CN101380410A - Medicine for treating hyperactivity of fire due to yin deficiency and preparation method of the formulation thereof - Google Patents
Medicine for treating hyperactivity of fire due to yin deficiency and preparation method of the formulation thereof Download PDFInfo
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Abstract
The invention relates to a traditional Chinese medicine preparation for curing syndrome of fire excess from yin deficiency, which has effective healing efficacy on fire excess from yin deficiency, tidal fever and night sweating, dry mouth and sore throat, tinnitus and spermatorrhea and brown urine, and has the efficacy of nourishing yin to reduce pathogenic fire. The invention is characterized in that a preparation method of the traditional Chinese medicine preparation-Zhi Bai Di Huang chewable tablet prepared by reforming Zhi Bai Di Huang tablet type has the technical proposal that a extraction process is optimized and filtered; modern new device, new technology and new method are adopted for the industrialization production; the research of the quality standard is that thin layer differentiation is perfected and improved on the basis of the original standard; the measurement method of the contents is drawn up; the quality control is carried out on all medicinal odour; the standard of the quality of products is advanced and controllable, thus guaranteeing the clinical healing efficacy.
Description
The invention belongs to field of traditional Chinese, relate to a kind of preparation method for the treatment of the medicine and the preparation thereof of syndrome of hyperactivity of fire due to deficiency of YIN.
Deficiency syndrome are the yin deficiency syndromes in common clinically, the multiple disease, particularly deficiency syndrome.Accelerate at modern society rhythm, people's operating pressure is big, under the high present situation of dietary protein content, and people's easier " getting angry " (hyperactivity of fire caused by deficiency of YIN), this disease sickness rate is ascendant trend day by day, and sickness rate rejuvenation day by day.Syndrome of hyperactivity of fire due to deficiency of YIN shows as hectic fever night sweat on tcm clinical practice, dysphoria with feverish sensation in the chest palms and soles, flush, xerostomia pharyngalgia, toothache, tinnitus seminal emission, diseases such as oliguria with reddish urine.The clinical diabetes that often show as of modern medicine, climacteric syndrome, seminal emission, tinnitus, diseases such as hypertension, infertility, acne.Therefore these diseases are very big to human health risk, treat and prevent this type of disease significant.Western medicine can only treatment according to differentiation of diseases to this type of disease, sometimes to having only subjective symptom not have the patient of objective indicator to feel simply helpless, and Chinese medicine is to this type of disease, using dialectical opinion from integral body controls, with multipath, multi-level, regulate body's immunity, prevention and prevention morbid state take place, development, and herbal toxic effect is little, has shown good advantages for development.Therefore develop safe and effectively, taking convenience can fundamentally reach the therapeutic purposes Chinese patent medicine, and human health and social development are of great immediate significance.
Record kind " ZHIBAIDIHUANG sheet " in the 5th in " Drug Standard of Ministry of Public Health of the Peoples Republic of China " Chinese traditional patent formulation preparation, be by classic prescriptions " LIUWEI DIHUANG WAN " add the Rhizoma Anemarrhenae, the Cortex Phellodendri prescription forms.Its reasonable recipe, on the basis of six drugs containing rehmanniae prescription nourishing kidney yin, the Rhizoma Anemarrhenae promotes the production of body fluid and moisturizes, and lets out fire mutually clearly, and the compatibility Cortex Phellodendri lets out fiery mutually strong clearly.All medicine compatibilities are played nourishing kidney-yin altogether, fall fire mutually, the merit of clearind deficient heat, to the hectic fever night sweat that the deficiency of YIN causes, dysphoria with feverish sensation in the chest palms and soles, flush, the xerostomia pharyngalgia, toothache, the tinnitus seminal emission, diseases such as oliguria with reddish urine have significant curative effect, be the different needs of adaptation extensive patients, so we further research and development have been carried out to this kind.
The objective of the invention is to the ZHIBAIDIHUANG sheet is rationally improved, the development onset more rapidly, take convenient chewable tablet.The effective ingredient of chewable tablet medicine when chewing just begins to be absorbed by oral mucosa, has just brought into play therapeutical effect after arriving gastrointestinal tract, and disintegrating procedue is of short duration, and the medicine stripping is rapid, therefore than the bioavailability height of general tablet; And the chewable tablet taking convenience even also can take medicine on time under the situation of hydropenia, has overcome tablet and has gone out, needing in the travelling process inconvenience with water delivery service; Chewable tablet has improved the bad mouthfeel when taking medicine owing to add correctives, makes patient be easy to accept.For this prescription has increased a novel form again, to adapt to the medication needs of different patients under varying environment.
Another object of the present invention is to be optimized on extraction process and to screen, and adopts modern new equipment, new technique, new method on preparation process, has formulated the production technology of reasonable science, is fit to industrialized great production.
Another purpose of the present invention is to adopt different auxiliary material to screen in the tablet formulation process, preferably is beneficial to the adjuvant of tablet molding and features good taste, has guaranteed the stability of tablet.Wherein said adjuvant comprises filler, correctives, disintegrating agent and lubricant, and wherein filler is selected from a kind of of lactose, mannitol or two kinds, and its consumption is 2%～10%; Correctives is selected from a kind of in citric acid, the tartaric acid or two kinds, and its consumption is 0.6%～1.2%; Disintegrating agent is selected from a kind of of microcrystalline Cellulose, carboxymethylstach sodium or two kinds, and its consumption is 3%～8%; Lubricant is selected from a kind of of magnesium stearate, sodium lauryl sulphate or two kinds, and its consumption is 0.6%～1.2%.A further object of the present invention is that preparation has been carried out detailed deep quality standard research, improves on the basis of primary standard, and all flavour of a drug have been carried out quality control.Only Cortex Moutan and Cortex Phellodendri are differentiated under the former tablet item that this product has all been carried out more deep Study on Identification to the medical material of respectively distinguishing the flavor of in the prescription in development process, revised the discriminating of Cortex Moutan and Cortex Phellodendri, and increased newly the thin layer discriminating of Fructus Corni.Method is all simple and feasible, and the feature speckle is obvious, and specificity is strong; Fructus Corni is this product ministerial drug, effect with liver and kidney tonifying, adopt loganin content in high effective liquid chromatography for measuring this product, the result shows that this method is simple and feasible, and method is stable, favorable reproducibility, and accuracy and precision are preferably arranged, can control the quality of this product effectively, guaranteed clinical efficacy.
Technical scheme of the present invention is: three flavors such as the Rhizoma Dioscoreae in the former ZHIBAIDIHUANG tablet recipe, Fructus Corni, Rhizoma Alismatis are ground into fine powder, and Cortex Moutan is ground into fine powder; Four flavors such as all the other Rhizoma Anemarrhenaes decoct with water secondary, and each 1.5 hours, collecting decoction, filter, filtrate is condensed into the thick paste that relative density is 1.20～1.25 (60 ℃), adds three flavor fine powders such as above-mentioned Rhizoma Dioscoreae, mixing, vacuum drying (50～60 ℃) is pulverized, with Cortex Moutan fine powder mixing, add right amount of auxiliary materials, mixing, make granule, drying, granulate, add right amount of auxiliary materials, be pressed into 1000, promptly.
In extraction dried particles of the present invention, add 3%～8% microcrystalline Cellulose or carboxymethylstach sodium, mixing sieves, and adds 0.6%～1.2% magnesium stearate or sodium lauryl sulphate, mixing, tabletting is tablet of the present invention.
Using method of the present invention: chew or suck clothes.One time 3,4 times on the one.Be described in further detail below by the extraction formulation method and the method for quality control of specific embodiment the ZHIBAIDIHUANG chewable tablet.
Embodiment 1:
Three flavors such as the Rhizoma Dioscoreae in the former ZHIBAIDIHUANG tablet recipe, Fructus Corni, Rhizoma Alismatis are ground into fine powder, and Cortex Moutan is ground into fine powder; Four flavors such as all the other Rhizoma Anemarrhenaes decoct with water secondary, and each 1.5 hours, collecting decoction, filter, filtrate is condensed into the thick paste that relative density is 1.20～1.25 (60 ℃), adds three flavor fine powders such as above-mentioned Rhizoma Dioscoreae, mixing, vacuum drying (50～60 ℃) is pulverized, with Cortex Moutan fine powder mixing, add lactose 35g and citric acid 4g, mixing is granulated, drying promptly gets the present invention and extracts dried particles.
Embodiment 2:
Three flavors such as the Rhizoma Dioscoreae in the former ZHIBAIDIHUANG tablet recipe, Fructus Corni, Rhizoma Alismatis are ground into fine powder, and Cortex Moutan is ground into fine powder; Four flavors such as all the other Rhizoma Anemarrhenaes decoct with water secondary, and each 1.5 hours, collecting decoction, filter, filtrate is condensed into the thick paste that relative density is 1.20～1.25 (60 ℃), adds three flavor fine powders such as above-mentioned Rhizoma Dioscoreae, mixing, vacuum drying (50～60 ℃) is pulverized, with Cortex Moutan fine powder mixing, add mannitol 20g and tartaric acid 5g, mixing is granulated, drying promptly gets the present invention and extracts dried particles.
Embodiment 3:
Three flavors such as the Rhizoma Dioscoreae in the former ZHIBAIDIHUANG tablet recipe, Fructus Corni, Rhizoma Alismatis are ground into fine powder, and Cortex Moutan is ground into fine powder; Four flavors such as all the other Rhizoma Anemarrhenaes decoct with water secondary, and each 1.5 hours, collecting decoction, filter, filtrate is condensed into the thick paste that relative density is 1.20～1.25 (60 ℃), adds three flavor fine powders such as above-mentioned Rhizoma Dioscoreae, mixing, vacuum drying (50～60 ℃) is pulverized, with Cortex Moutan fine powder mixing, add lactose 30g, mannitol 10g and citric acid 3g, mixing is granulated, drying promptly gets the present invention and extracts dried particles.
Embodiment 4:
To add the 20g microcrystalline Cellulose in any extraction dried particles in the various embodiments described above, mixing sieves, and adds the 5g magnesium stearate, mixing, and tabletting is tablet of the present invention.
Embodiment 5:
To add the 15g carboxymethylstach sodium in any extraction dried particles in the various embodiments described above, mixing sieves, and adds the 6g magnesium stearate, mixing, and tabletting is tablet of the present invention.
Embodiment 6:
To add the 16g carboxymethylstach sodium in any extraction dried particles in the various embodiments described above, mixing sieves, and adds the 6g sodium lauryl sulphate, mixing, and tabletting is tablet of the present invention.
Embodiment 7:
In the quality control of the present invention, the medical material of respectively distinguishing the flavor of in the prescription is all carried out more deep Study on Identification, revised the discriminating of Cortex Moutan and Cortex Phellodendri, and increased the thin layer discriminating of Fructus Corni newly.
The thin layer of Cortex Phellodendri is differentiated as follows: get 4 of this product, porphyrize adds methanol 10ml, and supersound process 15 minutes filters, and filtrate is as need testing solution.Other gets Cortex Phellodendri control medicinal material 0.2g, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, control medicinal material solution, reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10:6:1:1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
The thin layer of Cortex Moutan is differentiated as follows: get 6 of this product, and porphyrize, the 20ml that adds diethyl ether, supersound process 5 minutes filters, and filtrate volatilizes, and residue adds acetone 1ml makes dissolving, as need testing solution.Other gets Cortex Moutan control medicinal material 0.5g, shines medical material solution in pairs with legal system.Get the paeonol reference substance again, add acetone and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, control medicinal material solution, reference substance solution, put respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (3:1) is developing solvent, launch, take out, dry, spray is with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.
The thin layer of Fructus Corni is differentiated as follows: get Fructus Corni control medicinal material 0.5g, and the 20ml that adds diethyl ether, supersound process 5 minutes filters, and filtrate volatilizes, and residue adds acetone 2ml makes dissolving, in contrast medical material solution.It is an amount of that other gets the ursolic acid reference substance, adds dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, Fructus Corni control medicinal material solution and ursolic acid reference substance solution under the Cortex Moutan discriminating item, put respectively on same silica gel g thin-layer plate, upper solution with toluene-ethyl acetate-formic acid (15:2:1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.
In the quality control of the present invention, set up the assay of loganin:, be filler with the octadecylsilane chemically bonded silica according to high effective liquid chromatography for measuring; (get anhydrous sodium acetate 2.1g, add the about 200ml of water and make dissolving, regulate pH value to 4.5, add water to 500ml, promptly)-acetonitrile-water (30:15:55) is a mobile phase with acetate buffer with glacial acetic acid; Detect wavelength 240nm.Get the about 4mg of loganin reference substance, the accurate title, decide, and puts in the 10ml measuring bottle, adds 80% dissolve with methanol and be diluted to scale, shakes up; Precision is measured 1ml, puts in the 10ml measuring bottle, adds 50% methanol and is diluted to scale, shakes up, in contrast product solution.Get 20 of this product, the accurate title, decided porphyrize, get about 0.5g, the accurate title, decide, and puts in the 50ml tool plug conical flask, the accurate 50% methanol 25ml that adds, close plug claims to decide weight, supersound process (power 100W, frequency 40kHz) 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 50% methanol, filter, precision is measured subsequent filtrate 5ml, is added in neutral alumina post (100～200 orders, 4g, internal diameter 1cm) on, with 40% methanol 50ml eluting, collect effluent and eluent, evaporate to dryness, residue 50% dissolve with methanol, and be transferred in the 2ml measuring bottle, add 50% methanol to scale, shake up, as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
Below by test the adjuvant in the above-mentioned tablet formulation process is further screened and optimizes.
Test example 1: the selection of different filleies and consumption
Consider that this product dosage form is a chewable tablet, alternative filler has lactose, mannitol, starch, sucrose etc., and according to mouthfeel and compressibility, we screen above-mentioned adjuvant.Get recipe quantity crude drug of this product, in preparation technology under prescription ratio and the method for making item, Chinese medicine dry powder, add the Cortex Moutan fine powder, behind the mixing, get fine powder, add lactose, mannitol, sucrose, starch according to 2%, 8%, 10%, 12% ratio respectively; Mixing adopts 70% alcohol granulation respectively, drying, and granulate, tabletting is that index compares with mouthfeel and compressibility.The results are shown in Table 1.
The selection of table 1 filler and proportioning thereof
The result shows that preferred lactose, mannitol have mouthfeel preferably as filler, and the sheet hardness of extrusion is moderate, and determines that selecting the consumption of lactose, mannitol for use is 2%～10%.
Test example 2: the investigation of correctives citric acid consumption
Get the granule that makes, add citric acid in 0.4%, 0.6%, 0.8%, 1.2%, 1.4% ratio respectively, mixing, tabletting is an index with the mouthfeel respectively.The results are shown in Table 2.
The selection of table 2 citric acid consumption
The result shows that the citric acid consumption is 0.6～1.2% o'clock obtained tablet, and mouthfeel is better, determines that therefore the citric acid consumption is 0.6～1.2%.
Test example 3: the screening of different auxiliary material
Get the granule that makes, add magnesium stearate, sodium lauryl sulphate, micropowder silica gel respectively in 0.8% ratio respectively, 4% microcrystalline Cellulose, carboxymethylstach sodium, low-substituted hydroxypropyl cellulose, mixing, tabletting the results are shown in Table 3 respectively.
Table 3 different auxiliary material is to the influence of tablet
The result shows that preferred magnesium stearate, sodium lauryl sulphate are lubricant, and microcrystalline Cellulose, carboxymethylstach sodium are that disintegrating agent carries out the different proportion combination, and tablet appearance is better.
Test example 4: the investigation of different auxiliary material addition
At first the consumption of magnesium stearate is investigated
Get the granule that makes, add magnesium stearate in 0.4%, 0.6%, 0.8%, 1.2% ratio respectively, add 4% microcrystalline Cellulose, mixing, tabletting the results are shown in Table 4 respectively.
Table 4 magnesium stearate addition is to the influence of tablet
The magnesium stearate addition is 0.4% o'clock, and tablet weight variation is bigger, and 2 overruns are arranged; Consumption is 0.6% o'clock, and tablet weight variation is less, and consumption is 0.8% and 1.2% o'clock, and the label smooth surface is smooth, no sliver phenomenon.Therefore determine that the magnesium stearate consumption is 0.6～1.2%.
Further the consumption of microcrystalline Cellulose is investigated.
Get the granule that makes, add microcrystalline Cellulose in 2%, 3%, 4%, 8% ratio respectively, add 1% magnesium stearate, mixing, tabletting the results are shown in Table 5 respectively.
Table 5 microcrystalline Cellulose addition is to the influence of tablet
The microcrystalline Cellulose addition is 2% o'clock, and inter-particle adhesion is relatively poor, is easy to sliver; Consumption is 3% o'clock, and inter-particle adhesion is good, no sliver; Consumption is 4% and 8% o'clock, and tablet surface is bright and clean, and hardness is suitable, no sliver phenomenon.Therefore determine that the microcrystalline Cellulose addition is 3%～8%.
Claims (4)
1. a Chinese medicine preparation for the treatment of syndrome of hyperactivity of fire due to deficiency of YIN is characterized in that its preparation method is that three flavors such as the Rhizoma Dioscoreae in the former ZHIBAIDIHUANG tablet recipe, Fructus Corni, Rhizoma Alismatis are ground into fine powder, and Cortex Moutan is ground into fine powder; Four flavors such as all the other Rhizoma Anemarrhenaes decoct with water secondary, and each 1.5 hours, collecting decoction, filter, filtrate is condensed into the thick paste that relative density is 1.20～1.25 (60 ℃), adds three flavor fine powders such as above-mentioned Rhizoma Dioscoreae, mixing, vacuum drying (50～60 ℃) is pulverized, with Cortex Moutan fine powder mixing, add right amount of auxiliary materials, mixing, make granule, drying, granulate, add right amount of auxiliary materials, be pressed into 1000, promptly.Wherein said adjuvant comprises filler, correctives, disintegrating agent and lubricant, and wherein filler is selected from a kind of of lactose, mannitol or two kinds; Correctives is selected from citric acid, tartaric a kind of or two kinds; Disintegrating agent is selected from a kind of of microcrystalline Cellulose, carboxymethylstach sodium or two kinds; Lubricant is selected from a kind of of magnesium stearate, sodium lauryl sulphate or two kinds.
2. the described a kind of Chinese medicine preparation for the treatment of syndrome of hyperactivity of fire due to deficiency of YIN of claim 1 is characterized in that in the tablet formulation process that as lactose, the mannitol of filler, its consumption is 2%～10%; As citric acid, the tartaric acid of correctives, its consumption is 0.6%～1.2%; As microcrystalline Cellulose, the carboxymethylstach sodium of disintegrating agent, its consumption is 3%～8%; As magnesium stearate, the sodium lauryl sulphate of lubricant, its consumption is 0.6%～1.2%.
3. the described a kind of Chinese medicine preparation for the treatment of syndrome of hyperactivity of fire due to deficiency of YIN of claim 1 is characterized in that in the tablet formulation process that as the lactose of filler, its consumption is 8%; As the citric acid of correctives, its consumption is 0.8%; As the microcrystalline Cellulose of disintegrating agent, its consumption is 4%; As the magnesium stearate of lubricant, its consumption is 1.0%.
4. the described a kind of Chinese medicine preparation for the treatment of syndrome of hyperactivity of fire due to deficiency of YIN of claim 1 is characterized in that its quality control index is: (one) thin layer is differentiated as follows:
(1) get 4 of this product, porphyrize adds methanol 10ml, and supersound process 15 minutes filters, and filtrate is as need testing solution.Other gets Cortex Phellodendri control medicinal material 0.2g, shines medical material solution in pairs with legal system.Get the berberine hydrochloride reference substance again, add methanol and make the solution that every 1ml contains 0.1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, control medicinal material solution, reference substance solution, put respectively on same silica gel g thin-layer plate, with ethyl acetate-butanone-formic acid-water (10:6:1:1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) get 6 of this product, porphyrize, the 20ml that adds diethyl ether, supersound process 5 minutes filters, and filtrate volatilizes, and residue adds acetone 1ml makes dissolving, as need testing solution.Other gets Cortex Moutan control medicinal material 0.5g, shines medical material solution in pairs with legal system, gets the paeonol reference substance again, adds acetone and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, control medicinal material solution, reference substance solution, put respectively on same silica gel g thin-layer plate, with thiacyclohexane-ethyl acetate (3:1) is developing solvent, launch, take out, dry, spray is with the acid 5% ferric chloride alcoholic solution of hydrochloric acid, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get Fructus Corni control medicinal material 0.5g, the 20ml that adds diethyl ether, supersound process 5 minutes filters, and filtrate volatilizes, and residue adds acetone 2ml makes dissolving, in contrast medical material solution.It is an amount of that other gets the ursolic acid reference substance, adds dehydrated alcohol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution, Fructus Corni control medicinal material solution and ursolic acid reference substance solution under the Cortex Moutan discriminating item, put respectively on same silica gel g thin-layer plate, upper solution with toluene-ethyl acetate-formic acid (15:2:1) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear.In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show the speckle of same color.
(2) assay of loganin is as follows: according to high effective liquid chromatography for measuring, be filler with the octadecylsilane chemically bonded silica; (get anhydrous sodium acetate 2.1g, add the about 200ml of water and make dissolving, regulate pH value to 4.5, add water to 500ml, promptly)-acetonitrile-water (30:15:55) is a mobile phase with acetate buffer with glacial acetic acid; Detect wavelength 240nm.Get the about 4mg of loganin reference substance, the accurate title, decide, and puts in the 10ml measuring bottle, adds 80% dissolve with methanol and be diluted to scale, shakes up; Precision is measured 1ml, puts in the 10ml measuring bottle, adds 50% methanol and is diluted to scale, shakes up, in contrast product solution.Get 20 of this product, the accurate title, decided porphyrize, get about 0.5g, the accurate title, decide, and puts in the 50ml tool plug conical flask, the accurate 50% methanol 25ml that adds, close plug claims to decide weight, supersound process (power 100W, frequency 40kHz) 30 minutes is put cold, claim again to decide weight, supply the weight that subtracts mistake, shake up with 50% methanol, filter, precision is measured subsequent filtrate 5ml, is added in neutral alumina post (100～200 orders, 4g, internal diameter 1cm) on, with 40% methanol 50ml eluting, collect effluent and eluent, evaporate to dryness, residue 50% dissolve with methanol, and be transferred in the 2ml measuring bottle, add 50% methanol to scale, shake up, as need testing solution.Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly.
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| CNA2007101137317A CN101380410A (en) | 2007-09-05 | 2007-09-05 | Medicine for treating hyperactivity of fire due to yin deficiency and preparation method of the formulation thereof |
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| CNA2007101137317A CN101380410A (en) | 2007-09-05 | 2007-09-05 | Medicine for treating hyperactivity of fire due to yin deficiency and preparation method of the formulation thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102401821A (en) * | 2010-11-02 | 2012-04-04 | 河北以岭医药研究院有限公司 | Fluorescence reinforcing thin layer identification method of tree peony root-bark |
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN103134896A (en) * | 2011-11-25 | 2013-06-05 | 张金荣 | Detection method for Chinese materia medica preparation for treating chronic prostatitis |
| CN105456656A (en) * | 2015-12-10 | 2016-04-06 | 韦焜 | Traditional Chinese medicinal pills for treating toothache with syndrome of yin deficiency and preparation method of traditional Chinese medicinal pills |
| CN105477285A (en) * | 2015-12-10 | 2016-04-13 | 韦焜 | Preparation method of mouthwash for treating yin deficiency type toothache |
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2007
- 2007-09-05 CN CNA2007101137317A patent/CN101380410A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102401821A (en) * | 2010-11-02 | 2012-04-04 | 河北以岭医药研究院有限公司 | Fluorescence reinforcing thin layer identification method of tree peony root-bark |
| CN103134896A (en) * | 2011-11-25 | 2013-06-05 | 张金荣 | Detection method for Chinese materia medica preparation for treating chronic prostatitis |
| CN103134883A (en) * | 2011-11-28 | 2013-06-05 | 邯郸摩罗丹药业股份有限公司 | Medicine composition and detecting method of manufacturing agent of medicine composition |
| CN103134883B (en) * | 2011-11-28 | 2015-05-13 | 邯郸制药股份有限公司 | Medicine composition and detecting method of formula of medicine composition |
| CN105456656A (en) * | 2015-12-10 | 2016-04-06 | 韦焜 | Traditional Chinese medicinal pills for treating toothache with syndrome of yin deficiency and preparation method of traditional Chinese medicinal pills |
| CN105477285A (en) * | 2015-12-10 | 2016-04-13 | 韦焜 | Preparation method of mouthwash for treating yin deficiency type toothache |
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