CN1806846A - Chinese medicinal composition, its preparation process and quality control method - Google Patents
Chinese medicinal composition, its preparation process and quality control method Download PDFInfo
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- CN1806846A CN1806846A CNA2005102000420A CN200510200042A CN1806846A CN 1806846 A CN1806846 A CN 1806846A CN A2005102000420 A CNA2005102000420 A CN A2005102000420A CN 200510200042 A CN200510200042 A CN 200510200042A CN 1806846 A CN1806846 A CN 1806846A
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Abstract
The invention discloses a Chinese medicinal composition prepared from root of red rooted saliva, Ligusticum wallichii, kudzu vine root, earthworm, radix paeoniae rubrathe, safflower, curcuma aromatica, fleece-flower root, oriental water plantain rhizome, matrimony vine, wild jujuba seeds, polygala root, anemone rhizome, achyranthes and licorice root. The composition can be used for treating cardiovascular and cerebrovascular diseases. The invention discloses the method for preparing the medicinal composition and its quality control method.
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
Cardiovascular and cerebrovascular disease is modern society's serious threat human health, and severe patient causes dead principal disease.Be clinical common frdquently encountered disease, with qi depression to blood stasis, the turbid resistance network of expectorant disease sees that disease is seen palpitation and uneasiness more, discomfort uncomfortable in chest, stabbing pain over the chest, angor are fixed and are not moved, and go into Night Watch very, dizzy headache, coronary heart disease, myocardial infarction, cerebral arteriosclerosis, cerebral thrombosis etc. are seen above-mentioned syndrome more, and therefore, it is very necessary to explore a kind of medicine for the treatment of such disease.
Summary of the invention
The purpose of this invention is to provide a kind of preparation treatment qi depression to blood stasis, Chinese medicine composition of using in the turbid resistance network card of the expectorant medicine and preparation method thereof; The present invention also aims to provide a kind of method of quality control of Chinese medicine composition.
The present invention seeks to be achieved through the following technical solutions:
At first, the inventor has formulated a kind of Chinese medicine composition, and said composition is made by following bulk drugs:
Radix Salviae Miltiorrhizae 30-50 part Rhizoma Chuanxiong 20-40 part Radix Puerariae 20-40 part Pheretima 20-40 part
Radix Paeoniae Rubra 20-40 part Flos Carthami 10-30 part Radix Curcumae 2-4 part Radix Polygoni Multiflori 20-40 part
Rhizoma Alismatis 20-40 part Fructus Lycii 20-40 part Semen Ziziphi Spinosae 20-40 part Radix Polygalae 20-40 part
Rhizoma Anemones Altaicae 20-40 part Radix Achyranthis Bidentatae 20-40 part Radix Glycyrrhizae 10-30 part
Definitely, the weight ratio of each crude drug is
30 parts of 30 parts of Pheretimas of 30 parts of Radix Puerariaes of 40 parts of Rhizoma Chuanxiongs of Radix Salviae Miltiorrhizae
30 parts of 3 parts of Radix Polygoni Multiflori of 20 portions of Radix Curcumaes of 30 parts of Flos Carthamis of Radix Paeoniae Rubra
30 parts of 30 parts of Radix Polygalaes of 30 parts of Semen Ziziphi Spinosaes of 30 portions of Fructus Lyciis of Rhizoma Alismatis
20 parts in 30 portions of Radix Glycyrrhizaes of 30 parts of Radix Achyranthis Bidentataes of Rhizoma Anemones Altaicae
And the Radix Polygoni Multiflori in the prescription, Semen Ziziphi Spinosae are preferably Radix Polygoni Multiflori Preparata and Semen Ziziphi Spinosae (parched).
According to characteristics of prescriptions, the inventor thinks and this crude drug can be made modern solid preparation, is preferably tablet and pill; For this reason, the inventor has formulated preparation technology, comprising extracting refining and preparations shaping two parts.
Extract FF, the inventor has designed three kinds of schemes, all can reach goal of the invention, is described below respectively:
1) will write out a prescription in Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima decoct with water three times, gradation filters, merging filtrate is condensed into thick paste, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, add in the fluid extract, stir, drying, dried cream powder is broken into fine powder;
2) will write out a prescription in Rhizoma Chuanxiong, Flos Carthami, Radix Curcumae, Rhizoma Alismatis, Rhizoma Anemones Altaicae be ground into fine powder, standby; All the other medical materials decoct with water three times, and gradation filters, and merging filtrate concentrates the thick paste shape, and is standby; Get the said medicine fine powder, add in the thick paste, stir, drying, dried cream powder is broken into fine powder;
3) will write out a prescription in Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima decoct with water three times, be respectively 3 hours, 2 hours and 1 hour at every turn, gradation filters, merging filtrate, concentrating under reduced pressure becomes flowing soaking paste, cold drying is ground into fine powder, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, add in the dried cream powder, mix homogeneously, the extract fine powder.
The preparations shaping part, relatively simple, promptly need choose suitable adjuvant, mix with extraction gained fine powder, make corresponding dosage form, comprise tablet and pill.
In order effectively to control the quality of gained preparation of the present invention, the inventor has also formulated method of quality control, comprises qualitative identification and assay two parts, one or more that qualitative identification wherein can be following:
A. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml merges ether solution, adds 5% sodium bicarbonate 20ml washing once, discard, ether solution volatilizes, and residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, the 20ml that adds diethyl ether, and reflux 1 hour is put coldly, filters, and volatilizes ether solution, and residue adds dehydrated alcohol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography, drawing need testing solution 5 μ l, control medicinal material solution 2 μ l puts respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (12: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
B. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml gets the water liquid after the extracted with diethyl ether, with ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, add 5% sodium bicarbonate 20ml washing once, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the puerarin reference substance, adds methanol and makes the solution that every 1ml contains the 0.05mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-methanol-water (7: 2: 0.25), launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml gets the water liquid after the extracted with diethyl ether, with ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, add 5% sodium bicarbonate 20ml washing once, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the stilbene glucoside reference substance, adds methanol and makes the solution that every ml contains the 0.2mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-acetone-methanol (6: 1: 2), launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
D. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, with ether, ethyl acetate extraction three times, ether solution, ethyl acetate liquid discard respectively, and surplus water liquid is with water saturated n-butanol extraction three times, each 20ml merges n-butyl alcohol liquid, with ammonia solution washing three times, each 20ml discards the ammonia washing liquid, n-butyl alcohol liquid evaporate to dryness, residue adds ethanol 2ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds methanol and makes the solution that every 1ml contains the 0.5mg reference substance, in contrast product solution.Test according to thin layer chromatography, draw reference substance solution 3 μ l, need testing solution 10 μ l respectively, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% vanillin, 105 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the speckle that shows same color on the corresponding position of reference substance chromatograph.
E. get present composition preparation 2～5g, porphyrize adds methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, the extracted with diethyl ether secondary, each 20ml discards ether solution, and water liquid adds hydrochloric acid 2ml, and boiling water bath refluxed 1 hour, put cold, extracted with diethyl ether three times, each 20ml merges ether solution, with 5% sodium bicarbonate washing three times, each 30ml discards, ether solution volatilizes, and residue adds methanol 1ml makes dissolving, as need testing solution; It is an amount of that other evens up pier fruit acid reference substance, adds dissolve with methanol, makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw each 5 μ l of need testing solution and reference substance solution, put on same silica gel g thin-layer plate respectively, with cyclohexane extraction-chloroform-ethyl acetate-methanol-formic acid (20: 4: 4: 2: 1) upper strata is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire under 80 ℃ to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color
F. get present composition preparation 2～5g, porphyrize adds methanol 50ml, supersound extraction 30 minutes filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, and water liquid adds hydrochloric acid 2ml, chloroform 20ml, boiling water bath refluxed 1 hour, put coldly, discard chloroform solution, water liquid washs secondary with chloroform, each 20ml discards chloroform solution; Ethyl acetate extraction three times of water liquid, each 20ml merges, with 5% sodium carbonate liquor extraction three times, each 20ml merges sodium carbonate liquid, transfers pH2～3 with hydrochloric acid, reuse ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, volatilizes, residue dehydrated alcohol 5ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 2g in addition, according to the preparation method of need testing solution, the control medicinal material solution of system; According to the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (10: 1: 0.1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, hot blast drying.Put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Content assaying method can be following a kind of or two kinds:
A. the assay of danshensu sodium in the Radix Salviae Miltiorrhizae
Chromatographic condition and system suitability test are filler with octadecyl silane; Methanol-0.5% glacial acetic acid solution (5: 95) is a mobile phase; The detection wavelength is 280nm, and theoretical cam curve should be not less than 2000 by the danshensu peak.
It is an amount of that the danshensu sodium reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 50 μ g, promptly.
Present composition preparation 2g is got in the preparation of need testing solution, and accurate the title decides, and puts in the conical flask, the accurate 1% aqueous hydrochloric acid solution 50ml that adds claims to decide weight, 30 minutes (100W of supersound extraction, 50kHz), be cooled to room temperature, claim to decide weight, supply the weight that subtracts mistake with 1% aqueous hydrochloric acid solution, shake up, filter, get subsequent filtrate 10ml, add sodium chloride 1g dissolving, use ethyl acetate extraction four times, each 15ml, merge ethyl acetate liquid, volatilize, residue dissolves with mobile phase, and quantitatively is transferred in the 5ml measuring bottle, add mobile phase to scale, shake up, filter with microporous filter membrane (0.45 μ m), promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly.
B. content of puerarin is measured in the Radix Puerariae
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (12: 88) is a mobile phase, and flow velocity is 1.0ml/min, 40 ℃ of column temperatures.Detect wavelength 250nm.Number of theoretical plate calculates by puerarin peak should be not less than 4000.
The preparation precision of reference substance solution takes by weighing the puerarin reference substance that is dried to constant weight in right amount with phosphorus pentoxide, makes the solution that every 1ml contains 20 μ g with methanol, shakes up, promptly.
The about 0.5g of present composition preparation is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug triangular flask, precision adds 50% methanol 50ml, claims to decide weight, ultrasonic (250W, 50kHz) handle 30 minutes, put coldly, claim to decide weight again, supply the weight of loss with 50% methanol, shake up, leave standstill, get supernatant, filter with microporous filter membrane, as need testing solution.
Accurate respectively reference substance and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The specific embodiment:
Pharmaceutical preparation of the present invention has the QI invigorating row and stagnates blood circulation promoting and blood stasis dispelling, suppressing the hyperactive liver and subsiding YANG, the function of reinforcement and elimination in combination.The inventor cures mainly according to its function, from aspects such as coronary blood flow increasing, anticoagulants its pharmacodynamics is studied.
Be subjected to the reagent thing: the sharp brain heart sheet that makes respectively according to three kinds of preparation methoies of the present invention 1-3 number contains 0.55g crude drug/sheet.
YIMAIKANG PIAN: Kunming Sainuo Pharmaceutical Co., Ltd. produces, lot number: 20040101.
Instrument: computer platelet aggregation instrument (KD-200A), PB303-N electronic balance, Mettler-Toledo Instrument (Shanghai) Co., Ltd., centrifuge.
Animal: WistarSD rat male and female half and half, 200～250g; White rabbit male and female half and half, 1.9～2.0kg provides by new drug research center animal housing of China Medicine University.
Test 1: to the influence of coronary flow
Get 50 of Wistar rats, be divided into 5 groups at random, 10 every group, after pentobarbital sodium is pressed the anesthesia of 30mg/kg dosage, take out heart and put in 4 ℃ of perfusates, after heart stops to beat, make the Blangendorff specimen immediately.After treating the heartbeating recovery balance, prop up administration 0.2ml, coronary flow and the heart rate of record administration front and back 1,3,10min from the aorta side.See Table 1.
| Group | Before the administration (ml/min) | After the administration (ml/min) | X±s |
| Model control group | 7.0±0.07 | 7.1±0.07 | 101±5 |
| Organized by reagent thing I | 6.7±1.5 | 9.3±2 | 137±23 |
| Organized by reagent thing II | 6.7±1.6 | 9.5±1.7 | 136±20 |
| Organized by reagent thing III | 6.8±1.5 | 9.3±1.3 | 136±16 |
| The positive drug group | 6.7±1.4 | 9.1±2 | 135±11 |
Annotate: compare * P＜0.05, * * P＜0.01, * * * P＜0.001 with model control group.(down together)
Table 1 is the result show, isolated rat aorta side is propped up obviously coronary blood flow increasing of administration.
Experiment 2: to inductive rabbit platelet aggregation of ADP and clotting time influence
2.1 the rabbit extracorporeal platelet aggregation is influenced
Get 2 of rabbit, ♂, heart extracting blood under the waking state, 3.8% liquor sodii citratis (9: 1) anticoagulant.Centrifugal (600r/min) 8min gets turbid liquid platelet rich plasma (PRP), and remainder centrifugal again (3000r/min) 15min gets supernatant platelet poor plasma (PPP).The accurate title, decided ADP, is mixed with 40 μ m with the pH7.4 phosphate buffered solution, as derivant.Add PRP 25 μ l in opacity tube, accurately adding is subjected to reagent thing 50 μ l again, hatches 10min in 37 ℃ of water-baths.Accurately add ADP 40 μ m (making the ADP final concentration is 5 μ m), on KD-200A computer platelet aggregation instrument, measure tame Sanguis Leporis seu oryctolagi platelet aggregation rate (1min aggregation rate and 5min maximum agglutination rate).See Table 2.
Table 2 pair rabbit extracorporeal platelet aggregation influence (X ± s, n=10)
| Group | A(1)％ | A(max)％ |
| Model control group | 4.66±0.32 | 6.22±0.26 |
| Organized by reagent thing I | 2.59±1.26 | 8.61±1.48 |
| Organized by reagent thing II | 2.86±1.68 | 7.44±0.84 |
| Organized by reagent thing III | 3.01±1.245 | 8.63±2.01 |
| The positive drug group | 3.11±1.01 | 7.92±1.31 |
Table 2 is the result show, each administration group is compared with model control group, all the inductive platelet aggregation of ADP had significant inhibitory effect.
2.2 influence to external thrombin time (TT)
Get 1 of rabbit, ♂, carotid artery blood-letting under the waking state, 3.8% liquor sodii citratis (9: 1) anticoagulant.Centrifugal (3000r/min) 1Omin, it is stand-by to get supernatant blood plasma.Get the clean tube of silication, add 200 μ l medicines and 0.5ml blood plasma respectively, hatch 2min in 37 ℃ of water-baths, add temperature 37 in advance rapidly.The thrombin solution 1ml of C puts into 37 ℃ of water-bath incubations immediately behind the mixing, pick up counting simultaneously.Every 2～3s inclination test tube 1 time, the record fibrin solidifies, the motionless gained time of liquid level, obtains every pipe meansigma methods.See Table 3.
The influence of table 3 couple external TT (X ± s, n=10)
| Group | TT |
| Model control group | 11.36±0.54 |
| Organized by reagent thing I | 19.64±0.86 |
| Organized by reagent thing II | 18.38±1.68 |
| Organized by reagent thing III | 18.19±1.10 |
| The positive drug group | 19.68±0.81 |
Table 3 is the result show, respectively compares with model control group to the Ji group, all can prolong the rabbit TT time.
Test 3: acute toxicity test
Give mouse stomach drug extract 50g/kg of the present invention in one day, be equivalent to more than 700 times of clinical 70kg people's per kilogram of body weight consumption per day, observed continuously seven days, mice generally in order, none death illustrates this product low toxicity, safety.
Further specify technical scheme of the present invention by the following examples.
Embodiment one
[prescription] Radix Salviae Miltiorrhizae 30g Rhizoma Chuanxiong 20g Radix Puerariae 20g Pheretima 20g
Radix Paeoniae Rubra 20g Flos Carthami 10g Radix Curcumae 2g Radix Polygoni Multiflori Preparata 20g
Rhizoma Alismatis 20g Fructus Lycii 20g Semen Ziziphi Spinosae (stir-fry) 20g Radix Polygalae 20g Rhizoma Anemones Altaicae 20g Radix Achyranthis Bidentatae 20g Radix Glycyrrhizae 10g
[method for making] above ten five tastes decoct with water Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima three times, and gradation filters, and merging filtrate is condensed into thick paste, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, add in the fluid extract, stir, drying, dried cream powder is broken into fine powder, adds 1% carboxymethylstach sodium and microcrystalline Cellulose and adjusts total amount in right amount to 500g, mixing adds 30% ethanol and makes wetting agent, mix homogeneously, close and stick together 20 minutes, pill bar, gradation and round, pill polishing, cold drying, packing, promptly.
Embodiment two
[prescription] Radix Salviae Miltiorrhizae 40g Rhizoma Chuanxiong 30g Radix Puerariae 30g Pheretima 30g
Radix Paeoniae Rubra 30g Flos Carthami 20g Radix Curcumae 3g Radix Polygoni Multiflori Preparata 30g
Rhizoma Alismatis 30g Fructus Lycii 30g Semen Ziziphi Spinosae (stir-fry) 30g Radix Polygalae 30g
Rhizoma Anemones Altaicae 30g Radix Achyranthis Bidentatae 30g Radix Glycyrrhizae 20g
[method for making] above ten five tastes add 8 times of water gagings with Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima and decoct three times (3 hours, 2 hours, 1 hour), and gradation filters, and merging filtrate is evaporated to the fluid extract of relative density, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, cross 100 mesh sieves, add in the fluid extract, stir, drying under reduced pressure, dried cream powder is broken into fine powder, add carboxymethylstach sodium 5g, microcrystalline Cellulose 30g, ethanol moistening with 60%, cross 16 mesh sieve system granules, dry below 60 ℃, add magnesium stearate 2g, starch is regulated total amount in right amount to 290g, is pressed into 750, the bag film-coat, packing, promptly.
Embodiment three
[prescription] Radix Salviae Miltiorrhizae 50g Rhizoma Chuanxiong 40g Radix Puerariae 40g Pheretima 40g
Radix Paeoniae Rubra 40g Flos Carthami 30g Radix Curcumae 4g Radix Polygoni Multiflori Preparata 40g
Rhizoma Alismatis 40g Fructus Lycii 40g Semen Ziziphi Spinosae (stir-fry) 40g Radix Polygalae 40g
Rhizoma Anemones Altaicae 40g Radix Achyranthis Bidentatae 40g Radix Glycyrrhizae 30g
[method for making] above ten five tastes add 8 times of water gagings with Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima and decoct three times (3 hours, 2 hours, 1 hour), and gradation filters, and merging filtrate is evaporated to the fluid extract of relative density, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, cross 100 mesh sieves, add in the fluid extract, stir, drying under reduced pressure, dried cream powder is broken into fine powder, add carboxymethylstach sodium 5g, microcrystalline Cellulose 30g, ethanol moistening with 60%, cross 16 mesh sieve system granules, dry below 60 ℃, add magnesium stearate 2g, starch is regulated total amount in right amount to 290g, is pressed into 750, the bag film-coat, packing, promptly.
Method of quality control to above-mentioned tablet:
Differentiate:
A. get present composition preparation 4g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml merges ether solution, adds 5% sodium bicarbonate 20ml washing once, discard, ether solution wave in, residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, the 20ml that adds diethyl ether, and reflux 1 hour is put coldly, filters, and volatilizes ether solution, and residue adds dehydrated alcohol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography, drawing need testing solution 5 μ l, control medicinal material solution 2 μ l puts respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetate (12: 1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
B. get present composition preparation 4g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml gets the water liquid after the extracted with diethyl ether, with ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, add 5% sodium bicarbonate 20ml washing once, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the puerarin reference substance, adds methanol and makes the solution that every 1ml contains the 0.05mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-methanol-water (7: 2: 0.25), launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
C. get present composition preparation 4g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml gets the water liquid after the extracted with diethyl ether, with ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, add 5% sodium bicarbonate 20ml washing once, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the stilbene glucoside reference substance, adds methanol and makes the solution that every ml contains the 0.2mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-acetone-methanol (6: 1: 2), launches, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
D. get present composition preparation 4g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, with ether, ethyl acetate extraction three times, ether solution, ethyl acetate liquid discard respectively, and surplus water liquid is with water saturated n-butanol extraction three times, each 20ml merges n-butyl alcohol liquid, with ammonia solution washing three times, each 20ml discards the ammonia washing liquid, n-butyl alcohol liquid evaporate to dryness, residue adds ethanol 2ml makes dissolving, as need testing solution.Other gets the peoniflorin reference substance, adds methanol and makes the solution that every 1ml contains the 0.5mg reference substance, in contrast product solution.Test according to thin layer chromatography, draw reference substance solution 3 μ l, need testing solution 10 μ l respectively, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-formic acid (40: 5: 10: 0.2) be developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% vanillin, 105 ℃ dry by the fire to the speckle colour developing clear.In the test sample chromatograph, with the speckle that shows same color on the corresponding position of reference substance chromatograph.
E. get present composition preparation 4g, porphyrize adds methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, the extracted with diethyl ether secondary, each 20ml discards ether solution, and water liquid adds hydrochloric acid 2ml, and boiling water bath refluxed 1 hour, put cold, extracted with diethyl ether three times, each 20ml merges ether solution, with 5% sodium bicarbonate washing three times, each 30ml discards, ether solution volatilizes, and residue adds methanol 1ml makes dissolving, as need testing solution; It is an amount of that other evens up pier fruit acid reference substance, adds dissolve with methanol, makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography, draw each 5 μ l of need testing solution and reference substance solution, put on same silica gel g thin-layer plate respectively, with cyclohexane extraction-chloroform-ethyl acetate-methanol-formic acid (20: 4: 4: 2: 1) upper strata is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire under 80 ℃ to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
F. get present composition preparation 4g, porphyrize adds methanol 50ml, supersound extraction 30 minutes filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, and water liquid adds hydrochloric acid 2ml, chloroform 20ml, boiling water bath refluxed 1 hour, put coldly, discard chloroform solution, water liquid washs secondary with chloroform, each 20ml discards chloroform solution; Ethyl acetate extraction three times of water liquid, each 20ml merges, with 5% sodium carbonate liquor extraction three times, each 20ml merges sodium carbonate liquid, transfers pH2 ~ 3 with hydrochloric acid, reuse ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, volatilizes, residue dehydrated alcohol 5ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 2g in addition, according to the preparation method of need testing solution, the control medicinal material solution of system; According to the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (10: 1: 0.1) is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, hot blast drying.Put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Assay:
A. the assay of danshensu sodium in the Radix Salviae Miltiorrhizae
Chromatographic condition and system suitability test are filler with octadecyl silane; Methanol-0.5% glacial acetic acid solution (5: 95) is a mobile phase; The detection wavelength is 280nm, and theoretical cam curve should be not less than 2000 by the danshensu peak.
It is an amount of that the danshensu sodium reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 50 μ g, promptly.
Present composition preparation 2g is got in the preparation of need testing solution, and accurate the title decides, and puts in the conical flask, the accurate 1% aqueous hydrochloric acid solution 50ml that adds claims to decide weight, 30 minutes (100W of supersound extraction, 50kHz), be cooled to room temperature, claim to decide weight, supply the weight that subtracts mistake with 1% aqueous hydrochloric acid solution, shake up, filter, get subsequent filtrate 10ml, add sodium chloride 1g dissolving, use ethyl acetate extraction four times, each 15ml, merge ethyl acetate liquid, volatilize, residue dissolves with mobile phase, and quantitatively is transferred in the 5ml measuring bottle, add mobile phase to scale, shake up, filter with microporous filter membrane (0.45 μ m), promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly.
Every of this product contains Radix Salviae Miltiorrhizae with danshensu (C
9H
10O
5) meter, must not be less than 0.10mg.
B. content of puerarin is measured in the Radix Puerariae
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (12: 88) is a mobile phase, and flow velocity is 1.0ml/min, 40 ℃ of column temperatures.Detect wavelength 250nm.Number of theoretical plate calculates by puerarin peak should be not less than 4000.
The preparation precision of reference substance solution takes by weighing the puerarin reference substance that is dried to constant weight in right amount with phosphorus pentoxide, makes the solution that every 1ml contains 20 μ g with methanol, shakes up, promptly.
The about 0.5g of present composition preparation is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug triangular flask, precision adds 50% methanol 50ml, claims to decide weight, ultrasonic (250W, 50kHz) handle 30 minutes, put coldly, claim to decide weight again, supply the weight of loss with 50% methanol, shake up, leave standstill, get supernatant, filter with microporous filter membrane, as need testing solution.
Accurate respectively reference substance and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Puerariae with puerarin (C
21H
20O
9) meter, must not be less than 0.58mg.
Claims (9)
1. Chinese medicine composition is characterized in that said composition is to be made by the raw material of following weight portion:
Radix Salviae Miltiorrhizae 30-50 part Rhizoma Chuanxiong 20-40 part Radix Puerariae 20-40 part Pheretima 20-40 part
Radix Paeoniae Rubra 20-40 part Flos Carthami 10-30 part Radix Curcumae 2-4 part Radix Polygoni Multiflori 20-40 part
Rhizoma Alismatis 20-40 part Fructus Lycii 20-40 part Semen Ziziphi Spinosae 20-40 part Radix Polygalae 20-40 part
Rhizoma Anemones Altaicae 20-40 part Radix Achyranthis Bidentatae 20-40 part Radix Glycyrrhizae 10-30 part
2. Chinese medicine composition as claimed in claim 1 is characterized in that this Chinese medicine composition is to be made by the raw material of following weight portion:
30 parts of 30 parts of Pheretimas of 30 parts of Radix Puerariaes of 40 parts of Rhizoma Chuanxiongs of Radix Salviae Miltiorrhizae
30 parts of 3 parts of Radix Polygoni Multiflori of 20 portions of Radix Curcumaes of 30 parts of Flos Carthamis of Radix Paeoniae Rubra
30 parts of 30 parts of Radix Polygalaes of 30 parts of Semen Ziziphi Spinosaes of 30 portions of Fructus Lyciis of Rhizoma Alismatis
20 parts in 30 portions of Radix Glycyrrhizaes of 30 parts of Radix Achyranthis Bidentataes of Rhizoma Anemones Altaicae
3. Chinese medicine composition as claimed in claim 1 or 2 is characterized in that the Semen Ziziphi Spinosae in the crude drug is a Semen Ziziphi Spinosae (parched), and Radix Polygoni Multiflori is a Radix Polygoni Multiflori Preparata.
4. Chinese medicine composition as claimed in claim 3 is characterized in that said composition can be prepared into pill and tablet.
5. the preparation method of the described Chinese medicine composition of claim 4 is characterized in that during the method includes the steps of any:
1) will write out a prescription in Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima decoct with water three times, gradation filters, merging filtrate is condensed into thick paste, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, add in the fluid extract, stir, drying, dried cream powder is broken into fine powder;
2) will write out a prescription in Rhizoma Chuanxiong, Flos Carthami, Radix Curcumae, Rhizoma Alismatis, Rhizoma Anemones Altaicae be ground into fine powder, standby; All the other medical materials decoct with water three times, and gradation filters, and merging filtrate concentrates the thick paste shape, and is standby; Get the said medicine fine powder, add in the thick paste, stir, drying, dried cream powder is broken into fine powder;
3) will write out a prescription in Radix Salviae Miltiorrhizae, Radix Polygoni Multiflori, Fructus Lycii, Radix Paeoniae Rubra, Radix Puerariae, Pheretima decoct with water three times, be respectively 3 hours, 2 hours and 1 hour at every turn, gradation filters, merging filtrate, concentrating under reduced pressure becomes flowing soaking paste, cold drying is ground into fine powder, and is standby; Get nine flavors such as Rhizoma Chuanxiong and be ground into fine powder, add in the dried cream powder, mix homogeneously, the extract fine powder.
6. the preparation method of Chinese medicine composition as claimed in claim 5 is characterized in that the fine powder that any method obtains is added conventional adjuvant, makes tablet or pill.
7. the method for quality control of the described Chinese medicine composition of claim 3 is characterized in that qualitative identification method in this method comprises following one or more:
A. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml merges ether solution, adds 5% sodium bicarbonate 20ml washing once, discard, ether solution volatilizes, and residue adds dehydrated alcohol 2ml makes dissolving, as need testing solution; Other gets Rhizoma Chuanxiong control medicinal material 1g, the 20ml that adds diethyl ether, and reflux 1 hour is put coldly, filters, and volatilizes ether solution, and residue adds dehydrated alcohol 2ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography, drawing need testing solution 5 μ l, control medicinal material solution 2 μ l puts respectively on same silica gel g thin-layer plate, with cyclohexane extraction-ethyl acetates of 12: 1 was developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
B. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml gets the water liquid after the extracted with diethyl ether, with ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, add 5% sodium bicarbonate 20ml washing once, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the puerarin reference substance, adds methanol and makes the solution that every 1ml contains the 0.05mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-methanol-water of 7: 2: 0.25, launches, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
C. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, extracted with diethyl ether three times, each 20ml gets the water liquid after the extracted with diethyl ether, with ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, add 5% sodium bicarbonate 20ml washing once, evaporate to dryness, residue add methanol 5ml makes dissolving, as need testing solution; Other gets the stilbene glucoside reference substance, adds methanol and makes the solution that every ml contains the 0.2mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with benzene-acetone of 6: 1: 2-methanol, launches, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
D. get present composition preparation 2～5g, add methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 15ml makes dissolving, with ether, ethyl acetate extraction three times, ether solution, ethyl acetate liquid discard respectively, and surplus water liquid is with water saturated n-butanol extraction three times, each 20ml merges n-butyl alcohol liquid, with ammonia solution washing three times, each 20ml discards the ammonia washing liquid, n-butyl alcohol liquid evaporate to dryness, residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the peoniflorin reference substance, adds methanol and makes the solution that every 1ml contains the 0.5mg reference substance, in contrast product solution; Test according to thin layer chromatography, draw reference substance solution 3 μ l, need testing solution 10 μ l respectively, put respectively on same silica gel g thin-layer plate, with 40: 5: 10: chloroform-ethyl acetate of 0.2-methanol-formic acid was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid of 5% vanillin, 105 ℃ dry by the fire to the speckle colour developing clear; In the test sample chromatograph, with the speckle that shows same color on the corresponding position of reference substance chromatograph;
E. get present composition preparation 2～5g, porphyrize adds methanol 50ml, supersound extraction 30 minutes, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, the extracted with diethyl ether secondary, each 20ml discards ether solution, and water liquid adds hydrochloric acid 2ml, and boiling water bath refluxed 1 hour, put cold, extracted with diethyl ether three times, each 20ml merges ether solution, with 5% sodium bicarbonate washing three times, each 30ml discards, ether solution volatilizes, and residue adds methanol 1ml makes dissolving, as need testing solution; It is an amount of that other evens up pier fruit acid reference substance, adds dissolve with methanol, makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 5 μ l of need testing solution and reference substance solution, put on same silica gel g thin-layer plate respectively, with 20: 4: 4: cyclohexane extraction-chloroform of 2: 1-ethyl acetate-methanol-formic acid upper strata was developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire under 80 ℃ to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
F. get present composition preparation 2～5g, porphyrize adds methanol 50ml, supersound extraction 30 minutes filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, and water liquid adds hydrochloric acid 2ml, chloroform 20ml, boiling water bath refluxed 1 hour, put coldly, discard chloroform solution, water liquid washs secondary with chloroform, each 20ml discards chloroform solution; Ethyl acetate extraction three times of water liquid, each 20ml merges, with 5% sodium carbonate liquor extraction three times, each 20ml merges sodium carbonate liquid, transfers pH 2～3 with hydrochloric acid, reuse ethyl acetate extraction three times, each 20ml merges ethyl acetate liquid, volatilizes, residue dehydrated alcohol 5ml makes dissolving, as need testing solution; Extracting liquorice control medicinal material 2g in addition, according to the preparation method of need testing solution, the control medicinal material solution of system; According to the thin layer chromatography test, draw need testing solution 10 μ l, control medicinal material solution 2 μ l put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water of 10: 1: 0.1 was developing solvent, launched, and took out, dry, spray is with 10% ethanol solution of sulfuric acid, hot blast drying; Put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
8. the method for quality control of Chinese medicine composition as claimed in claim 7 is characterized in that comprising in this method one or more of following quantitative approach:
A. the assay of danshensu sodium in the Radix Salviae Miltiorrhizae
Chromatographic condition and system suitability test are filler with octadecyl silane; 5: 95 methanol-0.5% glacial acetic acid solution is a mobile phase; The detection wavelength is 280nm, and theoretical cam curve should be not less than 2000 by the danshensu peak;
It is an amount of that the danshensu sodium reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds mobile phase and makes the solution that every 1ml contains 50 μ g, promptly;
Present composition preparation 2g is got in the preparation of need testing solution, and accurate the title decides, and puts in the conical flask, the accurate 1% aqueous hydrochloric acid solution 50ml that adds claims to decide weight, supersound extraction 30 minutes, be cooled to room temperature, claim to decide weight, supply the weight that subtracts mistake with 1% aqueous hydrochloric acid solution, shake up, filter, get subsequent filtrate 10ml, add sodium chloride 1g dissolving, with ethyl acetate extraction four times, each 15ml merges ethyl acetate liquid, volatilizes, residue dissolves with mobile phase, and quantitatively be transferred in the 5ml measuring bottle, add mobile phase to scale, shake up, filter with 0.45 μ m microporous filter membrane, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject high performance liquid chromatograph, measure, promptly;
B. content of puerarin is measured in the Radix Puerariae
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; 12: 88 methanol-water is a mobile phase, and flow velocity is 1.0ml/min, 40 ℃ of column temperatures.Detect wavelength 250nm; Number of theoretical plate calculates by puerarin peak should be not less than 4000;
The preparation precision of reference substance solution takes by weighing the puerarin reference substance that is dried to constant weight in right amount with phosphorus pentoxide, makes the solution that every 1ml contains 20 μ g with methanol, shakes up, promptly;
The about 0.5g of present composition preparation is got in the preparation of need testing solution, and accurate the title decides, and puts in the tool plug triangular flask, precision adds 50% methanol 50ml, claims to decide weight, supersound process 30 minutes, put cold, claim to decide weight again, supply the weight of loss, shake up with 50% methanol, leave standstill, get supernatant, filter with microporous filter membrane, as need testing solution;
Accurate respectively reference substance and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
9. as claim 1, the application of 2 or 3 described Chinese medicine compositions in the medicine of diseases such as preparation treatment coronary heart disease, myocardial infarction, cerebral arteriosclerosis and cerebral thrombosis.
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