CN102228505B - Chinese medicinal composition with effects of nourishing heart and tranquilizing mind and preparation method and detection method thereof - Google Patents
Chinese medicinal composition with effects of nourishing heart and tranquilizing mind and preparation method and detection method thereof Download PDFInfo
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Abstract
The invention relates to a Chinese medicinal composition with effects of nourishing heart and tranquilizing mind, a preparation method and a quality control method thereof. The Chinese medicinal composition consists of raw medicines such as pearl stratum powder, lucid ganoderma, liquorice root and the like. Clinically acceptable formulations such as granules, capsules, tablets, a mixture and the like can be prepared by adding excipients by the conventional process. By the quality control method for the Chinese medicinal composition, the pearl stratum powder, the lucid ganoderma and the liquorice root are detected, so that the therapeutic effect of the medicine is ensured. The medicine has the effects of nourishing heart and tranquilizing mind, and has remarkable effects when used for treating diseases such as cardiopalmus, insomnia and the like.
Description
The present invention is for dividing an application, and the original bill application number is 200710179528.x, and the original bill applying date is on Dec 14th, 2007, and the original bill name is called Chinese medicine composition of a kind of mental-tranquilization and preparation method thereof and method of quality control.
Technical field
The present invention relates to a kind of Chinese drug-treated group and thing and preparation method thereof and method of quality control of mental-tranquilization, belong to technical field of traditional Chinese medicines.
Background technology
Insomnia be meant dyscoimesis, early awakening or wake up after difficult more sleeping, severe patient is lain awake all night, and makes that the people unsets, fatigue and weak, even the symptoms such as dreaminess, failure of memory that cause having a headache.Insomnia generally need be taken medicine as stubborn disease for a long time, but take some Western medicine such as barbiturates for a long time, Benzodiazepines can produce severe dependency.Some mental-tranquilization Chinese patent drugs are taken for a long time simultaneously; Can bring harm to human body, for example take Tianwang Buxin Dan, zhusha anshen pills, Angong Niuhuang Wan etc. for a long time, meeting accumulated because of contained cinnabar in the prescription and chronic mercury poisoning occurred; Cinnabar can cause fetal anomaly simultaneously, and the pregnant woman can not take.Be also noted that incompatibility, cinnabar is prone to generate methyl mercury with the medicine (like theophylline, inderal etc.) that contains methyl structural, causes mercury poisoning; Cinnabar and bromide, iodide share, and can generate mercuric bromide or mercuric iodixde deposition with toxicity, cause medicine source enteritis.Then there is not science of quality control in the relevant Chinese medicine of other, the unsettled situation of curative effect.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine composition of mental-tranquilization;
The object of the invention also is to provide a kind of preparation method of Chinese medicine composition of mental-tranquilization;
The object of the invention also is to provide a kind of method of quality control of Chinese medicine composition of mental-tranquilization.
The present invention seeks to realize through following technical scheme:
The Chinese medicine composition of mental-tranquilization of the present invention is to be processed by the bulk drug of following weight ratio:
Nacreous layer powder 100-200 weight portion, glossy ganoderma 500-800 weight portion, Radix Glycyrrhizae 100-200 weight portion;
The Chinese medicine composition of mental-tranquilization of the present invention is to be processed by the bulk drug of following weight ratio:
Nacreous layer powder 100 weight portions, glossy ganoderma 800 weight portions, Radix Glycyrrhizae 100 weight portions;
The Chinese medicine composition of mental-tranquilization of the present invention is to be processed by the bulk drug of following weight ratio:
Nacreous layer powder 200 weight portions, glossy ganoderma 500 weight portions, Radix Glycyrrhizae 200 weight portions;
The Chinese medicine composition of mental-tranquilization of the present invention is to be processed by the bulk drug of following weight ratio:
Nacreous layer powder 150 weight portions, glossy ganoderma 600 weight portions, Radix Glycyrrhizae 150 weight portions;
The Chinese medicine composition of mental-tranquilization of the present invention is to be processed by the bulk drug of following weight ratio:
Nacreous layer powder 150 weight portions, red sesame 600 weight portions, Radix Glycyrrhizae 150 weight portions, wilsonii 100 weight portions.
The preparation method of Chinese medicine composition of the present invention is:
Above flavour of a drug remove nacreous layer powder and add water and extract secondary, add 12 times of water gagings, extract filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of water gagings, extract 3 hours, filter merging filtrate; Filter, leave standstill, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃); Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder, and fine powder and above-mentioned clear cream mixing add auxiliary material and process the various conventional formulations in this area, as: granule, capsule, tablet, mixture promptly get;
The piece preparation method of Chinese medicine composition of the present invention is:
Above flavour of a drug, the flavour of a drug extracting in water secondary except that nacreous layer powder adds 12 times of water gagings of water the 1st time, extracts 3 hours, filters; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter merging filtrate; Filter, leave standstill, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃); Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder; Fine powder and above-mentioned clear cream mixing add the granulation of 25% starch, drying, add 0.5% dolomol compressing tablet, the bag film-coating; Dressing machine EAT is 40 ℃, and hydrojet speed is 120g/min, selects 8 rev/mins speed when the coating pan rotating speed begins for use; Along with of the continuous formation of film-coating layer on plain sheet surface, progressively increase rotating speed again, be 40 rev/mins up to rotating speed; After hydrojet finishes, with 60 ℃ of heated-air drying 25min; Promptly get.
The method of quality control of Chinese medicine composition of the present invention comprises one or more in following discriminating and/or the content assaying method:
[discriminating]:
Get preparation of the present invention and be equivalent to raw medicinal herbs 5.0-10.0g, put in the conical flask, add water 30-70ml, ultrasonic 10-30 minute (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101); With 5-20% ethanolic solution 80-120ml wash-out, discard eluent, add 60-80% methanol solution 30-70ml wash-out then, collect eluent; Water bath method, residue add normal butyl alcohol 20ml makes dissolving, extracts three times with the ammonia solution jolting, for the first time 10-30ml; The each 5-15ml of second and third time merges ammonia solution, extracts 1-3 time with the normal butyl alcohol jolting after adding hcl acidifying, at every turn 10-30ml; Merge normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 10-30 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; (10-15: 5-10: lower floor's solution 1-3) is developping agent, launches, and takes out with methenyl choloride one methanol-water; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 5-15 minute, and inspected under the daylight; In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 10.0-20.0g, and precision takes by weighing 1.0-3.0g, puts in the 10ml tool plug centrifuge tube adding distil water 3-10ml; The jolting dissolving centrifugal 5-15 minute, is left standstill; Discard upper solution, and then add 3-8ml distilled water, like method operation 2-5 time; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 5-15ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get;
The accurate need testing solution 15-40ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with the Calcium Disodium Versenate vs titration of 0.05mol/L, becomes blueness by redness to solution; The Calcium Disodium Versenate vs of every 1ml0.05mol/L is equivalent to the Ca of 2.004mg;
Preparation of the present invention is equivalent to raw medicinal herbs 0.7g, contains nacreous layer powder in Ca, must not be less than 40-80mg.
The method of quality control of Chinese medicine composition of the present invention comprises one or more in following discriminating and/or the content assaying method:
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight; In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get;
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution; The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg;
Preparation of the present invention is equivalent to raw medicinal herbs 0.7g, contains nacreous layer powder in Ca, must not be less than 60mg.
Prescription science of the present invention, but the Chinese crude drug of the medicine-food two-purpose of selected safety non-toxic is taken safer as bulk drug; The consumption proportion of each flavour of a drug has carried out optimizing screening through pharmacological evaluation in the prescription; And the preparation technology in conjunction with writing out a prescription to this Chinese medicine composition has carried out optimizing screening; In addition the quality of prescription has been carried out multi-level control; This control method is verified, made the present invention show stable higher curative effect.
Embodiment
Following experimental example and embodiment further specify but are not limited to the present invention down
The optimization experiment of experimental example 1. Chinese medicine composition preparation process conditions of the present invention and technical parameter
(1), technical study
1, extraction process is investigated:
The method for distilling that licorice medicinal materials is commonly used has water extraction, alcohol extracting method etc., learns that through experiment the principal element that in water extraction, influences extraction efficiency is a solvent volume, secondly is the pH value of extraction time and solution.The method for distilling of glossy ganoderma has alcohol extracting method and water extraction, and is wherein the highest with the water extraction polyoses content, higher about 5 times than the polyoses content of 70% alcohol extract.Experimentize in view of the above: draft 18 times, 22 times and 26 times of water respectively and extract, to confirm the The suitable solvent volume.In addition, the degree of grinding of medicinal material also has certain influence to extraction efficiency, directly extracts but extract the normal medicine materical crude slice that adopts in view of big production, therefore the pulverizing medicinal materials degree is not investigated in addition.
Method for distilling: take by weighing glossy ganoderma, Radix Glycyrrhizae, wilsonii raw medicinal material in embodiment 4 prescription ratios, mix, add the deionized water of ormal weight, decoct secondary; Each 3 hours, collecting decoction filtered, and placed; Get supernatant, concentrate drying is according to the amount calculated yield of dried cream.The result sees table 1:
Table 1 extraction process is investigated
The result shows: second group of paste-forming rate with the 3rd group is almost suitable, and second group more saves time, more practices thrift, and therefore adopts 22 times of amount solvents, extracts at twice; Add 12 times of amounts of water for the 1st time, extracted 3 hours, filter, the dregs of a decoction add 10 times of amounts of water; Extracted 3 hours, and filtered, merging filtrate, subsequent use.Therefore actual production adopts 22 times of amount solvents to extract.
2, concentration technology is investigated:
After the granulating process of this tablet adopts medicinal extract is concentrated to certain relative density, directly add nacreous layer powder, starch is granulated, and therefore needs to investigate the relative density that extract concentrates.Press embodiment 4 recipe quantities configurations Radix Glycyrrhizae, glossy ganoderma, wilsonii medicinal material, divide three groups to make an experiment by the method for making item, amount of water is 22 times of amounts, and extract is concentrated into following relative density respectively, is index with the wet granulation difficulty, the relative density after confirming to concentrate.The result sees table 2:
The investigation of table 2 relative density
Finally selecting relative density according to above test findings is 1.28～1.30 (70 ℃-80 ℃).
3, Study on Forming:
Because nacreous layer powder is the raw material that directly is used as medicine, so the granularity of nacreous layer powder has very big influence for the quality of preparation.The design that experimentizes in view of the above selects 100 orders, 200 orders, 300 purpose nacreous layer powders to carry out the research of moulding process.
Get the nacreous layer powder 50g of different meshes, add starch 21.5g respectively, mix, add 75g medicinal extract, be prepared into particle, compressing tablet is measured disintegration time limited.The result sees table 3:
The investigation of table 3 moulding process
The result shows: adopt the nacreous layer powder of the above smashing fineness of 200 orders, institute's tablet agent outward appearance is khaki, and is smooth, the even immaculate of color and luster, and little sweet, granular sensation is few, and disintegration is rapid.So select for use the above nacreous layer powder of 200 orders to prepare tablet.
4, the selection of dolomol consumption:
Know that the flowability of particle is poor in the process of screening nacreous layer powder granularity; Cause tablet weight variation big, need to add lubricant, according to conventional amount used; Add 0.3%, 0.5%, 1.0% dolomol respectively, with difficulty or ease, tablet weight variation and disintegration time limited of compressing tablet be the consumption that index is investigated dolomol.The result sees table 4:
The investigation of table 4 dolomol consumption
The result shows: when the dolomol consumption was 0.5%, mobility of particle can reach the requirement of compressing tablet, and that processes is unilateral smooth, and disintegration time limited is qualified.So select dolomol consumption 0.5% to be used for producing.
5, art for coating research:
In order to protect these article not receive the influence of effects such as humidity, oxidation, the stability of raising medicine is intended these article bag film-coating.Because the bag film-coating is with short production cycle, easy and simple to handle, rate of drying is fast, and medicine receives damp and hotly to influence for a short time, helps improving the quality of products.
5.1 test material: stomach dissolution type coating powder, 95% ethanol, purified water.
5.2 dressing is write out a prescription basically: stomach dissolution type coating powder, 95% ethanol, purified water, the plain sheet of tablet of the present invention.
5.3 coating solution preparation:
After the accurate weighing of stomach dissolution type coating powder, it is an amount of to add 95% ethanol, stirs half an hour, and adding purified water, to be made into concentration of alcohol be 80%, and coating solution concentration is 8% dressing solution, continues to stir to shake up, and treats that coating solution dissolves fully, promptly gets.
5.4 the screening of dressing process operation parameter
Unilateral smooth, fine and smooth key is the relation between GPRS pot temperature, discharge rate, the rotating speed three in the whole process, and this is the most important thing in the film coating operating process.If temperature is too high, then drying is too fast, and film forming is coarse easily, and the sheet look uneven; If temperature is low excessively, or spray speed is too fast, then can make pot interior excess moisture high, the phenomenons such as adhesion of sheet will soon occur.In order to address the above problem, down in the face of influencing several key process parameters of dressing: EAT, the hydrojet speed and the coating pan rotating speed of spray gun are optimized combination.Outward appearance, tablet weight variation, disintegration time limited with slice, thin piece are index.Designed three kinds of conditions altogether, seen table 5 investigating finished product outward appearance, tablet weight variation and disintegration time limited behind its dressing combination:
Table 5 coating conditions combination table
Three kinds of combinations according to above-mentioned table 5 make an experiment, and the coating conditions The selection result sees the following form 6:
Table 6 coating conditions is investigated the result
Experiment shows: dressing machine EAT is 40 ℃, and hydrojet speed is 120g/min, selects 8 rev/mins speed when the coating pan rotating speed begins for use, along with the continuous formation of film-coating layer on plain sheet surface, progressively increases rotating speed again, is 40 rev/mins up to rotating speed.After hydrojet finished, with heated-air drying 25 minutes, each item index was all more qualified.
Thin layer to Radix Glycyrrhizae in experimental example 2. pharmaceutical preparations of the present invention is differentiated
The investigation of reflux extracting time when (1) need testing solution prepares
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic filtration, the macroporous adsorptive resins of filtrating (internal diameter 1.5cm; Long 15cm D101), with 10% ethanolic solution 100ml wash-out, discards eluent, adds 70% methanol solution 50ml wash-out then; Collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving, extracts three times with the ammonia solution jolting, for the first time 20ml; The each 10ml of second and third time merges ammonia solution, extracts 2 times each 20ml with the normal butyl alcohol jolting after adding hcl acidifying; Merge normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry, spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes; Inspect the color developing effect of test sample and reference substance under the daylight, the result sees the following form:
The color developing effect of table 7 different extraction times
Can find out refluxing extraction 20min, the equal Pass Test requirement of the need testing solution of extraction and reference substance solution from last table.
(2) thin layer of Radix Glycyrrhizae is differentiated the preferred of developping agent proportioning in the above-mentioned discrimination method:
Draw each 20 μ l of need testing solution, reference substance solution respectively, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose, the upper solution that was respectively 23: 5: 1,18: 6: 1,13: 7: 2,8: 8: 2 with methenyl choloride-methanol-water is a developping agent; Launch; Take out, dry, spray is with 5% ethanol solution of sulfuric acid; 105 ℃ were heated 10 minutes, and inspected under the daylight.In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
Developping agent proportion optimization experimental result table in the discrimination method of table 8. Radix Glycyrrhizae
Can find out that from last table the developping agent proportioning is at 13: 7: 2 o'clock, on thin layer plate, launch effectively that principal spot is clear, does not have hangover, and is identical with the speckle displacement and the color of reference substance, is fit to testing requirements.
(3) sample solution point sample amount preferred in the above-mentioned Radix Glycyrrhizae discrimination method:
Drawing need testing solution 2 μ l, 10 μ l, 20 μ l, 30 μ l points on same silica gel g thin-layer plate, is developping agent with methenyl choloride-methanol-water (13: 7: 2), launches; Take out, dry, spray is with 5% ethanol solution of sulfuric acid; 105 ℃ were heated 10 minutes; Inspect under the daylight, observe the effect of test sample principal spot colour developing on the thin layer plate, the result sees the following form:
Sample solution point sample amount optimization experiment table as a result in the discrimination method of table 9. Radix Glycyrrhizae
Can find out test sample point sample amount when the 20 μ l from last table, color developing effect is good on thin layer plate, is fit to testing requirements.
(4) negative control test
Get the negative sample that lacks Radix Glycyrrhizae, prepare negative control solution, launch the back and corresponding spot on the reference substance solution correspondence position, do not occur, explain that selected identification experiment specificity is strong according to test sample sample in the discrimination method of above-mentioned Radix Glycyrrhizae and solution manufacturing method.
The screening of experimental example 3. content assaying methods
For improving the quality standard of preparation, we measure the content of the monarch drug in a prescription nacreous layer powder in the prescription, to improve the controllability of its quality.
1. reagent and reagent
Plum Teller electronic analytical balance hydrochloric acid: AR Beijing Chemical Plant
NaOH: AR Beijing Chemical Plant lime carbonate: AR Beijing Chemical Plant
2. the foundation of method
The preparation of need testing solution: get 20 in tablet of the present invention, remove film-coating, porphyrize, precision takes by weighing 1.5g; Put in the 10ml tool plug centrifuge tube adding distil water 5ml, jolting dissolving, centrifugal 10 minutes; Leave standstill, discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The preparation of reference substance solution: get the about 0.5g of lime carbonate, the accurate title, decide, and puts in the 100ml volumetric flask, adds watery hydrochloric acid to lime carbonate and all dissolve, and is diluted to scale with new boiled-out water, promptly gets.
2.1 negative control test
Get other medicinal material that lacks outside the nacreous layer powder medicinal material and become negative sample according to prepared, the preparation method according to need testing solution is prepared into negative sample solution again, measures with method.Feminine gender is not disturbed assay as a result.
2.2 precision test
Get need testing solution, replicate determination 5 times, the result sees table 10:
Table 10 Precision test result
The result shows: get with a need testing solution, 5 parts of METHOD FOR CONTINUOUS DETERMINATION, its average external volume are 13.9ml, and calculating the RSD value is 0.65%, and this method precision meets the requirements.
2.3 stability test
Get 6 parts of above-mentioned need testing solutions, respectively at 0,1,2,4,6,8 hour mensuration, investigation method stability, the result sees table 11:
Table 11. stability test result
The result shows: get with a need testing solution, respectively at titration in 0,1,2,4,6,8 hour, its average external volume was 13.8ml, and calculating the RSD value is 0.82%, and this need testing solution is basicly stable in 8 hours.
2.4 reappearance test
Get totally 5 parts in same lot number sample, prepare need testing solution and measure by the text method, calculate content, the result sees table 12:
Table 12. reproducible test results
Through calculating reappearance test RSD value is 1.39%, meets the requirements.
2.5 average recovery test
It is an amount of that precision takes by weighing the sample of known content, and the accurate again lime carbonate fine powder that adds known purity mixes, and measures calculate recovery rate by the text method.The result sees table 13:
Table 13. average recovery is measured the result
Get the average recovery that the known content sample carries out 0.5 times, 1 times and 1.5 times respectively and measure, the recovery is between 95.34～100.23%, and its average recovery rate is 98.01%, meets the requirements.
The assay result of table 14. three lot sample article sees the following form:
Can find out that by above methodology examination result its linear relationship of the content assaying method that medicine of the present invention adopted, stability, precision, reappearance etc. are all good, can effectively control drug quality of the present invention.
Tentative every of these article contain nacreous layer powder in Ca, must not be less than 60mg.
Experimental example 4. pharmacodynamic experiments
1 material
1.1 medicine:
Chinese medicine composition I of the present invention processes according to embodiment 3 methods;
Chinese medicine composition II of the present invention processes according to embodiment 4 methods;
The accurate word Z31020265 of Zhengheling tablet Shanghai Leiyun Pharmaceutical Industry Co., Ltd. traditional Chinese medicines
1.2 animal
Kunming mouse, rat, above animal male and female dual-purpose, body weight is seen after and is stated, and is provided by China Academy of TCM's Experimental Animal Center.
1.3 instrument
WT/1001 type electronic balance, Jiangsu ten thousand gets balance equipment factory.
WFZ800--D3B type ultraviolet-visible pectrophotometer, the Beijing Rayleigh Analytical Instrument Co.,Ltd.
FJ one 2021 type radio-immunity counters, Plant No. 262.
LDZ4-O8 hydro-extractor: Beijing Medical Centrifugal Machine Factory.
The KENZ-ECG electrocardiograph, Japan can anti-company.
2. method and result
2.1 to mouse normal pressure hypoxia endurance test
Get 60 of Kunming mouses, male and female half and half, body weight (20 ± 2) g is divided into 4 groups at random; The difference gastric infusion, physiological saline group, small capital invention Chinese medicine composition group, Zhengheling tablet group, the administration volume is all 0.2mL/10g; Dosage is equivalent to 10 times of people's consumption respectively, behind the administration 30Min, mouse is put into the airtight wide-necked bottle of same volume (250mL) respectively; Adorn soda lime 20g respectively in the bottle, be lined with filter paper on the soda lime, bottleneck is coated with vaseline; Put into behind the mouse and to pick up counting bottle is airtight, examine dead mouse, the record death time.Test findings is seen table 15.
The influence of the table 15. pair anti-anoxic of mouse normal pressure (X ± S)
Annotate: compare △ P＜0.05, △ △ P＜0.01 with the Zhengheling tablet group; Compare * P＜0.05, * * P＜0.01 with the physiological saline group
Test shows that under the clinical equivalent amount, Chinese medicine composition of the present invention is than the Zhengheling tablet significant prolongation anoxia in mice death time, and Chinese medicine composition II of the present invention is superior to Chinese medicine composition I of the present invention.
2.2 resisting myocardial ischemia property test
Get 40 of rats, male and female half and half, body weight (250 ± 20) g, random packet: physiological saline group, Chinese medicine composition of the present invention, Zhengheling tablet; Fixing under waking state, record II lead electrocardiogram is measured the normal II electrograph that leads, successive administration 7 days before the medicine; 30min after the administration in the 8th day, every rat is anaesthetized with urethane, and measures the rat cardiogram; The cardiogram of contrast rat this moment is the normal cardiogram of rat with changing little person before the medicine, claims back sublingual vein injection of pituitrin 0.2u/kg; Finish in the 10s injection, the cardiogram of record injection back 1min, 5min is judged the rat heart ischemia.Cardiogram criterion: positive criterion (cardiac muscle is ischemic obviously): ST section horizontal-shift, skew＞0.mV up or down; The T wave height is alarmmed, and surpasses with leading 1/2 of R ripple; The T wave height is alarmmed and is shifted with the ST section.Negative criterion (myocardial ischemia is not obvious): the oblique skew of ST section, or horizontal-shift＜0.1mV; The T ripple is low or two-way, inversion＜0.1mV.Height with ST field offset baseline is an index.Through the mV number average value of the summation (∑ ST) of every group of ST field offset baseline height index as the treating myocardial ischemia damage degree.The result sees table 16.
The test of table 16 resisting myocardial ischemia property
Annotate: through X
2Check is compared △ P＜0.05, △ △ P＜0.01 with the Zhengheling tablet group; Compare with the physiological saline group; * P＜0.05; * P＜0.01 resisting myocardial ischemia test shows that Chinese medicine composition of the present invention can obviously reduce rat heart muscle ischemic animal number, significantly improves the degree of rat heart muscle ischemic, and Chinese medicine composition II of the present invention is superior to Chinese medicine composition I of the present invention.
2.3 tranquilizing effect
Get 60 of Kunming mouses, body weight 18-22g, the male and female dual-purpose is divided into 4 groups at random, 15 every group.Physiological saline control group (control group): give physiological saline 0.2ml/10g and irritate stomach, every day 1 time, totally 3 days.Chinese medicinal composition preparation I of the present invention group, Chinese medicinal composition preparation II of the present invention group: get the particulate samples liquid 0.2ml/10g of the present invention for preparing and irritate stomach (be equivalent to people's consumption 9 times), every day 1 time, totally 3 days.Each is organized last and irritates 1h behind the stomach, after mouse is put into the spontaneous activity appearance and adapts to 3 minutes, begins to measure the spontaneous activity number of times and sleep surpasses 2 hours the length of one's sleep.The result sees the following form:
Table 17. pair spontaneous activity in mice number of times and the influence of the length of one's sleep
| Group | Dosage (g/kg) | The spontaneous activity number of times | The length of one's sleep (min) |
| The blank group | - | 168.6±64.2 | 41.0±15.6 |
| Zhengheling tablet | 0.5 | 127.47±27.76* | 54.4±32.4* |
| Chinese medicine composition I of the present invention | 0.5 | 103.5±56.3* | 64.4±24.6*※ |
| Chinese medicine composition II of the present invention | 0.5 | 81.8±35.3** | 86.4±23.7**※※ |
Annotate: compare with control group, * P＜0.05, ※ P＜0.05, ※ ※ P＜0.01 are compared with Zhengheling tablet in * * P＜0.01
It is remarkable that pharmaceutical composition of the present invention and beautiful Zhengheling tablet are compared tranquilizing effect, and Chinese medicine composition II of the present invention is superior to Chinese medicine composition I of the present invention.
2.4 influence to learning and memory of little mouse
50 of mouse are got in influence to learning and memory of little mouse, are divided into 5 groups at random, Chinese medicine composition I of the present invention, II, Zhengheling tablet group according to the form below dosage ig relative medicine solution; Control group gives equal-volume water, every day 1 time, 50min after the administration of 7d last continuously; Except that control group; Give ip in mice anisodine 10mg/kg, administration 1 time, all animals is done diving tower and passive avoidance response experiment behind the 10min.During experiment animal is placed on the diving tower, is shocked by electricity when animal skips on the electrical network, the normal reaction of animal is on the rebound diving tower. so after the training once; Mouse is put down gently on platform, in the latent period (SDL) that the record mouse stops, treat that mouse jumps off from platform on platform; When four limbs all contact electrical network, give electro photoluminescence immediately, on mouse rebound platform; The record mouse jumps off the latent period (EL) that receives to escape after the electro photoluminescence to the platform from platform, and with SDL and the index of EL as the judgement learning ability of mice, SDL is more little; EL is big more, just explains that the study acquisition of mouse is poor more, and the result sees table 18.
The experiment measuring value of each group of table 18
Compare ※ P＜0.05, ※ ※ P＜0.01 with the anisodine group; Compare * P＜0.05, * * P＜0.01 with the Zhengheling tablet group
Pharmaceutical composition of the present invention has been compared with Zhengheling tablet and has been strengthened the learning and memory effect, and Chinese medicine composition II of the present invention is superior to Chinese medicine composition I of the present invention.
Following embodiment all can realize the described effect of above-mentioned experimental example
Embodiment 1.
Nacreous layer powder 100g, glossy ganoderma 800g, Radix Glycyrrhizae 100g
More than three flavors, two flavor extracting in water secondaries except that nacreous layer powder add 12 times of water gagings of water, extracted filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter merging filtrate; Filter, place, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃).Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder, and fine powder and above-mentioned clear cream mixing add auxiliary material and process the various conventional formulations in this area, as: granule, capsule, tablet, soft capsule, mixture promptly get.
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition; According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight; In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg.
These article preparation is equivalent to raw medicinal herbs 0.7g, and nacreous layer powder must not be less than 60mg in Ca.
Embodiment 2. capsules
Nacreous layer powder 200g, glossy ganoderma 500g, Radix Glycyrrhizae 200g
More than three flavors, two flavor extracting in water secondaries except that nacreous layer powder add 12 times of water gagings of water, extracted filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter merging filtrate; Filter, place, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃).Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder, and fine powder and above-mentioned clear cream mixing add starch 100g granulation, encapsulated, get 1000 of capsules, promptly get.
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight; In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg.
These article preparation is equivalent to raw medicinal herbs 0.7g, contains nacreous layer powder in Ca, must not be less than 60mg.
Embodiment 3. granules
Nacreous layer powder 150g, glossy ganoderma 600g, Radix Glycyrrhizae 150g
More than three flavors, two flavor extracting in water secondaries except that nacreous layer powder add 12 times of water gagings of water, extracted filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter merging filtrate; Filter, place, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃).Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder, and fine powder and above-mentioned clear cream mixing add Icing Sugar 300g and granulate, and get particle 700g, promptly get.
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight.In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg.
These article preparation is equivalent to raw medicinal herbs 0.7g, and nacreous layer powder must not be less than 60mg in Ca.
Embodiment 4. granules
Nacreous layer powder 150g, red sesame 600g, Radix Glycyrrhizae 150g, wilsonii 100g
More than four flavors, three flavor extracting in water secondaries except that nacreous layer powder add 12 times of water gagings of water, extracted filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter merging filtrate; Filter, place, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃).Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder, and fine powder and above-mentioned clear cream mixing add Icing Sugar 360g and granulate, and get particle 800g, promptly get.
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight.In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg.
These article preparation is equivalent to raw medicinal herbs 0.7g, and nacreous layer powder must not be less than 60mg in Ca.
Embodiment 5. tablets
Nacreous layer powder 150g, glossy ganoderma 600g, Radix Glycyrrhizae 150g
More than three flavors, two flavor extracting in water secondaries except that nacreous layer powder add 12 times of water gagings of water, extracted filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter merging filtrate; Filter, place, get supernatant, being concentrated into relative density is the clear cream of 1.28～1.30 (70～80 ℃).Get nacreous layer powder and pulverize, sieve, the sieve aperture internal diameter is 75 μ m ± 4.1 μ m, gets fine powder; Fine powder and above-mentioned clear cream mixing add the granulation of 25% starch, drying, add 0.5% dolomol compressing tablet, the bag film-coating; Dressing machine EAT is 40 ℃, and hydrojet speed is 120g/min, selects 8 rev/mins speed when the coating pan rotating speed begins for use; Along with of the continuous formation of film-coating layer on plain sheet surface, progressively increase rotating speed again, be 40 rev/mins up to rotating speed.After hydrojet finishes,, get 1000 in tablet, promptly get with 60 ℃ of heated-air drying 25min.
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight.In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg.
Every of these article contain nacreous layer powder in Ca, must not be less than 60mg.
Embodiment 7. mixture
Nacreous layer powder 150g, glossy ganoderma 600g, Radix Glycyrrhizae 150g
More than three flavors, two flavor extracting in water secondaries except that nacreous layer powder add 12 times of water gagings of water, extracted filtration 3 hours for the 1st time; The dregs of a decoction add 10 times of amounts of water, extract 3 hours, filter, and merging filtrate filters; Place, get supernatant, being concentrated into relative density is 1.10～1.20 (70～80 ℃) concentrate, and nacreous layer powder water flies into fine powder, adds in the concentrate; Add Sodium Benzoate, each 5.0g of CMC, mixing is processed about 1000ml, promptly gets.
[discriminating]
Get preparation of the present invention and be equivalent to raw medicinal herbs 8.0g, put in the conical flask, add water 50ml, ultrasonic 20 minutes (power 300W, frequency 50kHz); Filter, and the macroporous adsorptive resins of filtrating (internal diameter 1.5cm, long 15cm, D101), with 10% ethanolic solution 100ml wash-out; Discard eluent, add 70% methanol solution 50ml wash-out then, collect eluent, water bath method, residue add normal butyl alcohol 20ml makes dissolving; Extract three times with the ammonia solution jolting, 20ml for the first time, the each 10ml of second and third time merges ammonia solution, extracts 2 times with the normal butyl alcohol jolting after adding hcl acidifying; Each 20ml merges normal butyl alcohol liquid, and evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight.In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color.
[assay]
The preparation of need testing solution is got preparation of the present invention and is equivalent to raw medicinal herbs 16.0g, and precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation add hydrochloric acid solution (1 → 2ml) 10ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get.
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add 5% sodium potassium tartrate tetrahydrate and triethanolamine solution (1 → 2ml) each 5ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with Calcium Disodium Versenate vs (0.05mol/L) titration, becomes blueness by redness to solution.The Calcium Disodium Versenate vs (0.05mol/L) of every 1ml is equivalent to the Ca of 2.004mg.
These article preparation is equivalent to raw medicinal herbs 0.7g, and nacreous layer powder must not be less than 60mg in Ca.
Claims (7)
1. the detection method of the Chinese medicine composition of a mental-tranquilization is characterized in that this method comprises following method:
Discrimination method is:
Get the said composition preparation that is equivalent to raw medicinal herbs 5.0-10.0g, put in the conical flask, add water 30-70ml, ultrasonic 10-30 minute, filter; The macroporous adsorptive resins of filtrating with 5-20% ethanolic solution 80-120ml wash-out, discards eluent, adds 60-80% methanol solution 30-70ml wash-out then, collects eluent; Water bath method, residue add normal butyl alcohol 20ml makes dissolving, extracts three times with the ammonia solution jolting, for the first time 10-30ml; The each 5-15ml of second and third time merges ammonia solution, extracts 1-3 time with the normal butyl alcohol jolting after adding hcl acidifying, at every turn 10-30ml; Merge normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition; According to an appendix VI of Chinese Pharmacopoeia version in 2005 B thin-layered chromatography test, draw each 10-30 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-water of 10-15: 5-10: 1-3 is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 5-15 minute, and inspected under the daylight; In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
Content assaying method is:
The preparation of need testing solution: get the said composition preparation that is equivalent to raw medicinal herbs 10.0-20.0g, precision takes by weighing 1.0-3.0g, puts in the 10ml tool plug centrifuge tube; Adding distil water 3-10ml, jolting dissolving, centrifugal 5-15 minute; Leave standstill; Discard upper solution, and then add 3-8ml distilled water, like method operation 2-5 time; To precipitate and move in the 250ml volumetric flask, gradation adds the hydrochloric acid solution 5-15ml of 1 → 2ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get;
The accurate need testing solution 15-40ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine solution of 5% sodium potassium tartrate tetrahydrate and 1 → 2ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with the Calcium Disodium Versenate vs titration of 0.05mol/L, becomes blueness by redness to solution; The Calcium Disodium Versenate vs of every 1ml0.05mol/L is equivalent to the Ca of 2.004mg; Be equivalent to raw medicinal herbs 0.7g said composition preparation, contain nacreous layer powder, must not be less than 40-80mg in Ca;
Wherein, the bulk drug of said Chinese medicine composition consists of: nacreous layer powder 150 weight portions, red sesame 600 weight portions, Radix Glycyrrhizae 150 weight portions, wilsonii 100 weight portions.
2. the detection method of Chinese medicine composition as claimed in claim 1 is characterized in that this method comprises following method:
Differentiate: get and be equivalent to raw medicinal herbs 8.0g said composition preparation, put in the conical flask, add water 50ml, ultrasonic 20 minutes, filter; The filtrated D101 macroporous adsorptive resins of internal diameter 1.5cm, long 15cm with 10% ethanolic solution 100ml wash-out, discards eluent, adds 70% methanol solution 50ml wash-out then, collects eluent; Water bath method, residue add normal butyl alcohol 20ml makes dissolving, extracts three times with the ammonia solution jolting, for the first time 20ml; The each 10ml of second and third time merges ammonia solution, extracts 2 times each 20ml with the normal butyl alcohol jolting after adding hcl acidifying; Merge normal butyl alcohol liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 1.0g shines medicinal material solution in pairs with legal system in addition; According to an appendix VIB of Chinese Pharmacopoeia version in 2005 thin-layered chromatography test, draw each 20 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the sodium carboxymethyl cellulose; Lower floor's solution with methenyl choloride-methanol-waters of 13: 7: 2 is developping agent, launches, and takes out; Dry; Spray is with 5% ethanol solution of sulfuric acid, and 105 ℃ were heated 10 minutes, and inspected under the daylight; In the test sample chromatogram, with reference substance chromatogram relevant position on, show the spot of same color;
Content assaying method is:
The preparation of need testing solution: get preparation of the present invention and be equivalent to raw medicinal herbs 16.0g, precision takes by weighing 1.5g, puts in the 10ml tool plug centrifuge tube adding distil water 5ml; The jolting dissolving centrifugal 10 minutes, is left standstill; Discard upper solution, and then add 5ml distilled water, like method operation 3 times; To precipitate and move in the 250ml volumetric flask, gradation adds the hydrochloric acid solution 10ml of 1 → 2ml, wait to precipitate whole dissolvings after,, shake up to scale with distilled water diluting, filter, promptly get;
The accurate need testing solution 25ml that draws of determination method; Place the 250ml conical flask, add water 20ml, add each 5ml of triethanolamine solution of 5% sodium potassium tartrate tetrahydrate and 1 → 2ml; Shake up; It is an amount of to add 20% sodium hydroxide solution 10ml and calcium indicator solution again, with the titration of 0.05mol/L Calcium Disodium Versenate vs, becomes blueness by redness to solution; The Calcium Disodium Versenate vs of every 1ml is equivalent to the Ca of 2.004mg; Be equivalent to the said composition preparation of raw medicinal herbs 0.7g, contain nacreous layer powder, must not be less than 60mg in Ca.
3. the application of Chinese medicine composition in the anti-anoxic of preparation, resisting myocardial ischemia or enhancing learning and memory medicine is characterized in that the bulk drug of said Chinese medicine composition consists of: nacreous layer powder 100-200 weight portion, glossy ganoderma 500-800 weight portion, Radix Glycyrrhizae 100-200 weight portion.
4. application as claimed in claim 3 is characterized in that the bulk drug of said Chinese medicine composition consists of: nacreous layer powder 100 weight portions, glossy ganoderma 800 weight portions, Radix Glycyrrhizae 100 weight portions.
5. application as claimed in claim 3 is characterized in that the bulk drug of said Chinese medicine composition consists of: nacreous layer powder 200 weight portions, glossy ganoderma 500 weight portions, Radix Glycyrrhizae 200 weight portions.
6. application as claimed in claim 3 is characterized in that the bulk drug of said Chinese medicine composition consists of: nacreous layer powder 150 weight portions, glossy ganoderma 600 weight portions, Radix Glycyrrhizae 150 weight portions.
7. application as claimed in claim 3 is characterized in that the bulk drug of said Chinese medicine composition consists of: nacreous layer powder 150 weight portions, red sesame 600 weight portions, Radix Glycyrrhizae 150 weight portions, wilsonii 100 weight portions.
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| CN200710179528XA Division CN101455714B (en) | 2007-12-14 | 2007-12-14 | Detection method of traditional Chinese medicine composition capable of nourishing the heart to calm the mind |
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| WO2013155714A1 (en) * | 2012-04-20 | 2013-10-24 | 江苏安惠生物科技有限公司 | Heart rejuvenating capsule |
| CN103005594B (en) * | 2012-12-18 | 2014-07-16 | 段海庆 | Beverage |
| CN104833661A (en) * | 2015-01-30 | 2015-08-12 | 吉林修正药业新药开发有限公司 | Quality control method of drug for nourishing blood and quieting spirit |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1269514C (en) * | 2004-07-30 | 2006-08-16 | 一笑堂（湖南）制药有限公司 | Kidney supplementing life prolonging preparation and its making method |
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| CN1269514C (en) * | 2004-07-30 | 2006-08-16 | 一笑堂（湖南）制药有限公司 | Kidney supplementing life prolonging preparation and its making method |
Non-Patent Citations (3)
| Title |
|---|
| 中华人民共和国***药典委员会编.珍合灵片.《***颁药品标准中药成方制剂第5册》.1992,93. * |
| 蔡德生等.珍合灵浸膏对小鼠中枢抑制作用和抗缺氧作用.《中国临床药理学与治疗学》.2003,第8卷(第6期),635-637. * |
| 许建中等.珍合灵片治疗女性更年期综合征36例疗效观察.《上海医药》.2000,第21卷(第1期),32-33. * |
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