in that:
Character: this product is the yellowish-brown drop pill, special fragrance is arranged, mildly bitter flavor;
Differentiate: be contrast, be developing solvent with the eucalyptol reference substance, according to thin layer chromatography discriminating Fructus cinnamomi camphorae with cyclohexane extraction-ethyl acetate; Be contrast, be developing solvent with the Rhizoma Chuanxiong control medicinal material, differentiate Rhizoma Chuanxiong according to thin layer chromatography with normal hexane-ethyl acetate;
Check: according to residual solvent algoscopy second method among two appendix VIII of Chinese Pharmacopoeia version in 2005 P, promptly capillary column headspace sampling system program temperature-raising method is measured the chloroform residual quantity; Other should meet among an appendix I of Chinese Pharmacopoeia version in 2005 K relevant every regulation under the drop pill item;
Assay: with the eucalyptol reference substance is contrast, is immobile phase with the SE-30 methyl silicone rubber, according to the content of eucalyptol in the gas chromatography determination drop pill among an appendix VI of Chinese Pharmacopoeia version in 2005 E; With the Borneolum Syntheticum reference substance is contrast, is immobile phase with the PEG-20M Polyethylene Glycol, according to the content of Borneolum Syntheticum in the gas chromatography determination drop pill among an appendix VI of Chinese Pharmacopoeia version in 2005 E.
3. the method for quality control of the dropping pill formulation of treatment obstruction of qi in the chest and cardialgia according to claim 1 and 2 is characterized in that: described discriminating is formed by following:
(1) Fructus cinnamomi camphorae is differentiated: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution; Other gets eucalyptol reference substance 20 μ l, adds dehydrated alcohol 1ml, in contrast product solution; According to thin layer chromatography test among an appendix VI of Chinese Pharmacopoeia version in 2005 B, drawing each 6 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, is that cyclohexane extraction-ethyl acetate of 9: 1 is developing solvent with volume ratio, launch, take out, dry, spray is with 5% vanillin sulfuric acid solution, 80 ℃ of bakings 5～10 minutes, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(2) Rhizoma Chuanxiong is differentiated: get this product 20 balls, add dehydrated alcohol 5ml, slight fever makes dissolving, is chilled to room temperature, filters, and gets filtrate as need testing solution; Get Rhizoma Chuanxiong control medicinal material 0.5g, the 10ml that adds diethyl ether, supersound process 20 minutes filters, and filtrate volatilizes, and filtering residue adds ethyl acetate 1ml dissolving, medical material solution in contrast; According to thin layer chromatography test among an appendix VI of Chinese Pharmacopoeia version in 2005 B, draw each 5 μ l of need testing solution and control medicinal material solution, putting respectively on same silica gel g thin-layer plate, is that normal hexane-ethyl acetate of 9: 1 is developing solvent with volume ratio, launches, take out, dry, put under the uviol lamp 365nm and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
4. the method for quality control of the dropping pill formulation of treatment obstruction of qi in the chest and cardialgia according to claim 1 and 2 is characterized in that: described inspection is:
Chromatographic condition and system suitability experiment: fixative is the fused-silica capillary column of 5% phenyl-crosslinked methyl polysiloxane of 95%SE-54, column length 30m, internal diameter 0.53mm, film thickness 1.0 μ m; Temperature programming, 30 ℃ of initial temperatures keep 8min, and the heating rate with 35 ℃/min rises to 200 ℃ again, keeps 5min; Injector temperature is 230 ℃; Detector is the FID flame ionization ditector, and detector temperature is 250 ℃; Split sampling not; Headspace sampling, head space bottle equilibrium temperature is 70 ℃, and equilibration time is 40min, and sampling volume is 1.0ml; Carrier gas is a nitrogen, presses before the post to be 25kPa, and head space device pressure is 40kPa; Theoretical cam curve is calculated by the chloroform peak and is not less than 5000, and the separating degree of chloroform and two chromatographic peaks of internal standard substance should be greater than 1.5;
Correction factor is measured: get 1, the 2-dichloroethanes is an amount of, accurately claims surely, adds methanol and makes every 1ml and contain 1, the inner mark solution of 2-dichloroethanes 2.0mg; It is an amount of that other gets chloroform, and accurate the title decides, and adds methanol and makes the standard solution that every 1ml contains chloroform 3.0mg; 10ml is in 20ml head space bottle in water intaking, accurate chloroform 30 μ g and the internal standard substance 20 μ g of adding, and sealing, 70 ℃ of balances 40 minutes are got 1.0ml head space gas sampling, repeat the sample introduction secondary, use the mean value calculation correction factor;
Test sample is measured: get and be milled to pulverous test sample 0.5g, the accurate title, decide, and puts in the 20ml head space bottle, adds water 10ml and 1,2-dichloroethanes 20 μ g, sealing, 70 ℃ of balances 40 minutes are got 1.0ml head space gas sampling, repeat the sample introduction secondary, measure, use mean value calculation, should be up to specification.
5. the method for quality control of the dropping pill formulation of treatment obstruction of qi in the chest and cardialgia according to claim 1 and 2 is characterized in that: the assay of eucalyptol, Borneolum Syntheticum is in the described drop pill:
(1) assay of eucalyptol
Chromatographic condition and system suitability test: with the SE-30 methyl silicone rubber is immobile phase; Carrier is 60～80 whitish eye color kieselguhr, and coating concentration is 5%; 2.0m * 3.0mm, 80 ℃ of column temperatures; Flame ionization ditector, 140 ℃ of detected temperatures; Number of theoretical plate calculates by the eucalyptol peak should be not less than 1000;
The preparation of reference substance solution: it is an amount of to get the eucalyptol reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 3mg, promptly;
The preparation of need testing solution: get the about 0.5g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 3 μ l of need testing solution of drawing, inject gas chromatograph is measured, promptly;
(2) Borneolum Syntheticum assay
Chromatographic condition and system suitability test: with the PEG-20M Polyethylene Glycol is immobile phase; Carrier is 60～80 whitish eye color kieselguhr, and coating concentration is 10%; 2.0m * 3.0mm, 135 ℃ of column temperatures; Flame ionization ditector, 170 ℃ of detected temperatures; Number of theoretical plate is pressed the Borneolum Syntheticum peak and is calculated, and should be not less than 1700;
The preparation of reference substance solution: it is an amount of to get the Borneolum Syntheticum reference substance, and accurate the title decides, and adds dehydrated alcohol and makes the solution that every 1ml contains 5mg, promptly;
The preparation of need testing solution: get the about 0.4g of this product, the accurate title, decide, and puts in the 10ml measuring bottle, and the about 1ml of drip dichloromethane adds dehydrated alcohol and is diluted to scale, shakes up, and filters, and gets subsequent filtrate, promptly;
Algoscopy: accurate respectively reference substance solution and each 3 μ l of need testing solution of drawing, inject gas chromatograph is measured, promptly.
6. according to the method for quality control of the dropping pill formulation of claim 1,2 or 5 described treatment obstruction of qi in the chest and cardialgia, it is characterized in that: the every ball of this product contains Fructus cinnamomi camphorae in eucalyptol, must not be less than 0.5mg; Every ball contains Blumeae preparatum Tabellae in Borneolum Syntheticum, must not be less than 1.6mg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910312108.3A CN101708274B (en) | 2009-12-23 | 2009-12-23 | Quality control method of pill preparation for treating chest impediment and cardialgia |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910312108.3A CN101708274B (en) | 2009-12-23 | 2009-12-23 | Quality control method of pill preparation for treating chest impediment and cardialgia |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101708274A true CN101708274A (en) | 2010-05-19 |
| CN101708274B CN101708274B (en) | 2014-03-05 |
Family
ID=42401096
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910312108.3A Active CN101708274B (en) | 2009-12-23 | 2009-12-23 | Quality control method of pill preparation for treating chest impediment and cardialgia |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101708274B (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102552496A (en) * | 2010-12-16 | 2012-07-11 | 贵州万胜药业有限责任公司 | Quality detection method of compound stomachache treating capsules |
| CN103105447A (en) * | 2011-11-09 | 2013-05-15 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN103341354A (en) * | 2013-06-08 | 2013-10-09 | 重庆海洲化学品有限公司 | Analysis of trichloromethane stationary phase by gas chromatography method, and preparation method and applications of stationary phase |
| CN103768349A (en) * | 2012-10-24 | 2014-05-07 | 贵州益佰制药股份有限公司 | Application of four-component fructus cinnamoii preparation in preparing drugs for treatment of cerebrovascular and related diseases |
| CN103768348A (en) * | 2012-10-24 | 2014-05-07 | 贵州益佰制药股份有限公司 | Pharmaceutical composition and medicinal preparation used for treating cardiovascular and cerebrovascular diseases, and applications and preparation method thereof |
| CN107202853A (en) * | 2017-06-30 | 2017-09-26 | 吉林省东方制药有限公司 | The finger-print and high performance liquid chromatography discrimination method of stasis open capsule |
| CN108310188A (en) * | 2018-05-10 | 2018-07-24 | 湖南康尔佳制药股份有限公司 | A kind of Chinese medicine composition and preparation method for treating angiocardiopathy |
| CN109668851A (en) * | 2019-03-04 | 2019-04-23 | 安徽协和成制药有限公司 | The quality standard detecting method of monarch drug in a prescription glossy ganoderma extract in a kind of pearl ganoderma lucidum slice |
| CN115420832A (en) * | 2022-09-20 | 2022-12-02 | 贵州医科大学 | GC-MS fingerprint spectrum and multi-index content determination method of litsea pungens oil |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4906470A (en) * | 1986-09-22 | 1990-03-06 | Yaguang Liu | Pharmaceutical composition for treating and preventing cardiovascular disease |
| CN1265828C (en) * | 2003-08-29 | 2006-07-26 | 贵州民族制药厂有限公司 | Chinese medicine preparation for curing coronary heart disease and angina pectoris and its preparation method |
-
2009
- 2009-12-23 CN CN200910312108.3A patent/CN101708274B/en active Active
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102552496A (en) * | 2010-12-16 | 2012-07-11 | 贵州万胜药业有限责任公司 | Quality detection method of compound stomachache treating capsules |
| CN103105447A (en) * | 2011-11-09 | 2013-05-15 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN103105447B (en) * | 2011-11-09 | 2014-09-24 | 贵州益佰制药股份有限公司 | Detection method for Cinnamomum migao heart-comforting preparation |
| CN103768349A (en) * | 2012-10-24 | 2014-05-07 | 贵州益佰制药股份有限公司 | Application of four-component fructus cinnamoii preparation in preparing drugs for treatment of cerebrovascular and related diseases |
| CN103768348A (en) * | 2012-10-24 | 2014-05-07 | 贵州益佰制药股份有限公司 | Pharmaceutical composition and medicinal preparation used for treating cardiovascular and cerebrovascular diseases, and applications and preparation method thereof |
| CN103768349B (en) * | 2012-10-24 | 2017-03-01 | 贵州益佰制药股份有限公司 | Application in preparation treatment cerebrovascular and relevant disease medicine for the four taste Fructus cinnamomi camphorae preparations |
| CN103341354A (en) * | 2013-06-08 | 2013-10-09 | 重庆海洲化学品有限公司 | Analysis of trichloromethane stationary phase by gas chromatography method, and preparation method and applications of stationary phase |
| CN107202853A (en) * | 2017-06-30 | 2017-09-26 | 吉林省东方制药有限公司 | The finger-print and high performance liquid chromatography discrimination method of stasis open capsule |
| CN108310188A (en) * | 2018-05-10 | 2018-07-24 | 湖南康尔佳制药股份有限公司 | A kind of Chinese medicine composition and preparation method for treating angiocardiopathy |
| CN109668851A (en) * | 2019-03-04 | 2019-04-23 | 安徽协和成制药有限公司 | The quality standard detecting method of monarch drug in a prescription glossy ganoderma extract in a kind of pearl ganoderma lucidum slice |
| CN115420832A (en) * | 2022-09-20 | 2022-12-02 | 贵州医科大学 | GC-MS fingerprint spectrum and multi-index content determination method of litsea pungens oil |
| CN115420832B (en) * | 2022-09-20 | 2024-03-19 | 贵州医科大学 | GC-MS fingerprint spectrum and multi-index content determination method for litsea coreana oil |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101708274B (en) | 2014-03-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101708274A (en) | Quality control method of pill preparation for treating chest impediment and cardialgia | |
| CN103381217B (en) | A kind of Liuweibuxue capsule and method of quality control thereof and application | |
| CN102688431A (en) | Kidney-reinforcing oral liquid and preparation method thereof | |
| CN109342631A (en) | The construction method of the HPLC finger-print of Chinese medicine composition and the quality determining method of Chinese medicine composition | |
| CN102590433A (en) | Ganchang preparation quality detection method | |
| CN103399094A (en) | Fingerprint spectrum detection method of pills for treating hyperplasia of mammary glands | |
| CN102100818A (en) | Quality control method for lophanthus antifebrile tablets | |
| CN101708208B (en) | Detection method of capsule preparation for treating painful swollen joint | |
| CN102426205B (en) | Detection method of thrombus sumalin capsules | |
| CN102038908B (en) | Detection method of tambac depression-alleviating pill as traditional Chinese medical preparation | |
| CN100464188C (en) | Quality control method of medicinal preparation for treating lypemania | |
| CN110780004A (en) | Method for establishing fingerprint of traditional Chinese medicine composition or preparation thereof with depression mood regulating effect | |
| CN102068549B (en) | Detection method for Chinese medicinal preparation heat clearing and blood cooling pills | |
| CN102778529B (en) | Method for testing quality of tibetan medicine composition Liuwei Datuoyeyunshi preparation | |
| CN110441407A (en) | A kind of pool art tablet quality control method | |
| CN103211907A (en) | Siwu decoction formulated particles, and preparation method and detection method thereof | |
| CN102507844B (en) | Testing method for Xueshuan xinmaining tablet | |
| CN102357231A (en) | Quality control method of compound fructus embeliae haemorrhoid suppository and preparation thereof | |
| CN103823016B (en) | Detecting method of DanTianJingShu oral preparation | |
| CN102706978B (en) | Wild chrysanthemum flower extractive and fingerprint spectrum detection method thereof | |
| CN101269203A (en) | Quality control testing method for brain-invigorating and heart-soothing capsule | |
| CN105169234B (en) | A kind of quality determining method of Chinese materia medica preparation that treating diabetic retinopathy | |
| CN106728651A (en) | The preparation method and its method of quality control of a kind of rhizoma cyperi SIWU KELI | |
| CN101953978A (en) | Heart-soothing and lipid-lowering tablet medicine quality standard detecting method | |
| CN102138973B (en) | Quality control method for six-meridian headache tablets |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| ASS | Succession or assignment of patent right |
Owner name: YIBAI PHARMACEUTICAL CO., LTD., GUIZHOU Free format text: FORMER OWNER: GUIZHOU NATIONAL PHARMACY CO., LTD. Effective date: 20111026 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 550025 GUIYANG, GUIZHOU PROVINCE TO: 550008 GUIYANG, GUIZHOU PROVINCE |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20111026 Address after: 550008 Baiyun Avenue, Guizhou, Guiyang 220-1 Applicant after: Yibai Pharmaceutical Co., Ltd., Guizhou Address before: 550025 Huaxi, Guizhou Province, Dong Dong weir Applicant before: Guizhou National Pharmacy Co., Ltd. |
|
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |