CN1887324A - Chinese composition and its prepn process and quality control method - Google Patents
Chinese composition and its prepn process and quality control method Download PDFInfo
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- CN1887324A CN1887324A CN 200510200353 CN200510200353A CN1887324A CN 1887324 A CN1887324 A CN 1887324A CN 200510200353 CN200510200353 CN 200510200353 CN 200510200353 A CN200510200353 A CN 200510200353A CN 1887324 A CN1887324 A CN 1887324A
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Abstract
The present invention is one kind of Chinese medicine composition, and belongs to the field of Chinese medicine technology. The Chinese medicine composition is prepared with nine kinds of Chinese medicinal materials, including prepared fleeceflower root, prepared rhizome of rehmannia, mulberry, angelica, malaytea scurfpea fruit, etc. and through certain technological process. It has high curative effect on liver and kidney deficiency and essence and blood deficiency caused alopecia, soreness of waist and knees, insomnia, dreamful sleep and other diseases. In addition, the present invention also discloses the preparation process and quality control method of the Chinese medicine composition.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof and method of quality control, belong to the field of Chinese medicines.
Background technology
Deficiency of the liver and kindey, essence and blood lose the alopecia due to the void, soreness of the waist and knees, and diseases such as insomnia and dreamful sleep are middle-aged and elderly people, brain overwork person, sexual life overfrequency person's common symptons.At modern medicine, more than all diseases belong to degeneration or sub-health state, do not have effective symptomatic treatment medicine.And, then belong to deficiency syndrome in the traditional Chinese medical science, and as long as tonification is proper, the effect that can obtain just.The advantage and the characteristic of performance treatment by Chinese herbs primary disease, further investigation and exploitation both can improve patient's quality of life to this sick medicine, can produce very high economic benefit again, and the exploitation of this veriety has broad prospects, and will bring glad tidings for extensive patients.
Summary of the invention
Treatment deficiency of the liver and kindey, the essence and blood that the present invention developed loses the alopecia due to the void, and soreness of the waist and knees, the Chinese medicine composition of insomnia and dreamful sleep are to be made by the crude drug of following weight part ratio:
Radix Polygoni Multiflori Preparata 5-15, Radix Rehmanniae Preparata 1-8, Fructus Mori 1-5, Fructus Lycii 1-5, Radix Angelicae Sinensis 1-5, Fructus Psoraleae 1-5, Rhizoma Chuanxiong 1-5, Poria 1-5, Pericarpium Citri Reticulatae 1-4.
The above-mentioned raw materials optimum ratio is: Radix Polygoni Multiflori Preparata 8, Radix Rehmanniae Preparata 4, Fructus Mori 3, Fructus Lycii 3, Radix Angelicae Sinensis 3, Fructus Psoraleae 3, Rhizoma Chuanxiong 3, Poria 3, Pericarpium Citri Reticulatae 2.
In the above crude drug, the Radix Polygoni Multiflori Preparata nourishing liver, invigorating kidney, replenishing essence is nourished blood, and blackening and generating hair is monarch drug; Fructus Lycii, Fructus Mori principal drug assistance are taken a tonic or nourishing food to build up one's health Liver and kidney, Radix Angelicae Sinensis, Radix Rehmanniae Preparata, Fructus Psoraleae nourshing blood and promoting blood circulation, the meridian dredging is opened a mao key, in order to hair growth, more than all medicines be ministerial drug altogether; Poria, Pericarpium Citri Reticulatae invigorating the spleen and benefiting QI, blood nourishing and hair, the source of the benefit hair growth promoting day after tomorrow is adjuvant drug; The Rhizoma Chuanxiong priming is up, and through sick institute is messenger drug, more than all medicine nourishing the liver and kidney, blood nourishing and hair, thus the alopecia of losing due to the void for deficiency of the liver and kindey, essence and blood has good therapeutical effect.
Aforementioned pharmaceutical compositions of the present invention adds the medicine correctives or/and drug excipient can be prepared into the pharmaceutical preparation that oral liquid, tablet, capsule, pill etc. use clinically according to the Chinese medicine preparation technology of routine.Said medicine correctives is one or more the combination in sucrose, sodium benzoate, stevioside, the protein sugar, so that the medicament of prepared one-tenth has good mouthfeel, overcomes and produces abnormal flavour behind the above Chinese herbal medicine compatibility and be difficult to the drawback that enters the mouth or swallow.Said drug excipient is one or more the combination in dextrin, magnesium stearate, microcrystalline Cellulose, carboxymethyl starch sodium, starch, Pulvis Talci, sodium bicarbonate, the citric acid, with the oral formulations that medication preparation of the present invention is become to be convenient to take.
The preparation method of above medicine can be in following two kinds of methods any:
1) above nine flavors decoct with water 1-3 time, add 5-12 times of water gaging at every turn, decoct 0.5-2 hour at every turn, collecting decoction filters, and filtrate was left standstill 8-48 hour, getting supernatant, to be evaporated to 20 ℃ relative density be 1.36 thick paste, and drying adds conventional adjuvant and makes capsule, pill, tablet etc.
2) get Radix Angelicae Sinensis, Fructus Psoraleae, Rhizoma Chuanxiong, Pericarpium Citri Reticulatae and add 4-9 and doubly measure the 30-90% alcohol reflux 1-3 time, each 1-3 hour, filter, it is 1.05～1.30 thick paste that filtrate is concentrated into relative density in the time of 60 ℃, standby; Medicinal residues and Radix Polygoni Multiflori Preparata, Radix Rehmanniae Preparata, Fructus Mori, Fructus Lycii, Poria decoct with water 1-3 time, add 6-12 times of water gaging at every turn, the each decoction 1-4 hour, collecting decoction filters, it is 1.05～1.30 clear paste that filtrate is concentrated into relative density in the time of 60 ℃, add the ethanol that 1-3 doubly measures, left standstill 8-36 hour, recovery ethanol is 1.05～1.30 clear paste to the relative density in the time of 60 ℃, merge with above-mentioned clear paste, add conventional adjuvant and make oral liquid.
By above method, can make the extract of the desired pharmaceutical composition of the present invention, through further test, can obtain preferred technology:
1) gets crude drug, decoct with water 3 times, add 10 times of amounts for the first time, add 8 times of amounts for the second time, add 6 times of amounts for the third time, the each decoction 1 hour, collecting decoction filters, and filtrate was left standstill 24 hours, getting supernatant, to be evaporated to 20 ℃ relative density be 1.36 thick paste, and drying is pulverized, medicine; Medicated powder is added suitable adjuvant, make required dosage form;
2) get Radix Angelicae Sinensis, Fructus Psoraleae, Rhizoma Chuanxiong, Pericarpium Citri Reticulatae and add 6 times of amount 75% alcohol reflux 1 time, 1 hour, filter, it is 1.10～1.20 thick paste that filtrate is concentrated into relative density in the time of 60 ℃, standby; Medicinal residues and Radix Polygoni Multiflori Preparata, Radix Rehmanniae Preparata, Fructus Mori, Fructus Lycii, Poria decoct with water 2 times, add 8 times of water gagings at every turn, decoct 1 hour at every turn, collecting decoction, filter, it is 1.10～1.20 clear paste that filtrate is concentrated into relative density in the time of 60 ℃, adds the ethanol of 2 times of amounts, left standstill 24 hours, recovery ethanol to the relative density in the time of 60 ℃ is 1.10～1.20 clear paste, merges drying with above-mentioned clear paste, pulverize, get medicated powder; Medicated powder is added suitable adjuvant, make required dosage form.
The inventor preferably makes capsule, and method is as follows:
The medicated powder that extraction process obtains is at last crossed 100 mesh sieves, add starch and be adjusted to required total amount, mix homogeneously, with 70% mistake, 20 mesh sieve wet granulations, drying, granulate incapsulates.
Medicine of the present invention can adopt following method to carry out assay and qualitative identification, makes the quality of the pharmaceutical preparations controlled.Select Radix Polygoni Multiflori Preparata, psoralen, isopsoralen, Hesperidin, Fructus Lycii in the prescription to carry out the thin layer discriminating, concrete grammar is as follows:
A. it is an amount of to get preparation of the present invention, uses methanol 50ml supersound extraction 30 minutes, filters, get subsequent filtrate 25ml, evaporate to dryness adds water 25ml and hydrochloric acid 3ml, chloroform 20ml, reflux 1 hour is put coldly, divides and to get chloroform layer, water layer adds chloroform again and extracts 2 times, each 10ml, combined chloroform liquid, evaporate to dryness, residue adds methanol makes dissolving, is settled to 10ml, as need testing solution; Other gets Radix Polygoni Multiflori control medicinal material 2g, decocts with water 1 hour, is concentrated in right amount, adds a small amount of kieselguhr mixing, drying, and the same legal system is shone medical material solution in pairs; Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned need testing solution 10 μ l, control medicinal material and reference substance solution, put respectively in same and contain on the silica gel g thin-layer plate that 0.3% sodium carboxymethyl cellulose is an adhesive, upper solution with petroleum ether-Ethyl formates of 15: 5: 1-formic acid is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle; Put in the ammonia smoked after, speckle becomes redness;
B. it is an amount of to get preparation of the present invention, and porphyrize adds ethyl acetate 20ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets psoralen, isopsoralen reference substance, adds ethyl acetate and makes the mixed solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetates of 4: 1 was developing solvent, launched, and took out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 10% potassium hydroxide methanol solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue and white fluorescence speckle;
C. it is an amount of to get preparation of the present invention, and porphyrize adds methanol 20ml, and supersound process 20 minutes filters, and filtrate is as need testing solution; Other gets the Hesperidin reference substance, adds methanol and makes saturated solution, in contrast product solution; According to the thin layer chromatography test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with methanol, open up about 3cm, spray was placed 3 hours with the methanol solution of 1% aluminum chloride, observed under the 365nm ultra-violet lamp; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D. it is an amount of to get preparation of the present invention, and add water 50ml and make dissolving, with ethyl acetate extraction twice, each 30ml, ethyl acetate liquid is concentrated into 0.5ml, as need testing solution; Other gets Fructus Lycii control medicinal material 5g, adds methanol 10ml and soaks 30 minutes in 50 ℃ of water-baths, filters, and filtrate is medical material solution in contrast; Each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 10: 0.2 chloroform-methanols was developing solvent, launched, and took out, dry, put in the ammonia steam and smoked 30 minutes, under the 365nm ultra-violet lamp, inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Emodin in the Radix Polygoni Multiflori Preparata medical material in the selection preparation is as the index of assay, and assay method is as follows:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water-glacial acetic acid of 60: 40: 1 is a mobile phase; The detection wavelength is 437nm.Number of theoretical plate calculates by the emodin peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the emodin reference substance, adds methanol and make the solution that every 1ml contains 4 μ g, promptly.
It is an amount of that preparation of the present invention is got in the preparation of need testing solution, porphyrize, mixing, get 1g, the accurate title, decide, and precision adds methanol 50ml, claim to decide weight, supersound process 60 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, evaporate to dryness adds water 25ml and hydrochloric acid 3ml, chloroform 20ml, reflux 1 hour, put coldly, divide and to get chloroform layer, water layer adds chloroform again and extracts 2 times, each 10ml, combined chloroform liquid, evaporate to dryness, residue add methanol makes dissolving, be settled to 10ml, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Extracting method in above qualitative identification method and the content assaying method can be supersound extraction, reflux, extract,, can be immersion, jolting also, leave standstill, and all belongs to the scope of extraction.
Preparation of the present invention is applied to clinically for many years always, and effect is obvious.In July, 2004 to the case of December, statistical result is as follows:
1) utilization Drug therapy 50 routine chronic alopecia patients of the present invention, 7 examples of fully recovering, produce effects 21 examples, effective 5 examples, invalid 17 examples, total effective rate 86.0%.The course of treatment is the shortest 21 days, and is the longest 39 days, average 32 days.
2) utilization combination treatment 32 routine deficiency of the liver and kindey of the present invention, essence and blood deficiency hair loss patient, the result cures 17 examples, produce effects 7 examples, effective 6 examples, invalid 2 examples, total effective rate 93.8%.
The specific embodiment
Embodiment 1:
Prescription: Radix Polygoni Multiflori Preparata 150g Radix Rehmanniae Preparata 80g Fructus Mori 50g
Fructus Lycii 50g Radix Angelicae Sinensis 50g Fructus Psoraleae 50g
Rhizoma Chuanxiong 50g Poria 50g Pericarpium Citri Reticulatae 40g
Method for making: above nine flavors, decoct with water 3 times, add 12 times of amounts for the first time, add 8 times of amounts for the second time, add 6 times of amounts for the third time, decocted 1 hour at every turn, collecting decoction filters, filtrate was left standstill 12 hours, got the thick paste that supernatant concentration to relative density is 1.36 (20 ℃), and drying is pulverized, cross 100 mesh sieves, add starch to aequum, mix homogeneously is granulated, drying, granulate adds magnesium stearate 2g, mixing, tabletting, promptly.
Embodiment 2:
Prescription: Radix Polygoni Multiflori Preparata 500g Radix Rehmanniae Preparata 100g Fructus Mori 100g
Fructus Lycii 100g Radix Angelicae Sinensis 100g Fructus Psoraleae 100g
Rhizoma Chuanxiong 100g Poria 100g Pericarpium Citri Reticulatae 100g
Method for making: above nine flavors, decoct with water 1 time, add 10 times of amounts of water, decocted 2 hours, decocting liquid filters, and filtrate was left standstill 48 hours, get the thick paste that supernatant concentration to relative density is 1.36 (20 ℃), drying is pulverized, cross 100 mesh sieves, add starch to aequum, mix homogeneously, granulate drying, granulate, incapsulate, promptly.
Embodiment 3:
Prescription: Radix Polygoni Multiflori Preparata 150g Radix Rehmanniae Preparata 80g Fructus Mori 40g
Fructus Lycii 40g Radix Angelicae Sinensis 30g Fructus Psoraleae 30g
Rhizoma Chuanxiong 20g Poria 50g Pericarpium Citri Reticulatae 20g
Method for making: get Radix Angelicae Sinensis, Fructus Psoraleae, Rhizoma Chuanxiong, Pericarpium Citri Reticulatae and add 9 times of amount 90% alcohol reflux 1 time, 1 hour, filter, filtrate is concentrated into the thick paste that relative density is 1.05～1.10 (60 ℃), and is standby; Medicinal residues and Radix Polygoni Multiflori Preparata, Radix Rehmanniae Preparata, Fructus Mori, Fructus Lycii, Poria decocts with water 3 times, add 12 times of water gagings at every turn, the each decoction 3 hours, collecting decoction filters, it is 1.10～1.20 clear paste that filtrate is concentrated into relative density in the time of 60 ℃, add the ethanol of 2 times of amounts, left standstill 24 hours, recovery ethanol is 1.10～1.20 clear paste to the relative density in the time of 60 ℃, merge with above-mentioned clear paste, it is an amount of to add refined honey and syrup, with low amounts of water sodium benzoate is dissolved, and under agitation adds in the medicinal liquid, add distilled water and transfer to 1000ml, shake up, cold preservation filters secondary, sterilization, embedding, promptly.
Embodiment 4:
Prescription: Radix Polygoni Multiflori Preparata 160g Radix Rehmanniae Preparata 80g Fructus Mori 60g
Fructus Lycii 60g Radix Angelicae Sinensis 60g Fructus Psoraleae 60g
Rhizoma Chuanxiong 60g Poria 60g Pericarpium Citri Reticulatae 40g
Method for making: get Radix Angelicae Sinensis, Fructus Psoraleae, Rhizoma Chuanxiong, Pericarpium Citri Reticulatae and add 4 times of amount 30% alcohol reflux 3 times, each 1.5 hours, filter, it is 1.20～1.30 thick paste that filtrate is concentrated into relative density in the time of 60 ℃, standby; Medicinal residues and Radix Polygoni Multiflori Preparata, Radix Rehmanniae Preparata, Fructus Mori, Fructus Lycii, Poria decoct with water 2 times, add 10 times of water gagings at every turn, decoct 1 hour at every turn, collecting decoction, filter, it is 1.20～1.30 clear paste that filtrate is concentrated into relative density in the time of 60 ℃, adds the ethanol of 3 times of amounts, left standstill 36 hours, recovery ethanol to the relative density in the time of 60 ℃ is 1.25～1.30 clear paste, merges drying with above-mentioned clear paste, pulverize, get medicated powder, cross 100 mesh sieves, it is an amount of to add carboxymethylstach sodium 100g and starch, be adjusted to required total amount, mix homogeneously adds water pill, drying, packing, promptly.
Embodiment 5: to the qualitative identification of product of the present invention
Get granule 1g of the present invention, use methanol 50ml supersound extraction 30 minutes, filter, get subsequent filtrate 25ml, evaporate to dryness adds water 25ml and hydrochloric acid 3ml, chloroform 20ml, reflux 1 hour is put coldly, divides and to get chloroform layer, water layer adds chloroform again and extracts 2 times, each 10ml, combined chloroform liquid, evaporate to dryness, residue adds methanol makes dissolving, is settled to 10ml, as need testing solution.Other gets Radix Polygoni Multiflori control medicinal material 2g, decocts with water 1 hour, is concentrated in right amount, adds a small amount of kieselguhr mixing, drying, and the same legal system is shone medical material solution in pairs.Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw each 2 μ l of above-mentioned need testing solution 10 μ l, control medicinal material and reference substance solution, put respectively in same and contain on the silica gel g thin-layer plate that 0.3% sodium carboxymethyl cellulose is an adhesive, upper solution with petroleum ether (30～60 ℃)-Ethyl formate-formic acid (15: 5: 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 identical orange-yellow fluorescence speckle; Put in the ammonia smoked after, speckle becomes redness.
Get granule 1g of the present invention, porphyrize adds ethyl acetate 20ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution.Other gets psoralen, isopsoralen reference substance, adds ethyl acetate and makes the mixed solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue and white fluorescence speckle.
Get granule 1g of the present invention, porphyrize adds methanol 20ml, and supersound process 20 minutes filters, and filtrate is as need testing solution.Other gets the Hesperidin reference substance, adds methanol and makes saturated solution, in contrast product solution.According to the thin layer chromatography test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with methanol, open up about 3cm, spray was placed 3 hours with the methanol solution of 1% aluminum chloride, observed down at ultra-violet lamp (365nm).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
Get granule 1g of the present invention, add water 50ml and make dissolving, with ethyl acetate extraction twice, each 30ml, ethyl acetate liquid is concentrated into 0.5ml, as need testing solution.Other gets Fructus Lycii control medicinal material 5g, adds methanol 10ml and soaks 30 minutes in 50 ℃ of water-baths, filters, and filtrate is medical material solution in contrast.Each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, chloroform-methanol (10: 0.2) is developing solvent, launches, and takes out, dry, put in the ammonia steam and smoked 30 minutes, under ultra-violet lamp (365nm), inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
Embodiment 6: to the assay of product of the present invention
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water-glacial acetic acid (60: 40: 1) is a mobile phase; The detection wavelength is 437nm.Number of theoretical plate calculates by the emodin peak should be not less than 3000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the emodin reference substance, adds methanol and make the solution that every 1ml contains 4 μ g, promptly.
Granule 10g of the present invention, porphyrize, mixing are got in the preparation of need testing solution, get 1g, the accurate title, decide, and precision adds methanol 50ml, claim to decide weight, supersound process 60 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, evaporate to dryness adds water 25ml and hydrochloric acid 3ml, chloroform 20ml, reflux 1 hour, put coldly, divide and to get chloroform layer, water layer adds chloroform again and extracts 2 times, each 10ml, combined chloroform liquid, evaporate to dryness, residue add methanol makes dissolving, be settled to 10ml, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Claims (9)
1. a Chinese medicine composition is characterized in that said composition is to be made by the crude drug of following weight ratio: Radix Polygoni Multiflori Preparata 5-15, Radix Rehmanniae Preparata 1-8, Fructus Mori 1-5, Fructus Lycii 1-5, Radix Angelicae Sinensis 1-5, Fructus Psoraleae 1-5, Rhizoma Chuanxiong 1-5, Poria 1-5, Pericarpium Citri Reticulatae 1-4.
2. Chinese medicine composition as claimed in claim 1 is characterized in that the optimum weight ratio of each crude drug is: Radix Polygoni Multiflori Preparata 8, Radix Rehmanniae Preparata 4, Fructus Mori 3, Fructus Lycii 3, Radix Angelicae Sinensis 3, Fructus Psoraleae 3, Rhizoma Chuanxiong 3, Poria 3, Pericarpium Citri Reticulatae 2.
3. Chinese medicine composition as claimed in claim 1 or 2 is characterized in that said composition can make various peroral dosage forms clinical or that pharmacy is required, as oral liquid, tablet, capsule, pill etc.
4. the preparation method of the described Chinese medicine composition of claim 3 is characterized in that this method can be arbitrary in following two methods:
1) get crude drug, decoct with water 1-3 time, add 5-12 times of water gaging at every turn, decocted 0.5-2 hour at every turn, collecting decoction filters, and filtrate was left standstill 8-48 hour, and getting supernatant, to be evaporated to 20 ℃ relative density be 1.36 thick paste, and drying is pulverized, medicated powder; Medicated powder is added proper auxiliary materials, make required dosage form;
2) get Radix Angelicae Sinensis, Fructus Psoraleae, Rhizoma Chuanxiong, Pericarpium Citri Reticulatae and add 4-9 and doubly measure the 30-90% alcohol reflux 1-3 time, each 1-3 hour, filter, it is 1.05～1.30 thick paste that filtrate is concentrated into relative density in the time of 60 ℃, standby; Medicinal residues and Radix Polygoni Multiflori Preparata, Radix Rehmanniae Preparata, Fructus Mori, Fructus Lycii, Poria decoct with water 1-3 time, add 6-12 times of water gaging at every turn, decoct 1-4 hour at every turn, collecting decoction, filter, it is 1.05～1.30 clear paste that filtrate is concentrated into relative density in the time of 60 ℃, adds the ethanol that 1-3 doubly measures, left standstill 8-36 hour, recovery ethanol to the relative density in the time of 60 ℃ is 1.05～1.30 clear paste, merges drying with above-mentioned clear paste, pulverize, get medicated powder; Medicated powder is added suitable adjuvant, make required dosage form.
5. the preparation method of Chinese medicine composition as claimed in claim 4 is characterized in that the technical process after preferred is as follows:
1) gets crude drug, decoct with water 3 times, add 10 times of amounts for the first time, add 8 times of amounts for the second time, add 6 times of amounts for the third time, the each decoction 1 hour, collecting decoction filters, and filtrate was left standstill 24 hours, getting supernatant, to be evaporated to 20 ℃ relative density be 1.36 thick paste, and drying is pulverized, medicine; Medicated powder is added suitable adjuvant, make required dosage form;
2) get Radix Angelicae Sinensis, Fructus Psoraleae, Rhizoma Chuanxiong, Pericarpium Citri Reticulatae and add 6 times of amount 75% alcohol reflux 1 time, 1 hour, filter, it is 1.10～1.20 thick paste that filtrate is concentrated into relative density in the time of 60 ℃, standby; Medicinal residues and Radix Polygoni Multiflori Preparata, Radix Rehmanniae Preparata, Fructus Mori, Fructus Lycii, Poria decoct with water 2 times, add 8 times of water gagings at every turn, decoct 1 hour at every turn, collecting decoction, filter, it is 1.10～1.20 clear paste that filtrate is concentrated into relative density in the time of 60 ℃, adds the ethanol of 2 times of amounts, left standstill 24 hours, recovery ethanol to the relative density in the time of 60 ℃ is 1.10～1.20 clear paste, merges drying with above-mentioned clear paste, pulverize, get medicated powder; Medicated powder is added suitable adjuvant, make required dosage form.
6. as the preparation method of Chinese medicine composition as described in claim 4 or 5, it is characterized in that the preparation method of capsule is: medicated powder is added starch be adjusted to required total amount, mix homogeneously is crossed 20 mesh sieve wet granulations with 70% ethanol, drying, and granulate incapsulates, promptly.
7. the method for quality control of Chinese medicine composition as claimed in claim 1 or 2 is characterized in that discrimination method in this method can be following one or more:
A. it is an amount of to get preparation of the present invention, uses methanol 50ml supersound extraction 30 minutes, filters, get subsequent filtrate 25ml, evaporate to dryness adds water 25ml and hydrochloric acid 3ml, chloroform 20ml, reflux 1 hour is put coldly, divides and to get chloroform layer, water layer adds chloroform again and extracts 2 times, each 10ml, combined chloroform liquid, evaporate to dryness, residue adds methanol makes dissolving, is settled to 10ml, as need testing solution; Other gets Radix Polygoni Multiflori control medicinal material 2g, decocts with water 1 hour, is concentrated in right amount, adds a small amount of kieselguhr mixing, drying, and the same legal system is shone medical material solution in pairs; Get the emodin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned need testing solution 10 μ l, control medicinal material and reference substance solution, put respectively in same and contain on the silica gel g thin-layer plate that 0.3% sodium carboxymethyl cellulose is an adhesive, upper solution with petroleum ether-Ethyl formates of 15: 5: 1-formic acid is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with control medicinal material and the corresponding position of reference substance chromatograph on, show identical orange-yellow fluorescence speckle; Put in the ammonia smoked after, speckle becomes redness;
B. it is an amount of to get preparation of the present invention, and porphyrize adds ethyl acetate 20ml, and supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution; Other gets psoralen, isopsoralen reference substance, adds ethyl acetate and makes the mixed solution that every 1ml contains 2mg, in contrast product solution; According to the thin layer chromatography test, draw above-mentioned need testing solution 10 μ l, reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetates of 4: 1 was developing solvent, launched, and took out, dry, spray is put under the 365nm ultra-violet lamp and is inspected with 10% potassium hydroxide methanol solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical blue and white fluorescence speckle;
C. it is an amount of to get preparation of the present invention, and porphyrize adds methanol 20ml, and supersound process 20 minutes filters, and filtrate is as need testing solution; Other gets the Hesperidin reference substance, adds methanol and makes saturated solution, in contrast product solution; According to the thin layer chromatography test, draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, be developing solvent with methanol, open up about 3cm, spray was placed 3 hours with the methanol solution of 1% aluminum chloride, observed under the 365nm ultra-violet lamp; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D. it is an amount of to get preparation of the present invention, and add water 50ml and make dissolving, with ethyl acetate extraction twice, each 30ml, ethyl acetate liquid is concentrated into 0.5ml, as need testing solution; Other gets Fructus Lycii control medicinal material 5g, adds methanol 10ml and soaks 30 minutes in 50 ℃ of water-baths, filters, and filtrate is medical material solution in contrast; Each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 10: 0.2 chloroform-methanols was developing solvent, launched, and took out, dry, put in the ammonia steam and smoked 30 minutes, under the 365nm ultra-violet lamp, inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
8. the method for quality control of Chinese medicine composition as claimed in claim 7 is characterized in that the content assaying method in this method is as follows:
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Acetonitrile-water-glacial acetic acid of 60: 40: 1 is a mobile phase; The detection wavelength is 437nm; Number of theoretical plate calculates by the emodin peak should be not less than 3000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the emodin reference substance, adds methanol and make the solution that every 1ml contains 4 μ g, promptly;
It is an amount of that preparation of the present invention is got in the preparation of need testing solution, porphyrize, mixing, get 1g, the accurate title, decide, and precision adds methanol 50ml, claim to decide weight, supersound process 60 minutes is put cold, claim to decide weight, supply the weight that subtracts mistake, shake up with methanol, filter, discard filtrate just, precision is measured subsequent filtrate 25ml, evaporate to dryness adds water 25ml and hydrochloric acid 3ml, chloroform 20ml, reflux 1 hour, put coldly, divide and to get chloroform layer, water layer adds chloroform again and extracts 2 times, each 10ml, combined chloroform liquid, evaporate to dryness, residue add methanol makes dissolving, be settled to 10ml, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
9. Chinese medicine composition as claimed in claim 1 or 2 loses the alopecia due to the void, soreness of the waist and knees, the application in the medicine of diseases such as insomnia and dreamful sleep at preparation treatment deficiency of the liver and kindey, essence and blood.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104857155A (en) * | 2015-04-29 | 2015-08-26 | 安徽信灵检验医学科技有限公司 | Health care formula for improving sleep quality |
| CN109613166A (en) * | 2019-01-16 | 2019-04-12 | 鲁南制药集团股份有限公司 | A kind of head luxuriant growth Tongbian capsule quality determining method |
| CN110187046A (en) * | 2019-06-12 | 2019-08-30 | 贵州联盛药业有限公司 | The thin layer of fructus lycii, aurantiin and icariin identifies measuring method in Shengjing tablet for invigoration |
| CN110763642A (en) * | 2018-07-27 | 2020-02-07 | 九芝堂股份有限公司 | Detection method of traditional Chinese medicine preparation |
| CN115252698A (en) * | 2022-08-30 | 2022-11-01 | 乐泰药业有限公司 | A Chinese medicinal composition for treating alopecia and premature gray hair due to liver and kidney deficiency, and its preparation method and content control method |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1215871C (en) * | 2003-08-04 | 2005-08-24 | 刘泊言 | Species and liniment for treating alopecia areata, seborrheic alpoecia and nervoalopecia |
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2005
- 2005-06-27 CN CN200510200353A patent/CN1887324B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104857155A (en) * | 2015-04-29 | 2015-08-26 | 安徽信灵检验医学科技有限公司 | Health care formula for improving sleep quality |
| CN110763642A (en) * | 2018-07-27 | 2020-02-07 | 九芝堂股份有限公司 | Detection method of traditional Chinese medicine preparation |
| CN110763642B (en) * | 2018-07-27 | 2023-07-07 | 九芝堂股份有限公司 | Detection method of traditional Chinese medicine preparation |
| CN109613166A (en) * | 2019-01-16 | 2019-04-12 | 鲁南制药集团股份有限公司 | A kind of head luxuriant growth Tongbian capsule quality determining method |
| CN110187046A (en) * | 2019-06-12 | 2019-08-30 | 贵州联盛药业有限公司 | The thin layer of fructus lycii, aurantiin and icariin identifies measuring method in Shengjing tablet for invigoration |
| CN110187046B (en) * | 2019-06-12 | 2021-08-17 | 贵州联盛药业有限公司 | Thin-layer identification and determination method for barbary wolfberry fruit, naringin and icariin in Shengjing tablets |
| CN115252698A (en) * | 2022-08-30 | 2022-11-01 | 乐泰药业有限公司 | A Chinese medicinal composition for treating alopecia and premature gray hair due to liver and kidney deficiency, and its preparation method and content control method |
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| CN1887324B (en) | 2010-05-12 |
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