CN101543545B - Traditional Chinese medicine preparation for curing rhinitis and quality control method thereof - Google Patents
Traditional Chinese medicine preparation for curing rhinitis and quality control method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 58
- 239000003814 drug Substances 0.000 title claims abstract description 14
- 206010039083 rhinitis Diseases 0.000 title claims abstract description 6
- 238000003908 quality control method Methods 0.000 title description 10
- 238000000034 method Methods 0.000 claims abstract description 42
- 238000001514 detection method Methods 0.000 claims abstract description 33
- 241000205585 Aquilegia canadensis Species 0.000 claims abstract 2
- 238000012360 testing method Methods 0.000 claims description 104
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 41
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a traditional Chinese medicine preparation for curing rhinitis and a quality checking method thereof, by optimizing and screening preparation technological parameters of the preparation, in the quality checking method of the preparation, the lamella qualitative detection of honeysuckle and gamene and the quantitive detection of magnolin are carried out, thereby ensuring the security and the effectiveness of the medicine, improving the quality of products and being convenient for standardizing production.
Description
Technical field
The present invention relates to a kind of Chinese medicine preparation and method of quality control thereof for the treatment of rhinitis, belong to technical field of Chinese medicines.
Background technology
6 204 pages in Chinese traditional patent formulation preparation promulgated by the ministries or commissions of the Central Government, standard No. is WS3-B-1266-92, its function cures mainly and is the lung qi dispersing that dispels the wind, heat-clearing and toxic substances removing, understand things pain-stopping.Be used to the nasal sinusitis of having a stuffy nose, it is not smooth to ventilate, and the watery nasal discharge Huang is turbid, has a bad nose headache, superciliary ridge disease.But its preparation technology is more coarse, make by the product quality of this method preparation uneven, its method of quality control has only a physicochemical identification, be difficult to reflect the real quality and the curative effect of medicine, so be necessary its preparation technology is further studied, and corresponding method of quality control improved, so that the quality of medicine and curative effect are guaranteed.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine preparation;
The object of the invention also is to provide the method for quality control of this Chinese medicine preparation.
For realizing above goal of the invention, the technical solution used in the present invention is as follows:
A kind of Chinese medicine preparation for the treatment of rhinitis, said preparation are to be made by the raw material of following weight ratio,
Fructus Xanthii 1664g Flos Magnoliae 312g Flos Chrysanthemi Indici 104g
Flos Lonicerae 104g Radix Rubiae 104g
The preparation method of said preparation is:
Above five tastes medical material is got Flos Magnoliae and Flos Chrysanthemi Indici and is added 12 times of water gaging distillations extraction in 5 hours volatile oil, and the aqueous solution after distillation device is in addition collected; Fructus Xanthii extracting in water twice, 2 hours for the first time, amount of water was 8 times, and 1 hour for the second time, amount of water was 6 times, and collecting decoction filters, and filtrate is left standstill; Flos Lonicerae adds water in 70～80 ℃ of warm macerating secondaries, 2 hours for the first time, amount of water is 10 times, and 1 hour for the second time, amount of water was 8 times, merge immersion, filter, filtrate is left standstill, and merges above-mentioned two kinds of clarification medicinal liquids and Flos Magnoliae and Flos Chrysanthemi Indici aqueous solution, in temperature is 70 ℃, and pressure is 1.20 extractum for concentrating under reduced pressure under the-0.06Mpa condition becomes relative density; Other gets Radix Rubiae and is ground into coarse powder, makes solvent with 8 times of amount 70% ethanol, floods after 48 hours, with the speed percolation of 5ml/minkg, collect the liquid of filtering, reclaim ethanol, relative density is 1.02 extractum when being concentrated into 60 ℃, leaves standstill, and gets supernatant and above-mentioned concentrated solution and merges, leave standstill, filter, filtrate is 70 ℃ in temperature, pressure is-the 0.06Mpa condition under concentrating under reduced pressure, being concentrated into relative density is 1.25～1.30, add sucrose 800g and potassium sorbate 1.67g, boil dissolving, filter, put cold, add volatile oil such as above-mentioned Flos Magnoliae, add water to 1000ml, stir evenly, fill, 105 ℃ of flowing steam sterilization 30min promptly.
The method of quality control of said preparation comprises one or more in following a, b, three kinds of detection methods of c:
A. the qualitative detection of Flos Lonicerae
Get preparation of the present invention and extract with the chloroform jolting, evaporate to dryness, residue add methanol makes dissolving, as need testing solution.
The extracting honeysuckle control medicinal material adds the chloroform supersound process in addition, filters, and filtrate evaporate to dryness, residue add methanol makes dissolving, in contrast medical material solution.
Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone is developing solvent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
B. the qualitative detection of Radix Rubiae
Get preparation of the present invention, extract combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness, residue add ethyl acetate makes dissolving, as need testing solution.
Other gets the Radix Rubiae control medicinal material, adds the ethyl acetate supersound process, filters, and filtrate evaporate to dryness, residue add ethyl acetate makes dissolving, in contrast medical material solution.
According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone is developing solvent, launches, and takes out, dry, put under the uviol lamp and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
C. the detection by quantitative of magnelin
Get the magnelin reference substance, the accurate title, decide, and makes reference substance solution with dissolve with methanol, promptly.
Precision takes by weighing preparation of the present invention, puts in the separatory funnel, and thin up disperses, and adds ethyl acetate extraction, collects extracting solution, water bath method, and residue adds dissolve with methanol, puts in the volumetric flask, is settled to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Accurate respectively reference substance solution, the need testing solution drawn injects chromatograph of liquid, measures, promptly.
The every 1g of preparation of the present invention contains Flos Magnoliae with magnelin (C
23H
28O
7) the amount meter, must not be less than 50 μ g.
This method of quality control can also be one or more in following a, b, three kinds of detection methods of c:
A. the qualitative detection of Flos Lonicerae
Get preparation 50ml of the present invention, extract 4 times with the chloroform jolting, each 30ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
Extracting honeysuckle control medicinal material 1g adds chloroform 10ml supersound process 30 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.
Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (5: 1) is developing solvent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue spot.
B. the qualitative detection of Radix Rubiae
Get preparation 50ml of the present invention, extract 4 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.
Other gets Radix Rubiae control medicinal material 1g, adds ethyl acetate 10ml supersound process 30 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution.
Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (10: 0.5) 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 identical yellow green speckle.
C. the detection by quantitative of magnelin
With the octadecylsilane chemically bonded silica is filler; With acetonitrile-water-oxolane (38: 61: 1) is mobile phase; The detection wavelength is 278nm.Number of theoretical plate calculates by the magnelin peak should be not less than 2000.
It is an amount of to get the magnelin reference substance, accurate claims surely, makes the solution that every 1ml contains 65 μ g with dissolve with methanol, product solution in contrast, promptly.
Precision takes by weighing this preparation 20g, puts in the separatory funnel, adds water 20ml dilution and disperses, and adds ethyl acetate extraction 5 times, each 50ml, collect extracting solution, water bath method, residue adds dissolve with methanol, puts in the 25ml volumetric flask, is settled to scale, shake up, filter, get subsequent filtrate, promptly.Accurate respectively reference substance solution 5 μ l, the need testing solution 10 μ l of drawing inject chromatograph of liquid, measure, promptly.
The every 1g of this preparation contains Flos Magnoliae with magnelin (C
23H
28O
7) the amount meter, must not be less than 50 μ g
This preparation method, drawn the production process control parameter of optimizing in conjunction with pharmacodynamics and pharmacy test, and drawn by test of many times that thin layer is differentiated and content assaying method has carried out qualitative and detection by quantitative to the active ingredient of medicine, made said preparation have curative effect height, stay-in-grade characteristics.
The specific embodiment
Following experimental example and embodiment further specify but are not limited to the present invention down.
Experimental example 1. Study on extraction
1. volatile oil Study on extraction
1. extracting amount of water investigates:
Take by weighing 3 parts of Flos Magnoliae, Flos Chrysanthemi Indici two flavor medical materials by embodiment 1, add 10 times, 12 times, 14 times water gagings respectively, distilled respectively 5 hours, respectively testing gained extraction volatile oil with collection is index, determines to extract amount of water.The results are shown in Table 1:
Table 1 Flos Magnoliae, Flos Chrysanthemi Indici extract amount of water and investigate
With the oil pump capacity is index, second group as can be seen (12 times of amount of water), the 3rd group (14 times of amount of water), oil yield is more or less the same, and is energy savings and shortening production time, so second group of test parameters adopted in decision in big the production.
2. distillation time is investigated:
Take by weighing 3 parts of Flos Magnoliae, Flos Chrysanthemi Indici three flavor medical materials, respectively add 12 times of amounts of water, distilled respectively 4 hours, 5 hours, 6 hours, respectively testing gained extraction volatile oil with collection is index, determines extraction time.The results are shown in Table 2:
Table 2 extracts amount of water and investigates
With the oil pump capacity is index, second group as can be seen (extracting 5 hours), the 3rd group (extracting 6 hours), oil yield is more or less the same, and is energy savings and shortening production time, so second group of test parameters adopted in decision in big the production.Promptly adding 12 times of amounts of water extracted 5 hours.
2. extract the amount of water technical study:
Get 3 parts of medical materials of Fructus Xanthii, every part of 1664g, twice of extracting in water, decocted 2 hours for the first time, decocted 1 hour for the second time, divide 3 groups to test, 6 times of amounts of first group of amount of water, 4 times of amounts, 8 times of amounts of second group of amount of water, 6 times of amounts, 10 times of amounts of the 3rd group of amount of water, 8 times of amounts, collecting decoction, filter, leave standstill, get supernatant concentration to relative density and be 1.20 clear paste (60 ℃), to go out the clear paste amount is index, determines amount of water.The results are shown in Table 3.
Table 3: water is carried amount of water
To go out the clear paste amount is index, second group as can be seen (8 times of amounts of amount of water, 6 times of amounts), the 3rd group (10 times of amounts of amount of water, 8 times of amounts), paste-forming rate is more or less the same, for energy savings and shortening production time, so decision is adopted second group in big the production.Be extracting in water twice, 2 hours for the first time, amount of water was 8 times, and 1 hour for the second time, amount of water was 6 times.
3. warm macerating amount of water technical study:
Every part of 104g of 3 parts of medical materials of extracting honeysuckle adds water temperature and soaks twice, and warm macerating is 2 hours for the first time, warm macerating is 1 hour for the second time, divides 3 groups to test, 8 times of amounts of first group of amount of water, 6 times of amounts, 10 times of amounts of second group of amount of water, 8 times of amounts, 10 times of amounts of the 3rd group of amount of water, 10 times of amounts, collecting decoction filters, leave standstill, getting supernatant concentration, to become relative density be 1.20 clear paste (60 ℃), is index to go out the clear paste amount, determines amount of water.The results are shown in Table 4:
Table 4: warm macerating amount of water
To go out the clear paste amount is index, second group as can be seen (10 times of amounts of amount of water, 8 times of amounts), the 3rd group (10 times of amounts of amount of water, 10 times of amounts), paste-forming rate is more or less the same, for energy savings and shortening production time, so the 3rd group of test parameters adopted in decision in big the production.Promptly add water temperature and soak twice, 2 hours for the first time, amount of water was 10 times, and 1 hour for the second time, amount of water was 8 times.
4. percolation technical study:
Get every part of 104g of 3 parts of medical materials of Radix Rubiae, add equivalent 70% ethanol moistening respectively, fitted tube adds 2 times of amount 70% ethanol, flooded 48 hours, add 5 times of amount percolation continuously, percolation speed is respectively: first group of 3ml/min*kg, second group of 5ml/min*kg, the 3rd group of 7ml/min*kg, collect percolate, reclaim ethanol, being condensed into relative density and being 1.02 extractum (60 ℃), is index to go out the clear paste amount, determines technological parameter.The results are shown in Table 5:
Table 5 percolation technical study
To go out the clear paste amount is index, as can be seen with the speed percolation of second group of 5ml/min*kg, can reach preferably the seepage effect and can save time.
Get 3 parts of medical materials of Radix Rubiae, every part of 104g adds 6 times of 70% ethanol, 8 times, 10 times amounts respectively, flooded 48 hours, and percolation, percolation speed 5ml/min*kg collects percolate.Main chemical compositions is an anthraquinone component in the Radix Rubiae, shows red (getting ethanol liquid 10ml, hydro-oxidation sodium test solution 2ml) with the sodium hydroxide reaction and determines amount of alcohol for index.The results are shown in Table 6:
Table 6 is determined amount of alcohol
To go out the clear paste amount is index, and second group of result of the test is close with the 3rd group of result of the test as can be seen, determines that the technological parameter consumption is 8 times of amounts of 70% ethanol, the speed percolation of 5ml/min*kg.
5. demonstration test
According to above-mentioned preferred condition, verify three batches, the results are shown in Table 7,8,9,10.
Table 7 volatile oil test data
Table 8 water is carried the amount of water test data
Table 9 warm macerating amount of water test data
Table 10 percolation tests data
As seen, demonstration test result and result of study are more approaching, and technological parameter is more stable, determine technological parameter thus.
The research of experimental example 2. concentration technologies:
1. concentration technology research for the first time:
Get and extract that three batches of demonstration test volatile oil, water are carried, clear paste carries out concentration technology research under the warm macerating item, concentrating under reduced pressure (70 ℃ ,-0.06Mpa) to become relative density be 1.20 extractum, is index to go out clear paste amount degree of balance, determines technological parameter.Result of the test sees Table 11.
The research of table 11 concentration technology
2. concentration technology research for the second time:
Get and extract that clear paste and above-mentioned concentrated gained extractum carry out concentration technology research under three batches of demonstration test percolation items, by carry out under the former process recipes item concentrating under reduced pressure (70 ℃ ,-0.06Mpa), dispose last cumulative volume, determine medicinal liquid density to concentrate volume, result of the test sees Table 12.
Table 12 concentration technology research for the second time
The The above results table as seen, density when extractum is concentrated into 390ml, density is defined as 1.25～1.30.
The screening of experimental example 3 sterilising conditions
Respectively at 105 ℃, 105 ℃, 105 ℃ following flowing steam sterilizations 30,40,45min, investigate the outward appearance of sample, the indexs such as front and back pH value, content of sterilizing after the fill.The results are shown in Table 13.
Table 13 sterilising conditions is to the influence of medicinal liquid
Conclusion: through investigating this product solution, outward appearance, the pH value before and after the sterilization, have no significant change through 105 ℃ of following flowing steam sterilizations 30,40,45min.So selecting the sterilising conditions of this product solution is 105 ℃ of following flowing steam sterilization 30min.
The qualitative checking method research of experimental example 4 Flos Loniceraes
Get this product 50ml, extract 4 times with the chloroform jolting, each 30ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Extracting honeysuckle control medicinal material 1g adds chloroform 10ml supersound process 30 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (5: 1) is developing solvent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue spot.
1, sample and reference substance extract the preferred of solvent in the qualitative detection of Flos Lonicerae:
Get by totally 4 parts of embodiment 1 resulting product 50ml, extract 4 times with the following solvents jolting, each 30ml, merge extractive liquid,, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Measure wherein chlorogenic acid content, the results are shown in following table:
Table 14 extracts the optimization experiment result of solvent
| Solvent species | Ethyl acetate | Chloroform | Ether | Petroleum ether |
| Chlorogenic acid content (mg) | 45.2? | 53.3? | 35.6? | 35.7? |
As can be seen from Table 1, handle the extraction that just relatively is suitable for chlorogenic acid with chloroform, so the preparation preferred solvent of this laboratory sample solution is a chloroform.
2, developing solvent consumption proportion preferred in this detection method:
Get need testing solution, with each 10 μ l point of control medicinal material solution of method preparation on different silica gel g thin-layer plates, using petroleum ether (30～60 ℃)-acetone proportioning respectively is that 3: 1,4: 1,5: 1,6: 1,7: 1 developing solvent launches, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, be heated to the speckle colour developing at 105 ℃, observe the unfolded effect of each speckle of test sample on each lamellae, the results are shown in following table:
Table 15 developing solvent consumption proportion optimization experiment result
| The developing solvent proportioning | 3∶1? | 4∶1? | 5∶1? | 6∶1? | 7∶1? |
| Launch effect | Very poor | Difference | Good | Relatively poor | Hangover appears |
Developing solvent proportioning as can be seen from Table 2 is 5: 1 o'clock, and it is best that need testing solution launches effect, and appearance hangover, principal spot separate phenomenons such as bad.
3, sample solution point sample amount preferred in this detection method:
Get test sample and reference substance solution each 4 μ l, 6 μ l, 8 μ l, 10 μ l, 12 μ l respectively, point is on same silica gel g thin-layer plate, launch with petroleum ether (30～60 ℃)-developing solvent of 5: 1 of acetone, take out, dry, spray is heated to the speckle colour developing with 5% phosphomolybdic acid ethanol solution at 105 ℃, observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
Table 16 sample solution point sample amount optimization experiment result
| The point sample amount | 4μl? | 6μl? | 8μl? | 10μl? | 12μl? |
| Effect | Test sample is at corresponding reference substance position immaculate | Test sample is more shallow in the colour developing of corresponding reference substance position speckle | Test sample is more shallow in the colour developing of corresponding reference substance position speckle | Test sample develops the color at corresponding reference substance position speckle | Test sample separates bad at corresponding reference substance position speckle |
Test sample point sample amount is when 10 μ l as can be seen from Table 3, and color developing effect is good on lamellae, is fit to test requirements document.
4, negative control test
Get the negative sample that lacks Flos Lonicerae, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected test experience specificity is strong according to need testing solution preparation method in the above-mentioned detection method.
The detection method of determining Flos Lonicerae in the preparation of the present invention according to above experiment is:
Get preparation 50ml of the present invention, extract 4 times with the chloroform jolting, each 30ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Extracting honeysuckle control medicinal material 1g adds chloroform 10ml supersound process 30 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (5: 1) is developing solvent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue spot.
The qualitative checking method research of experimental example 5 Radix Rubiaes
1, sample and reference substance extract the preferred of solvent in the qualitative detection of Radix Rubiae:
Get by totally 4 parts of embodiment 1 resulting product 50ml, extract 4 times with the following solvents jolting, each 30ml, merge extractive liquid,, evaporate to dryness, residue add same solvent 1ml makes dissolving, as need testing solution.Measure wherein rubican content, the results are shown in following table:
Table 17 extracts solvent optimization experiment result
| Solvent species | Petroleum ether | Ether | Ethyl acetate | Chloroform |
| Rubican content (mg) | 6.8? | 9.9? | 15.2? | 11.5? |
As can be seen from Table 1, handle the extraction that just relatively is suitable for rubican with ethyl acetate, so the preparation preferred solvent of this laboratory sample solution is an ethyl acetate.
2, developing solvent consumption proportion preferred in this detection method:
Get need testing solution, with each 10 μ l point of control medicinal material solution of method preparation on different silica gel g thin-layer plates, using petroleum ether (30～60 ℃)-acetone proportioning respectively is that 10: 2.5,10: 2.0,10: 1.5,10: 1.0,10: 0.5 developing solvent launches, take out, dry, put under the uviol lamp (365nm) and inspect, observe the unfolded effect of each speckle of test sample on each lamellae, the results are shown in following table:
Table 18 developing solvent consumption proportion optimization experiment result
| The developing solvent proportioning | 10∶2.5? | 10∶2.0? | 10∶1.5? | 10∶1.0? | 10∶0.5? |
| Launch effect | Very poor | Difference | Relatively poor | Relatively poor | Good |
Developing solvent proportioning as can be seen from Table 2 is 10: 0.5 o'clock, and it is best that need testing solution launches effect, and appearance hangover, principal spot separate phenomenons such as bad.
3, sample solution point sample amount preferred in this detection method:
Get test sample and reference substance solution each 4 μ l, 5 μ l, 8 μ l, 10 μ l, 12 μ l respectively, point is on same silica gel g thin-layer plate, with petroleum ether (30～60 ℃)-acetone proportioning is that 10: 0.5 developing solvent launches, take out, dry, put under the uviol lamp (365nm) and inspect, observe the effect of test sample principal spot colour developing on the lamellae, the results are shown in following table:
Table 19 sample solution point sample amount optimization experiment result
| The point sample amount | 4μl? | 5μl? | 8μl? | 10μl? | 12μl? |
| Effect | Test sample is more shallow in corresponding reference substance position spot colors | Test sample is clear in the colour developing of corresponding reference substance position speckle | Test sample is clear in the colour developing of corresponding reference substance position speckle | Test sample is clear in the colour developing of corresponding reference substance position speckle | Test sample separates bad at corresponding reference substance position speckle |
[0138]Test sample point sample amount is when 5～10 μ l as can be seen from Table 3, and color developing effect is good on lamellae, is fit to test requirements document.
4, negative control test
Get the negative sample that lacks Radix Rubiae, prepare negative control solution, launch the back and corresponding speckle on the reference substance solution correspondence position, do not occur, illustrate that selected test experience specificity is strong according to need testing solution preparation method in the above-mentioned detection method.
The detection method of determining Radix Rubiae in the preparation of the present invention according to above experiment is:
Get preparation 50ml of the present invention, extract 4 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets Radix Rubiae control medicinal material 1g, adds ethyl acetate 10ml supersound process 30 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (10: 0.5) 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 identical yellow green speckle.
The content detection of experimental example 6 magnelins
1. instrument and sample
Detecting instrument: Tianjin, the island SPD-10ATvp of company type high performance liquid chromatograph
Injector: automatic sampler
Chromatographic column: enlightening horse (Diamonsil C
184.6 * 150mm, 5 μ m)
Mobile phase: acetonitrile-water-oxolane (38: 61: 1) (acetonitrile chromatographic grade, water are redistilled water, the oxolane chromatographic grade)
Flow velocity: 1.0ml/min
Detect wavelength: 278nm
Column temperature: room temperature
The reference substance source: magnelin is purchased lot number: the 110882-200504 in Nat'l Pharmaceutical ﹠ Biological Products Control Institute
Assay method: get assay by embodiment 1[] down the preparation method of need testing solution prepare sample liquid; And by preparing the blank sample that lacks Flos Magnoliae under [method for making] item, the preparation negative controls.With microporous filter membrane (0.45 μ m), accurate respectively each the 10 μ l of reference substance solution, negative controls and need testing solution that draw inject chromatograph of liquid, measure, promptly.
2. content assaying method is investigated
(1) linear relationship is investigated and to be got reference substance solution (65 μ g/ml) and shake up, accurate respectively 3,5,7,10,12, the 15 μ l of absorption inject high performance liquid chromatograph, measure peak area, the results are shown in Table 20, and drawing standard curve, the result shows that magnelin is linear between 195 μ g～975 μ g, and its regression equation is: Area=508.14x-375.69 (r=0.9999).
Table 20 linear relationship is investigated the result
(2) stability test need testing solution respectively at preparing the back 0,2,4,6,12,24 hour, is measured in accordance with the law, sampling volume 10 μ l, and the result shows that it is basicly stable in 24 hours, the results are shown in Table 21.
Table 21 stability test result
(3) precision test
The accurate need testing solution 10 μ l that draw repeat sample introduction 5 times, try to achieve relative standard deviation＜2%, the results are shown in Table 22.
22 Precision test result
(4) the text method is pressed in repeatability test, gets 5 parts of same batch samples, and every part is measured, and tries to achieve relative standard deviation＜2%, the results are shown in Table 23.
Table 23 reproducible test results
(5) the recovery test precision takes by weighing same batch sample 10g, puts in the separatory funnel, after adding entry 10ml dilution and disperseing, accurate magnelin reference substance solution (0.65mg/ml) 1ml that adds, the jog mixing adds ethyl acetate extraction 5 times, each 50ml collects extracting solution, water bath method, residue adds dissolve with methanol, puts in the 25ml volumetric flask, is settled to scale, shake up, filter, get subsequent filtrate, measure its content, and calculate its response rate, measurement result sees Table 24:
Table 24 recovery test result
From above result of the test as can be seen, its linear relationship of content assaying method of the present invention, stability, precision, repeatability, the response rate are all good, can effectively control the content of lignanoid in the present composition.
Embodiment 1
Fructus Xanthii 1664g Flos Magnoliae 312g Flos Chrysanthemi Indici 104g
Flos Lonicerae 104g Radix Rubiae 104g
The preparation method of said preparation is:
Above five tastes medical material is got Flos Magnoliae and Flos Chrysanthemi Indici and is added 12 times of water gaging distillations extraction in 5 hours volatile oil, and the aqueous solution after distillation device is in addition collected; Fructus Xanthii extracting in water twice, 2 hours for the first time, amount of water was 8 times, and 1 hour for the second time, amount of water was 6 times, and collecting decoction filters, and filtrate is left standstill; Flos Lonicerae adds water in 70～80 ℃ of warm macerating secondaries, 2 hours for the first time, amount of water is 10 times, and 1 hour for the second time, amount of water was 8 times, merge immersion, filter, filtrate is left standstill, and merges above-mentioned two kinds of clarification medicinal liquids and Flos Magnoliae and Flos Chrysanthemi Indici aqueous solution, in temperature is 70 ℃, and pressure is 1.20 extractum for concentrating under reduced pressure under the-0.06Mpa condition becomes relative density; Other gets Radix Rubiae and is ground into coarse powder, makes solvent with 8 times of amount 70% alcohol, floods after 48 hours, with the speed percolation of 5ml/min*kg, collect the liquid of filtering, reclaim ethanol, relative density is 1.02 extractum when being concentrated into 60 ℃, leaves standstill, and gets supernatant and above-mentioned concentrated solution and merges, leave standstill, filter, filtrate is 70 ℃ in temperature, pressure is-the 0.06Mpa condition under concentrating under reduced pressure, being concentrated into relative density is 1.25～1.30, adds sucrose 800g and potassium sorbate 1.67g, boils dissolving, filter, put coldly, add volatile oil such as above-mentioned Flos Magnoliae, add water to 1000ml, stir evenly, fill, 105 ℃, flowing steam sterilization 30min promptly.
Embodiment 2-10
In test agent in 9 batches of the identical method of embodiment 1 and the preparations of prescription ratio.
The method of quality control of preparation of the present invention:
(1) get embodiment 1-10 preparation 50ml respectively, extract 4 times with the chloroform jolting, each 30ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.
Extracting honeysuckle control medicinal material 1g adds chloroform 10ml supersound process 30 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution.
Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (5: 1) is developing solvent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue spot.
(2) qualitative detection of Radix Rubiae
Get embodiment 1-10 preparation 50ml respectively, extract 4 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.
Other gets Radix Rubiae control medicinal material 1g, adds ethyl acetate 10ml supersound process 30 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution.
Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether-acetone (10: 0.5) 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 identical yellow green speckle.
(3) detection by quantitative of magnelin
With the octadecylsilane chemically bonded silica is filler; With acetonitrile-water-oxolane (38: 61: 1) is mobile phase; The detection wavelength is 278nm.Number of theoretical plate calculates by the magnelin peak should be not less than 2000.
It is an amount of to get the magnelin reference substance, accurate claims surely, makes the solution that every 1ml contains 65 μ g with dissolve with methanol, product solution in contrast, promptly.
Precision takes by weighing embodiment 1-10 preparation 20g, puts in the separatory funnel, adds water 20ml dilution and disperses, and adds ethyl acetate extraction 5 times, each 50ml, collect extracting solution, water bath method, residue adds dissolve with methanol, puts in the 25ml volumetric flask, is settled to scale, shake up, filter, get subsequent filtrate, promptly.Accurate respectively reference substance solution 5 μ l, the need testing solution 10 μ l of drawing inject chromatograph of liquid, measure, promptly.
The magnelin assay result of table 25 embodiment 1-10
In addition, also ratio and the preparation technology with the prescription crude drug made the negative sample that does not contain Flos Lonicerae, Radix Rubiae, prepared negative control solution according to the preparation method for test agent in the method for quality control, on silica gel g thin-layer plate, speckle does not appear in described 2 kinds of negative samples on the relevant position, through repetition test, this method of quality control specificity, good reproducibility can be used as the qualitative checking method that this quality of the pharmaceutical preparations is controlled.
Claims (1)
1. a detection method for the treatment of the Chinese medicine preparation of rhinitis is characterized in that this method comprises the steps:
Said preparation is made by the crude drug of following weight ratio:
Fructus Xanthii 1664g Flos Magnoliae 312g Flos Chrysanthemi Indici 104g
Flos Lonicerae 104g Radix Rubiae 104g;
The preparation method of said preparation is:
Above five tastes medical material is got Flos Magnoliae and Flos Chrysanthemi Indici and is added 12 times of water gaging distillations extraction in 5 hours volatile oil, and the aqueous solution after distillation device is in addition collected; Fructus Xanthii extracting in water twice, 2 hours for the first time, amount of water was 8 times, and 1 hour for the second time, amount of water was 6 times, and collecting decoction filters, and filtrate is left standstill; Flos Lonicerae adds water in 70～80 ℃ of warm macerating secondaries, 2 hours for the first time, amount of water is 10 times, and 1 hour for the second time, amount of water was 8 times, merge immersion, filter, filtrate is left standstill, and merges above-mentioned two kinds of clarification medicinal liquids and Flos Magnoliae and Flos Chrysanthemi Indici aqueous solution, in temperature is 70 ℃, and pressure is 1.20 extractum for concentrating under reduced pressure under the-0.06Mpa condition becomes relative density; Other gets Radix Rubiae and is ground into coarse powder, makes solvent with 8 times of amount 70% ethanol, floods after 48 hours, with the speed percolation of 5ml/min*kg, collect the liquid of filtering, reclaim ethanol, relative density is 1.02 extractum when being concentrated into 60 ℃, leaves standstill, and gets supernatant and above-mentioned concentrated solution and merges, leave standstill, filter, filtrate is 70 ℃ in temperature, pressure is-the 0.06Mpa condition under concentrating under reduced pressure, being concentrated into relative density is 1.25～1.30, add sucrose 800g and potassium sorbate 1.67g, boil dissolving, filter, put cold, add volatile oil such as above-mentioned Flos Magnoliae, add water to 1000ml, stir evenly, fill, 105 ℃ of flowing steam sterilization 30min are promptly;
The detection method of said preparation comprises following a, b, three kinds of detection methods of c:
A. the qualitative detection of Flos Lonicerae
Get this preparation 50ml, extract 4 times with the chloroform jolting, each 30ml, combined chloroform liquid, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution;
Extracting honeysuckle control medicinal material 1g adds chloroform 10ml supersound process 30 minutes in addition, filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, in contrast medical material solution;
Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, petroleum ether-acetone with 5: 1 ratios is developing solvent, launch, take out, dry, spray is with 5% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue spot;
B. the qualitative detection of Radix Rubiae
Get this preparation 50ml, extract 4 times with the ethyl acetate jolting, each 30ml, combined ethyl acetate liquid, evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution;
Other gets Radix Rubiae control medicinal material 1g, adds ethyl acetate 10ml supersound process 30 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, in contrast medical material solution;
Test according to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin layer chromatography, draw each 5～10 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, petroleum ether-acetone with 10: 0.5 ratios is developing solvent, launch, take out, dry, putting wavelength is to inspect under the 365nm uviol lamp; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical yellow green speckle;
C. the detection by quantitative of magnelin
With the octadecylsilane chemically bonded silica is filler; Acetonitrile-water-oxolane mixed solution with 38: 61: 1 ratios is a mobile phase; The detection wavelength is 278nm; Number of theoretical plate calculates by the magnelin peak should be not less than 2000;
It is an amount of to get the magnelin reference substance, accurate claims surely, makes the solution that every 1ml contains 65 μ g with dissolve with methanol, product solution in contrast, promptly;
Precision takes by weighing this preparation 20g, puts in the separatory funnel, adds water 20ml dilution and disperses, and adds ethyl acetate extraction 5 times, each 50ml, collect extracting solution, water bath method, residue adds dissolve with methanol, puts in the 25ml volumetric flask, is settled to scale, shake up, filter, get subsequent filtrate, promptly; Accurate respectively reference substance solution 5 μ l, the need testing solution 10 μ l of drawing inject chromatograph of liquid, measure, promptly;
The every 1g of this preparation contains Flos Magnoliae in the magnelin amount, must not be less than 50 μ g.
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| CN103690641A (en) * | 2012-09-27 | 2014-04-02 | 张献奎 | A traditional Chinese medicine used for treating rhinitis |
| CN104510875A (en) * | 2015-01-16 | 2015-04-15 | 青岛市市立医院 | Method for preparing traditional Chinese preparation for treating acute and chronic rhinitis |
| CN106728146A (en) * | 2017-02-13 | 2017-05-31 | 佛山市腾瑞医药科技有限公司 | A kind of Chinese medicine for treating rhinitis composition and preparation method thereof |
| CN111089930B (en) * | 2019-11-20 | 2022-04-12 | 广东一方制药有限公司 | Method for constructing UPLC characteristic spectrum of magnolia flower formula granules and determination of component content of magnolia flower formula granules |
| CN114755361B (en) * | 2022-04-24 | 2024-03-08 | 江苏省中医院 | Quality detection method of traditional Chinese medicine compound composition for treating allergic rhinitis of children |
| CN118021897B (en) * | 2024-04-12 | 2024-06-11 | 山东新时代药业有限公司 | Pharmaceutical composition and application thereof in medicines for treating coronary heart disease |
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