CN1846762A - Medicine composition for treating coronary heart disease and its prepn process - Google Patents
Medicine composition for treating coronary heart disease and its prepn process Download PDFInfo
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- CN1846762A CN1846762A CN 200610058112 CN200610058112A CN1846762A CN 1846762 A CN1846762 A CN 1846762A CN 200610058112 CN200610058112 CN 200610058112 CN 200610058112 A CN200610058112 A CN 200610058112A CN 1846762 A CN1846762 A CN 1846762A
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- fructus schisandrae
- chloroform
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- 208000029078 coronary artery disease Diseases 0.000 title claims abstract description 16
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Abstract
The present invention discloses one kind of Chinese medicine composition for treating coronary heart disease and its preparation process. The Chinese medicine composition is prepared with the Chinese medicinal materials, including astragalus root, Dangshen, ophiopogon root, schisandra and southern schisandra. The preparation process includes water extracting, filtering, centrifuging, decompression concentrating, adding dextrin, drying, adding pharmaceutically acceptable excipient and other steps to prepare granule, capsule, dripping pill, tablet, slow releasing preparation, oral liquid or injection powder. The present invention also provides the quality control method for the Chinese medicine composition preparing process and the usage of the Chinese medicine composition.
Description
Invention field
The present invention relates to a kind of pharmaceutical composition and preparation method thereof and method of quality control, particularly a kind of pharmaceutical composition for the treatment of coronary heart disease and preparation method thereof and method of quality control.
Background technology
Coronary heart disease is one of the most dangerous disease of modern humans, also be the adult most important cause of the death disease of crowd of China, and sickness rate increases day by day.
The full name of coronary heart disease is coronary heart disease, mainly is owing to the coronary artery of supply heart blood because reason such as atherosis, and luminal stenosis causes deficiency myocardial blood supply.Angina pectoris can appear in the lighter, and weight person can cause myocardial infarction, even sudden death.Clinical main performance be exactly chest pain or uncomfortable in chest, feel suffocated the chest pain that occurs after activity or when excited especially.
Angina pectoris is to need the disease of treatment in time, treats untimely or malpractice, can develop into acute myocardial infarction.In case the generation myocardial infarction even at condition tertiary hospitals preferably, still have the case fatality rate about 10%, can not get the treatment of standard, case fatality rate is up to 30%.
There are many problems that wait to solve in western medical treatment coronary heart disease, as toleration, drug resistance and the side reaction etc. of medicine.
Summary of the invention
The object of the invention is to provide a kind of pharmaceutical composition and preparation method thereof, and another purpose of the present invention is to provide the method for quality control and the purposes of this pharmaceutical composition.
The present invention seeks to be achieved through the following technical solutions:
Pharmaceutical composition of the present invention is to make by the five tastes raw material of following weight portion:
Radix Astragali 3-12 weight portion, Radix Codonopsis 2-8 weight portion, Radix Ophiopogonis the 2-8 weight portion, Fructus Schisandrae Chinensis 0.5-4 weight portion, Fructus Schisandrae Sphenantherae 0.5-4 weight portion.
The preferred weight proportioning of above-mentioned five tastes crude drug is as follows:
The Radix Astragali 6 weight portions, Radix Codonopsis 4 weight portions, Radix Ophiopogonis 4 weight portion, Fructus Schisandrae Chinensis 1 weight portion, Fructus Schisandrae Sphenantherae 1 weight portion.
The preferred weight proportioning of above-mentioned five tastes crude drug is as follows:
The Radix Astragali 3.5 weight portions, Radix Codonopsis 2.5 weight portions, Radix Ophiopogonis 7.5 weight portion, Fructus Schisandrae Chinensis 3.5 weight portions, Fructus Schisandrae Sphenantherae 1 weight portion.
The preferred weight proportioning of above-mentioned five tastes crude drug is as follows:
The Radix Astragali 11 weight portions, Radix Codonopsis 3 weight portions, Radix Ophiopogonis 7 weight portion, Fructus Schisandrae Chinensis 1 weight portion, Fructus Schisandrae Sphenantherae 3 weight portions.
The preferred weight proportioning of above-mentioned five tastes crude drug is as follows:
The Radix Astragali 4 weight portions, Radix Codonopsis 7 weight portions, Radix Ophiopogonis 3 weight portion, Fructus Schisandrae Chinensis 3.5 weight portions, Fructus Schisandrae Sphenantherae 0.7 weight portion.
The preferred weight proportioning of above-mentioned five tastes crude drug is as follows:
The Radix Astragali 10 weight portions, Radix Codonopsis 7.5 weight portions, Radix Ophiopogonis 2.5 weight portion, Fructus Schisandrae Chinensis 0.7 weight portion, Fructus Schisandrae Sphenantherae 3.5 weight portions.
The Radix Astragali in the aforementioned pharmaceutical compositions can be a Radix Astragali (processed with Mel).
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make clinical acceptable granule, capsule, drop pill, tablet, oral liquid, slow releasing agent or lyophilized injectable powder according to common process.
The concrete preparation technology of drug composition oral solid preparation of the present invention is as follows:
Get above-mentioned five tastes crude drug, decoct with water 2～4 times, each 1～3 hour, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 4～13 weight portions, mixing, drying is made granular preparation.
The preferred for preparation method of medicament composition granule agent of the present invention is as follows:
Get above-mentioned five tastes crude drug, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 6.4 weight portions, mixing, drying is made granular preparation, packing, promptly.
The method of quality control of drug composition oral solid preparation of the present invention comprises following discrimination method and/or content assaying method:
Discrimination method comprises one or more in the following method:
A, get this drug composition oral solid preparation 2～15g, with chloroform 30～50ml, supersound process 10～30 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml chloroform contains 1mg schisandrin B product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 30～60 ℃ of petroleum ether: Ethyl formate: formic acid=12-18: 4-6: 1 upper solution is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get this drug composition oral solid preparation 10g, add water 20ml and make dissolving, add hydrochloric acid 0.5～2ml, heated and boiled 5 minutes, put coldly, extract, divide and get chloroform liquid with chloroform 10～20ml jolting, evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, and filtrate adds hydrochloric acid 0.5ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: acetone=3-5: 1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, get this drug composition oral solid preparation 5g, add methanol 20ml, supersound process 20-40 minute, filter, filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=12-18: 4-6: 1-3 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5～10 minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Content assaying method in the method for quality control is as follows:
Get this drug composition oral solid preparation 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 1～3 time, each 20～30ml discards ether layer, and water layer extracts 2～5 times with water saturated n-butyl alcohol jolting, each 20～40ml; Merge n-butanol extracting liquid, with ammonia solution washing 1～3 time, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 3～5ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins, water 80～150ml eluting discards water liquid, reuse 40% ethanol 20～30ml eluting, discard 40% ethanol elution, continue with 70% ethanol, 50～100ml eluting, collect eluent, evaporate to dryness, residue adds methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, add methanol and be diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=60-70: 30-40: 8-12 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan according to thin layer chromatography, wavelength X S=530nm, λ R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly;
This drug composition oral solid preparation, every gram contains astragaloside C
41H
68O
14, should be no less than 0.19mg.
This pharmaceutical composition has benefiting qi and nourishing yin, the effect of the tonifying the lung that nourishes heart, and diseases such as the coronary heart disease of deficiency of both QI and YIN, shortness of breath and palpitation and old weakness are had better curative effect.There is no untoward reaction, clinical practice safety in treatment coronary heart disease in the course of treatment and after the treatment.
Show according to the test of pesticide effectiveness: this pharmaceutical composition can improve the tolerance of body, enhancing body's immunological function; Have function of resisting myocardial ischemia, improve cardiac flow, reduce the generation of ischemic arrhythmia.Preventing that acute myocardial ischemia to aspect the infringement of cardiac hemodynamic, having certain drug action.
Pharmaceutical composition of the present invention adopts advanced technologies such as spray drying, the sugar type granules preparation of making, and suitable equally to the taboo sugar patient of diseases such as obesity, diabetes and hyperlipidemia, effective ingredient keeps more complete, and technology more becomes rationally, and quality obviously improves.Tool is easy to carry, it is easy to take, determined curative effect, characteristics such as applied widely.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
1 medicament composition granule agent of experimental example is to the influence of mice tolerance
The agent of this medicament composition granule of table 1 is to the influence of mice following time-to-live of normobaric hypoxia ((x ± SD)
| Group | Number of animals (n) | Time-to-live (branch) |
| This medicament composition granule of dosage group agent small dose group HUANGQI SHENGMAI YIN group in the agent of this medicament composition granule of the heavy dose of group of this medicament composition granule of blank group agent | 20 20 20 20 20 | 42.53±7.58 50.12±8.42** 51.38±10.69** 42.56±6.73 51.32±12.30** |
The agent of this medicament composition granule of table 2 is to the influence of mice swimming time (x ± SD)
| Group | Number of animals (n) | Time-to-live (branch) |
| This medicament composition granule of dosage group agent small dose group HUANGQI SHENGMAI YIN group in the agent of this medicament composition granule of the heavy dose of group of this medicament composition granule of blank group agent | 10 10 10 10 10 | 141.7±73.1 194.7±65.4** 186.6±42.61** 190.5±72.63** 202.7±59.14** |
Experimental study proves: medicament composition granule agent of the present invention can obviously improve the body tolerance of whole animal, prolongs following time-to-live of normobaric hypoxia and the extremely dead time of swimming of mice.
2 medicament composition granule agent of experimental example are to effect of immunologic function
This medicament composition granule of table 3 agent influence that pouring is changeed to mice T (x ± SD)
| Group | Example number (n) | T drenches commentaries on classics | The P value |
| The CTX+ granule is organized CTX+ granule therapeutic dose group CTX+ HUANGQI SHENGMAI YIN group CTX+ ordinary water normal group most for big dose | 10 10 10 10 10 | 19746±1461 18711±1896 19078±3413 15396±3190 32638±2661 | ＜0.05 ＜0.05 ＜0.05 ＜0.01 |
The agent of this medicament composition granule of table 4 is to the influence of mice M φ phagocytic percentage (x ± SD)
| Group | Example number (n) | Phagocytic percentage % | The P value |
| The heavy dose of group of CTX+ granule CTX+ granule therapeutic dose group CTX+ HUANGQI SHENGMAI YIN group CTX+ ordinary water normal group | 10 10 10 10 10 | 32.6±7.2 27.2±6.8 25.2±5.8 18.31±5.6 43.6±5.6 | ＜0.01 ＜0.01 ＜0.05 ＜0.01 |
Experimental study proves: medicament composition granule agent of the present invention can the enhancing human body immunity function; Can improve T lymphocyte transformation function and M φ phagocytosis by immunologic hypofunction mice due to the CTX.
3 medicament composition granule agent of experimental example are to the influence of pig acute myocardial ischemia
The agent of this medicament composition granule of table 5 gavages the reaction that the normal whole pig in back occurs
| Observation index | Response situation (+or-) | |||
| The heavy dose of group of granule (2.1g/kg/d) | Granule therapeutic dose group (0.7g/kg/d) | HUANGQI SHENGMAI YIN group (0.7g/kg/d) | ||
| Spontaneous activity | Increase reduce scurry run roll up motionless | - - - - | - - - - | - - - - |
| Muscular movement | The paralysis of withering is lost in the tic mutual aid of trembling | - - - - | - - - - | - - - - |
| Reaction | Nervous blunt | - - | - - | - - |
| The autonomic nervous system reaction | The perpendicular hair streams tear sialorrhea little protruding eye diarrhoea of people of opening one's eyes is turned round body | - - - - - - - | - - - - - - - | - - - - - - - |
The agent of this medicament composition granule of table 6 to coronary ligation after blood pressure (BP, kpa), heart rate (HR, inferior/minute), left chamber shrinks peak pressure (LVSP, kpa), left side chamber end diastolic pressure (LVEDP, kpa), the maximum climbing speed of left indoor pressure (the dP/dtmax, (x ± SD) of influence kPa/s)
| Group | Before the ischemia | Behind the ischemia (min) | ||||
| 15 | 30 | 60 | 120 | |||
| Matched group (n=5) | ||||||
| BP HR LVSP LVEDP dP/dtmax | 16.6±0.5 162.12±5.2 10.8±1.1 0.9±0.3 344.8±41.7 | 14.3±0.6 166.5±11.1 8.7±0.5 1.2±0.3 339.8±34.8 | 14.5±0.1 166.1±8.8 8.6±0.9 1.2±0.5 342.2±38.7 | 14.1±0.5 169.8±6.4 8.4±0.3 1.4±0.1 335.1±36.7 | 14.0±0.2 169.5±5.7 8.3±0.1 1.4±0.4 334.3±37.2 | |
| This medicament composition granule agent 1 group (0.7g/kg/d) (n=5) | ||||||
| BP HR LVSP LVEDP dP/dtmax | 15.8±0.5 162.19±5.0 12.2±0.3 0.8±0.1 364.8±32.1 | 13.7±0.6 168.5±10.1 11.0±0.4 1.2±0.3 359.4±34.1 | 13.5±0.1 167.1±8.5 11.5±0.6 1.2±0.3 357.9±37.2 | 12.9±0.5 163.8±6.1 9.6±0.1 1.2±0.3 360.7±54.8 | 10.0±0.2* 165.5±5.3 10.2±0.4* 1.2±0.6 358.9±17.7* | |
| This medicament composition granule agent 2 groups (2.1g/kg/d) (n=5) | ||||||
| BP HR LVSP LVEDP dP/dtmax | 16.8±0.5 164.12±5.2 13.9±0.8 0.9±0.2 343.6±32.5 | 14.7±0.6 165.5±11.1 12.4±1.2 1.1±0.1 329.6±26.4 | 14.5±0.4 162.1±8.8 11.6±0.8 1.0±0.2 337.9±31.5 | 14.9±0.5 162.8±6.2 12.3±1.1 1.1±0.1 340.2±29.4 | 15.7±0.2* 163.5±5.4 13.0±1.2* 1.2±0.1* 342.1±36.1* | |
| HUANGQI SHENGMAI YIN (0.7g/kg/d) (n=5) | ||||||
| BP HR LVSP LVEDP dP/dtmax | 16.2±0.5 162.42±5.2 13.6±0.9 0.9±0.1 356.3±23.1 | 14.3±0.6 168.5±10.2 12.1±0.7 1.1±0.2 356.3±21.1 | 13.5±0.1 166.3±8.1 12.2±0.8 1.0±0.1 350.2±23.4 | 13.9±0.5 163.8±6.1 12.0±0.8 1.1±0.1 351.5±24.7 | 15.6±0.2* 163.5±4.7 12.5±0.6* 1.1±0.2* 353.3±27.2* | |
Compare with matched group t-check * P＜0.05
The agent of this medicament composition granule of table 7 is to the influence of acute myocardial infarction scope
| Group | n | Ventricle gross weight (g) | Infarcted myocardium weight (g) | The white proportion by subtraction of infarcted myocardium (%) |
| This medicament composition granule agent (2.1g/kg/d) group HUANGQI SHENGMAI YIN (0.7g/kg/d) group is organized in this medicament composition granule of matched group agent (0.7g/kg/d) | 5 5 5 5 | 67.4±2.4 65.9±3.1 64.5±1.3 65.5±2.0 | 4.2±0.5 3.8±0.3 3.6±0.2 3.7±0.2 | 6.2±0.4 5.7±0.3* 5.5±0.4* 5.6±0.2* |
* compare with matched group P＜0.05
Experimental study proves: medicament composition granule agent of the present invention has function of resisting myocardial ischemia, improve cardiac hemodynamic, the obviously change of the myocardial cell electrophysiological characteristics that pig is caused because of the acute ischemia anoxia and increase the effect of myocardial cell electrical stability, thereby reduce the degree and the scope of myocardial ischemia, reduce the generation of ischemic arrhythmia.
In sum, experimentation confirms that agent of this medicament composition granule and HUANGQI SHENGMAI YIN have same drug action.(1) obviously improves the body tolerance of whole animal, prolong the normobaric hypoxia time-to-live of mice and swimming to the dead time.(2) can the enhancing human body immunity function; Can improve T lymphocyte transformation function and M φ phagocytosis by immunologic hypofunction mice due to the CTX.(3) has function of resisting myocardial ischemia, improve cardiac hemodynamic, the obviously change of the myocardial cell electrophysiological characteristics that pig is caused because of the acute ischemia anoxia and increase the effect of myocardial cell electrical stability, thus the degree and the scope of myocardial ischemia reduced, reduce the generation of ischemic arrhythmia.Therefore preventing that acute myocardial ischemia to aspect the infringement of cardiac hemodynamic, having certain drug action.
The clinical trial of 4 medicament composition granule agent treatments of experimental example coronary artery disease with deficiency of both qi and yin
Case 161 examples are verified in the clinical verification of treatment coronary heart disease syndrome of deficiency of both qi and yin altogether.Wherein inpatient's 116 examples account for 72.1% of total checking case.Be divided into treatment at random and organize 60 examples, matched group 60 examples, open treatment group 41 examples.Treatment group, the medicament composition granule agent of the present invention of open treatment group, the matched group HUANGQI SHENGMAI YIN.
Therapeutic outcome:
One, efficacy result
(1) treatment group efficacy result
1, treatment group therapeutic effect of syndrome:
The integration situation of change saw Table 8 before and after single symptom treatment was organized in treatment:
(x ± s) is organized before and after the treatment of each symptom integral value relatively in table 8 treatment
| Symptom | n | Integration | The t value | The P value | |
| Before the treatment | After the treatment | ||||
| The feeling of oppression and pain in the chest palpitaition palpitation and short breath tiredness with no desire to speak out of breath few Tianjin of dry total mark of having a dizzy spell | 54 53 56 51 50 48 60 | 1.93±0.72 1.83±0.75 1.70±0.69 1.63±0.72 1.68±0.71 1.67±0.69 9.03±3.25 | 0.48±0.50 0.55±0.57 0.48±0.57 0.59±0.70 0.66±0.66 0.39±0.61 2.70±1.92 | 13.80 12.56 11.66 8.31 9.77 10.43 14.17 | ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 |
60 routine patients use this medicament composition granule agent therapeutic outcome and show: produce effects 32 examples (53.3%), effective 22 examples (36.7%), invalid 6 examples (10%), obvious effective rate 53.3%, total effective rate 90%.Treatment back symptom integral all has obvious decline (P＜0.01).
2, open group symptom curative effect:
The integration situation of change sees Table 9 before and after the single symptom treatment of open group:
Compare before and after each the symptom integral value treatment of the open group of table 9 (x ± s)
| Symptom | n | Integration | The t value | The P value | |
| Before the treatment | After the treatment | ||||
| The feeling of oppression and pain in the chest palpitaition palpitation and short breath tiredness with no desire to speak out of breath few Tianjin of dry total mark of having a dizzy spell | 41 41 37 40 40 30 41 | 2.05±0.71 2.02±0.61 1.93±0.93 1.78±0.69 1.49±0.60 2.0±0.70 10.71±2.98 | 0.66±0.69 0.73±0.59 0.85±0.61 0.65±0.61 0.49±0.60 0.67±0.61 4.0±2.25 | 12.53 11.47 11.67 11.72 12.29 9.10 16.62 | ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 |
41 routine patients use this medicament composition granule agent therapeutic outcome and show: produce effects 20 examples (48.8%), effective 18 examples (43.9%), invalid 3 examples (7.3%), obvious effective rate 48.8%, total effective rate 92.7%.The all obviously decline (P＜0.01) of treatment back symptom integral.
(2) matched group efficacy result
The integration situation of change sees Table 10 before and after the single symptom treatment of matched group:
Compare before and after each the symptom integral value treatment of table 10 matched group (x ± s)
| Symptom | n | Integration | The t value | The P value | |
| Before the treatment | After the treatment | ||||
| The feeling of oppression and pain in the chest palpitaition palpitation and short breath tiredness with no desire to speak out of breath few Tianjin of dry total mark of having a dizzy spell | 58 57 54 51 40 45 60 | 2.03±0.65 1.98±0.72 1.93±0.72 1.51±0.61 1.51±0.51 1.27±0.50 8.83±2.94 | 0.91±0.66 0.86±0.61 0.87±0.67 0.61±0.67 0.68±0.61 0.41±0.54 2.92±2.42 | 11.82 11.96 11.82 9.56 8.78 9.30 15.14 | ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 ＜0.01 |
60 routine patients use the HUANGQI SHENGMAI YIN therapeutic outcome and show: produce effects 24 examples (40%), effective 28 examples (46.7%), obvious effective rate 40%, total effective rate 86.7%.Treatment back symptom integral all has obvious decline (P＜0.01).
(3) respectively organize curative effect relatively
1, respectively organize obvious effective rate and total effective rate relatively, see Table 11:
Table 11 is respectively organized therapeutic effect of syndrome relatively
| Group | n | Produce effects | Effectively | Invalid | Obvious effective rate (%) | Total effective rate (%) |
| The open group of treatment group treatment group+opening group matched group | 60 41 101 60 | 32 20 52 24 | 22 18 40 28 | 6 3 9 8 | 53.3 48.8 51.5 40 | 90 92.7 91.1 86.7 |
Analyze through Ridit, treatment group and the open group similar no significant difference of curative effect (P＞0.05), treatment group and matched group, treatment group+opening group and matched group curative effect be no significant difference (P＞0.05) relatively all.
2, respectively organize each symptom treatment front and back integration differential relatively, see Table 12:
Table 12 is respectively organized before and after each symptom treatment relatively (x ± s) of integration differential
| Symptom | Group | n | Product moment | The t value | P value (comparing) with matched group |
| The feeling of oppression and pain in the chest palpitaition palpitation and short breath tiredness with no desire to speak out of breath few Tianjin of dry total mark of having a dizzy spell | The open group of the treatment group treatment group+open group of the opening group treatment of control group group treatment group+open group of the opening group treatment of control group group treatment group+open group of the opening group treatment of control group group treatment group+open group of the opening group treatment of control group group treatment group+open group of the opening group treatment of control group group treatment group+open group of opening group treatment of control group group treatment group+opening group control group | 54 41 95 58 53 41 94 57 56 37 93 54 51 40 91 51 50 40 90 40 48 30 78 45 60 41 101 60 | 1.44±0.77 1.39±0.74 1.42±0.75 1.16±0.75 1.28±0.74 1.29±0.72 1.29±0.73 1.12±0.71 1.21±0.78 1.19±0.62 1.20±0.72 1.06±0.66 1.02±0.88 1.13±0.61 1.07±0.77 0.90±0.69 1.04±0.78 1.03±0.53 1.03±0.68 0.83±0.59 1.27±0.84 1.33±0.80 1.29±0.82 0.87±0.63 6.33±3.41 6.66±2.75 6.47±3.18 5.91±2.62 | 1.95 1.51 2.08 / 1.16 1.16 1.40 / 1.09 0.95 1.17 / 0.64 1.52 1.16 / 1.41 1.60 1.61 / 2.58 2.78 2.97 / 0.76 1.39 1.15 / | ＞0.05 ＞0.05 ＜0.05 / ＞0.05 ＞0.05 ＞0.05 / ＞0.05 ＞0.05 ＞0.05 / ＞0.05 ＞0.05 ＞0.05 / ＞0.05 ＞0.05 ＞0.05 / ＜0.05 ＜0.05 ＜0.05 / ＞0.05 ＞0.05 ＞0.05 / |
Treatment group, open group, treatment add open group and matched group integration differential relatively, respectively organize curative effect and be better than matched group except that the symptom of the few Tianjin of xerostomia; Treatment adds open group and compares with matched group, and there were significant differences (P＜0.05) to alleviating the feeling of oppression and pain in the chest symptom; Each group of integration differential does not more all have significant difference (P＞0.05) with matched group before and after all the other each symptom treatments.
3, respectively organize the ECG curative effect result relatively, see Table 13:
Table 13 is respectively organized the ECG curative effect result relatively
| Group | n | Produce effects | Effectively | Invalid | Obvious effective rate (%) | Total effective rate (%) |
| The open group of treatment group treatment group+opening group matched group | 54 41 95 49 | 11 8 19 8 | 13 9 22 11 | 30 24 54 30 | 20.4 19.5 20 16.3 | 44.4 41.5 43.2 38.8 |
The result shows: each organizes the equal no significant difference of ECG curative effect, all P＞0.05.
Treatment group, treatment add open group and matched group obvious effective rate and total effective rate there was no significant difference (P＞0.05).
Two, treatment group safety observed result
(1) obvious adverse reaction does not appear in all cases during the treatment.
(2) treatment detects routine blood test before and after organizing 61 routine patient treatments, hepatic and renal function the results are shown in Table 14:
Compare before and after the treatment of table 14 treatment group safety indexes (x ± s)
| Test item | n | Before the treatment | After the treatment | The t value | The P value |
| Hgb(g/L) WBC(×10 9/L) PLT(×10 9/L) ALT(u/L) Cr(umol/L) BUN(mmol/L) | 61 61 61 61 61 61 | 144.4±10.5 5.48±1.62 128.3±65.2 18.62±11.46 88.22±27.96 5.74±4.79 | 141.5±10.3 5.42±1.41 131.9±58.5 17.98±9.06 85.42±25.74 6.08±5.92 | 1.76 0.44 1.76 1.01 1.62 1.17 | ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 ＞0.05 |
Show after testing: the every index in treatment back have no significant change (P＞0.05).
By to the clinical trial of this pharmaceutical composition, the result is: treatment group obvious effective rate is 53.3%, and effective percentage is 36.7%, and total effective rate is 90%; Treatment adds open group, and obvious effective rate is 51.5%, and effective percentage is 39.6%, and total effective rate is 91.1%; The matched group obvious effective rate is 40%, and effective percentage is 46.7%, total effective rate 86.7%.Electrocardiogram is improved: treatment group obvious effective rate is 20.4%, and total effective rate is 44.4%; It is 20% that treatment adds open group obvious effective rate, and total effective rate is 43.2%; The matched group obvious effective rate is 16.3%, and total effective rate is 38.8%.The agent of this medicament composition granule and matched group HUANGQI SHENGMAI YIN the curative effect of treatment coronary heart disease with compare aspect electrocardiogram improves, learn by statistics and handle the P value all＞0.05, difference does not have significance, untoward reaction is not found in whole clinical trial, treatment detects the no abnormality seen variation as a result of hematuria routine, hepatic and renal function, this medicine clinical practice safety before and after organizing 60 routine patient treatments.
Following embodiment all can realize the effect of above-mentioned experimental example.
Embodiment 1: the preparation of tablet
Radix Astragali 3.5kg, Radix Codonopsis 2.5kg, Radix Ophiopogonis 7.5kg, Fructus Schisandrae Chinensis 3.5kg, Fructus Schisandrae Sphenantherae 1kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make tablet according to common process.
Embodiment 2: the preparation of capsule
(processed with honey) Radix Astragali 11kg, Radix Codonopsis 3kg, Radix Ophiopogonis 7kg, Fructus Schisandrae Chinensis 1kg, Fructus Schisandrae Sphenantherae 3kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make capsule according to common process.
Embodiment 3: the preparation of lyophilized injectable powder
Radix Astragali 10kg, Radix Codonopsis 7.5kg, Radix Ophiopogonis 2.5kg, Fructus Schisandrae Chinensis 0.7kg, Fructus Schisandrae Sphenantherae 3.5kg.
Get the above-mentioned raw materials medicine, add conventional adjuvant,, make lyophilized injectable powder according to common process.
Embodiment 4: the preparation of granule
(processed with honey) Radix Astragali 6kg, Radix Codonopsis 4kg, Radix Ophiopogonis 4kg, Fructus Schisandrae Chinensis 1kg, Fructus Schisandrae Sphenantherae 1kg.
Get above five tastes crude drug, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 6.4kg, mixing, drying is made granule, packing, promptly.
Embodiment 5: the preparation of granule
Radix Astragali 9kg, Radix Codonopsis 4.5kg, Radix Ophiopogonis 1.5kg, Fructus Schisandrae Chinensis 1.5kg, Fructus Schisandrae Sphenantherae 2.85kg.
Get above five tastes crude drug, decoct with water 3 times, each 1.5 hours, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 7kg, mixing, drying is made granule, packing, promptly.
Embodiment 6: the preparation of granule
(processed with honey) Radix Astragali 6kg, Radix Codonopsis 4kg, Radix Ophiopogonis 4kg, Fructus Schisandrae Chinensis 1kg, Fructus Schisandrae Sphenantherae 1kg.
Get above five tastes crude drug, decoct with water 4 times, each 2.5 hours, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 6.45kg, mixing, drying is made granule, packing, promptly.
Embodiment 7: the method for quality control of granule
Discrimination method:
A, get embodiment 4 content 8.5g, use chloroform 40ml, supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml contains 1mg product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 45 ℃ of petroleum ether: Ethyl formate: the upper solution of formic acid=15: 5: 1 is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get embodiment 4 content 10g, add water 20ml and make dissolving, add hydrochloric acid 1.25ml, heated and boiled 5 minutes is put coldly, extracts with chloroform 15ml jolting, divides and gets chloroform liquid, and evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, and filtrate adds hydrochloric acid 0.5ml, shines medical material solution in pairs with legal system; According to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: acetone=4: 1 be developing solvent, launches, and takes out, and dries, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, get embodiment 4 content 5g, add methanol 20ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=15: 5: 2 be developing solvent, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 8 minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiment 8: the method for quality control of granule
Content assaying method:
Get embodiment 5 content 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 2 times, each 25ml discards ether layer, and water layer extracts 3 times with water saturated n-butyl alcohol jolting, at every turn 30ml; Merge n-butanol extracting liquid, with ammonia solution washing 2 times, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 4ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins (internal diameter 1.5cm, long 11cm), water 115ml eluting, discard water liquid, reuse 40% ethanol 25ml eluting discards 40% ethanol elution, continues with 70% ethanol 75ml eluting, collect eluent, evaporate to dryness, residue add methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, adds methanol and is diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=65: 35: 10 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength X according to thin layer chromatography
S=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly;
Medicament composition granule agent of the present invention, every g contains astragaloside C
41H
68O
14Should be no less than 0.19mg.
Embodiment 9: the method for quality control of granule
Discrimination method:
A, get embodiment 6 content 3g, use chloroform 45ml, supersound process 15 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml chloroform contains 1mg schisandrin B product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 55 ℃ of petroleum ether: Ethyl formate: the upper solution of formic acid=12: 6: 1 is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get embodiment 6 content 10g, add water 20ml and make dissolving, add hydrochloric acid 0.6ml, heated and boiled 5 minutes is put coldly, extracts with chloroform 18ml jolting, divides and gets chloroform liquid, and evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, and filtrate adds hydrochloric acid 0.5ml, shines medical material solution in pairs with legal system; According to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: acetone=3: 1 be developing solvent, launches, and takes out, and dries, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, get embodiment 6 content 5g, add methanol 20ml, supersound process 25 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw above-mentioned two kinds of each 10ul of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=12: 6: 1 be developing solvent, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 8 minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The pharmaceutical composition of getting embodiment 6 carries out assay.
Get embodiment 6 content 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 1 time, each 30ml discards ether layer, and water layer extracts 2 times with water saturated n-butyl alcohol jolting, at every turn 35ml; Merge n-butanol extracting liquid, with ammonia solution washing 1 time, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 5ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins (internal diameter 1.5cm, long 11cm), water 85ml eluting, discard water liquid, reuse 40% ethanol 30ml eluting discards 40% ethanol elution, continues with 70% ethanol 55ml eluting, collect eluent, evaporate to dryness, residue add methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, adds methanol and is diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=60: 40: 8 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength X according to thin layer chromatography
S=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly; Medicament composition granule agent of the present invention, every gram contains astragaloside C
41H
68O
14Should be no less than 0.19mg.
Embodiment 10: the method for quality control of tablet
Discrimination method:
A, get embodiment 1 content 14g, use chloroform 35ml, supersound process 25 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml chloroform contains 1mg schisandrin B product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10ul, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 35 ℃ of petroleum ether: Ethyl formate: the upper solution of formic acid=18: 4: 1 is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
B, get embodiment 1 content 10g, add water 20ml and make dissolving, add hydrochloric acid 1.8ml, heated and boiled 5 minutes is put coldly, extracts with chloroform 12ml jolting, divides and gets chloroform liquid, and evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, and filtrate adds hydrochloric acid 0.5ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: acetone=5: 1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The pharmaceutical composition of getting embodiment 1 carries out assay.
Get embodiment 1 content 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 3 times, each 20ml discards ether layer, and water layer extracts 4 times with water saturated n-butyl alcohol jolting, at every turn 25ml; Merge n-butanol extracting liquid, with ammonia solution washing 3 times, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 3ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins, water 145ml eluting discards water liquid, reuse 40% ethanol 20ml eluting, discard 40% ethanol elution, continue with 70% alcohol 95 ml eluting, collect eluent, evaporate to dryness, residue adds methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, add methanol and be diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography; Test, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=70: 30: 12 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan according to thin layer chromatography, wavelength X=530nm, λ=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly;
Pharmaceutical composition tablet of the present invention, every gram contains astragaloside C
41H
68O
14, should be no less than 0.19mg.
Embodiment 11: the method for quality control of granule
Discrimination method:
A, get embodiment 4 content 8.5g, use chloroform 40ml, supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml chloroform contains 1mg schisandrin B product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 45 ℃ of petroleum ether: Ethyl formate: the upper solution of formic acid=15: 5: 1 is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
C, get embodiment 4 content 5g, add methanol 20ml, supersound process 35 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=18: 4: 3 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5～10 minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The pharmaceutical composition of getting embodiment 4 carries out assay.
Get embodiment 4 content 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 1 time, each 30ml discards ether layer, and water layer extracts 2 times with water saturated n-butyl alcohol jolting, at every turn 25ml; Merge n-butanol extracting liquid, with ammonia solution washing 3 times, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 3ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins, water 145ml eluting discards water liquid, reuse 40% ethanol 20ml eluting, discard 40% ethanol elution, continue with 70% alcohol 95 ml eluting, collect eluent, evaporate to dryness, residue adds methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, add methanol and be diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=70: 30: 12 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan according to thin layer chromatography, wavelength X=530nm, λ=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly;
Medicament composition granule agent of the present invention, every gram contains astragaloside C
41H
68O
14, should be no less than 0.19mg.
Claims (19)
1, a kind of pharmaceutical composition for the treatment of coronary heart disease, it is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight: Radix Astragali 3-12 weight portion, Radix Codonopsis 2-8 weight portion, Radix Ophiopogonis the 2-8 weight portion, Fructus Schisandrae Chinensis 0.5-4 weight portion, Fructus Schisandrae Sphenantherae 0.5-4 weight portion.
2, pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight: the Radix Astragali 6 weight portions, Radix Codonopsis 4 weight portions, Radix Ophiopogonis 4 weight portion, Fructus Schisandrae Chinensis 1 weight portion, Fructus Schisandrae Sphenantherae 1 weight portion.
3, pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight: the Radix Astragali 3.5 weight portions, Radix Codonopsis 2.5 weight portions, Radix Ophiopogonis 7.5 weight portion, Fructus Schisandrae Chinensis 3.5 weight portions, Fructus Schisandrae Sphenantherae 1 weight portion.
4, pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight: the Radix Astragali 11 weight portions, Radix Codonopsis 3 weight portions, Radix Ophiopogonis 7 weight portion, Fructus Schisandrae Chinensis 1 weight portion, Fructus Schisandrae Sphenantherae 3 weight portions.
5, pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight: the Radix Astragali 4 weight portions, Radix Codonopsis 7 weight portions, Radix Ophiopogonis 3 weight portion, Fructus Schisandrae Chinensis 3.5 weight portions, Fructus Schisandrae Sphenantherae 0.7 weight portion.
6, pharmaceutical composition as claimed in claim 1 is characterized in that this pharmaceutical composition is to be made by following raw material medicaments in part by weight: the Radix Astragali 10 weight portions, Radix Codonopsis 7.5 weight portions, Radix Ophiopogonis 2.5 weight portion, Fructus Schisandrae Chinensis 0.7 weight portion, Fructus Schisandrae Sphenantherae 3.5 weight portions.
7,, it is characterized in that the Radix Astragali described in this pharmaceutical composition is a Radix Astragali (processed with Mel) as claim 1,2,3,4,5 or 6 described pharmaceutical compositions.
8, as claim 1,2,3,4,5 or 6 described pharmaceutical compositions, it is characterized in that getting the above-mentioned composition crude drug, add conventional adjuvant,, make granule, capsule, drop pill, tablet, oral liquid, slow releasing agent or lyophilized injectable powder according to common process.
9, pharmaceutical composition as claimed in claim 7 is characterized in that getting the above-mentioned composition crude drug, adds conventional adjuvant, according to common process, makes granule, capsule, drop pill, tablet, oral liquid, slow releasing agent or lyophilized injectable powder.
10, as claim 1,2,3,4,5 or 6 described preparation of drug combination methods, it is characterized in that this method may further comprise the steps: get the Radix Astragali, Radix Codonopsis, Radix Ophiopogonis, Fructus Schisandrae Chinensis and Fructus Schisandrae Sphenantherae five tastes crude drug, decoct with water 2～4 times, each 1～3 hour, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, add dextrin 4～13 weight portions, mixing, drying is made granular preparation.
11, preparation of drug combination method as claimed in claim 10 is characterized in that this method may further comprise the steps: get the Radix Astragali, Radix Codonopsis, Radix Ophiopogonis, Fructus Schisandrae Chinensis and Fructus Schisandrae Sphenantherae five tastes crude drug, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 6.4 weight portions, mixing, drying is made granular preparation.
12, preparation of drug combination method as claimed in claim 7, it is characterized in that this method may further comprise the steps: get Radix Astragali (processed with Mel), Radix Codonopsis, Radix Ophiopogonis, Fructus Schisandrae Chinensis and Fructus Schisandrae Sphenantherae five tastes crude drug, decoct with water 2～4 times, each 1～3 hour, filter, merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, add dextrin 4-13 weight portion, mixing, drying is made granular preparation.
13, preparation of drug combination method as claimed in claim 12 is characterized in that this method may further comprise the steps: get Radix Astragali (processed with Mel), Radix Codonopsis, Radix Ophiopogonis, Fructus Schisandrae Chinensis and Fructus Schisandrae Sphenantherae five tastes crude drug, decoct with water secondary, 2 hours for the first time, 1.5 hours for the second time, filter merging filtrate, centrifugal, relative density is 1.08 clear paste when getting supernatant and being evaporated to 80 ℃, adds dextrin 6.4 weight portions, mixing, drying is made granular preparation.
14, the method for quality control of pharmaceutical composition as claimed in claim 8 is characterized in that this method comprises one or more in the following discriminating:
A, get this drug composition oral solid preparation 2～15g, with chloroform 30～50ml, supersound process 10～30 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml chloroform contains 1mg schisandrin B product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 30-60 ℃ of petroleum ether: Ethyl formate: formic acid=12-18: 4-6: 1 upper solution is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get this drug composition oral solid preparation 10g, add water 20ml and make dissolving, add hydrochloric acid 0.5～2ml, heated and boiled 5 minutes, put coldly, extract, divide and get chloroform liquid with chloroform 10～20ml jolting, evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, and filtrate adds hydrochloric acid 0.5ml, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: acetone=3-5: 1 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, get this drug composition oral solid preparation 5g, add methanol 20ml, supersound process 20～40 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, shines medical material solution in pairs with legal system; According to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=12-18: 4-6: 1-3 is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 5～10 minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
15, the method for quality control of pharmaceutical composition as claimed in claim 14 is characterized in that this method comprises one or more in the following discriminating:
A, get this drug composition oral solid preparation 8.5g, use chloroform 40ml, supersound process 20 minutes filters, and filtrate evaporate to dryness, residue add chloroform 0.5ml makes dissolving, as need testing solution; Other gets the schisandrin B reference substance, and chlorination is copied into solution that every 1ml chloroform contains 1mg schisandrin B product solution in contrast; According to the thin layer chromatography test, draw need testing solution 10 μ l, reference substance solution 5 μ l put in same silica gel G F respectively
254On the lamellae, with 45 ℃ of petroleum ether: Ethyl formate: the upper solution of formic acid=15: 5: 1 is developing solvent, launches, and takes out, and dries, and puts under the 254nm ultra-violet lamp and inspects; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
B, get this drug composition oral solid preparation 10g, add water 20ml and make dissolving, add hydrochloric acid 1.25ml, heated and boiled 5 minutes, put coldly, extract, divide and get chloroform liquid with chloroform 15ml jolting, evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material 1g Radix Ophiopogonis, adds water 20ml, decocts 10 minutes, filters, and filtrate adds hydrochloric acid 0.5ml, shines medical material solution in pairs with legal system; According to thin layer chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform: acetone=4: 1 be developing solvent, launches, and takes out, and dries, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ be heated to speckle develop the color clear; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
C, get this drug composition oral solid preparation 5g, add methanol 20ml, supersound process 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution; Other gets Radix Codonopsis control medicinal material 2g, shines medical material solution in pairs with legal system; According to thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene: ethyl acetate: formic acid=15: 5: 2 be developing solvent, launches, and takes out, and dries, and spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ were dried by the fire 8 minutes; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
16,, it is characterized in that comprising in this method following assay as the method for quality control of claim 14 or 15 described pharmaceutical compositions:
Get this drug composition oral solid preparation 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 1～3 time, each 20～30ml discards ether layer, and water layer extracts 2～5 times with water saturated n-butyl alcohol jolting, each 20～40ml; Merge n-butanol extracting liquid, with ammonia solution washing 1～3 time, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 3～5ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins, water 80～150ml eluting discards water liquid, reuse 40% ethanol 20-30ml eluting, discard 40% ethanol elution, continue with 70% ethanol, 50～100ml eluting, collect eluent, evaporate to dryness, residue adds methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, add methanol and be diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=60-70: 30-40: 8-12 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength X according to thin layer chromatography
S=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly;
This drug composition oral solid preparation, every gram contains astragaloside C
41H
68O
14, should be no less than 0.19mg.
17, require the method for quality control of 16 described pharmaceutical compositions as profit, it is characterized in that assay is in this method:
Get this drug composition oral solid preparation 5g, the accurate title, decide, and after the water 30ml dissolving, puts in the separatory funnel, and with ether washing 2 times, each 25ml discards ether layer, and water layer extracts 3 times with water saturated n-butyl alcohol jolting, at every turn 30ml; Merge n-butanol extracting liquid, with ammonia solution washing 2 times, each 40ml discards ammoniacal liquor; N-butyl alcohol liquid evaporate to dryness, residue add water 4ml makes dissolving, puts coldly, and the top set end is added with the D of 2.5g neutral alumina
101On the type macroporous adsorptive resins, water 115ml eluting discards water liquid, reuse 40% ethanol 25ml eluting, discard 40% ethanol elution, continue with 70% ethanol 75ml eluting, collect eluent, evaporate to dryness, residue adds methanol also quantitatively is transferred in the 2ml measuring bottle dissolving, add methanol and be diluted to scale, shake up, as need testing solution; Other precision takes by weighing through dry 24 hours astragaloside reference substance of phosphorus pentoxide an amount of, adds methanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw need testing solution 3 μ l, 6 μ l and reference substance solution 3 μ l, 6 μ l respectively, the cross point is on same silica gel g thin-layer plate respectively, with chloroform: methanol: water=65: 35: 10 is developing solvent placing lower floor's solution at a night below 10 ℃, launches, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the speckle colour developing at 105 ℃; On lamellae, cover onesize glass plate, use immobilization with adhesive tape on every side, scan wavelength X according to thin layer chromatography
S=530nm, λ
R=700nm measures test sample trap integrated value and reference substance trap integrated value, calculates, promptly;
This drug composition oral solid preparation, every gram contains astragaloside C
41H
68O
14Should be no less than 0.19mg.
18, as claim 1,2,3,4, the application of 5 or 6 described pharmaceutical compositions in the medicine of preparation treatment coronary heart disease.
19, the application of pharmaceutical composition as claimed in claim 7 in the medicine of preparation treatment coronary heart disease.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100581128A CN1313132C (en) | 2006-03-02 | 2006-03-02 | Medicine composition for treating coronary heart disease and its prepn process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100581128A CN1313132C (en) | 2006-03-02 | 2006-03-02 | Medicine composition for treating coronary heart disease and its prepn process |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120121743A1 (en) * | 2009-07-30 | 2012-05-17 | Sebastien Garnier | Schisandra sphenanthera fruit extract and cosmetic, dermatological and nutraceutical compositions comprising same |
| CN111214609A (en) * | 2020-03-02 | 2020-06-02 | 浙江新光药业股份有限公司 | Application of a kind of Huangqi Shengmai Decoction in the preparation of pulmonary arterial hypertension medicine |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1491707A (en) * | 2003-08-02 | 2004-04-28 | 浙江天一堂集团有限公司 | Pulse-activating astragalus root soft capsule and its preparing method |
| CN1682923A (en) * | 2005-03-08 | 2005-10-19 | 北京正大绿洲医药科技有限公司 | Body strengthening dripping pill for invigorating qi and refreshing and its preparing method |
-
2006
- 2006-03-02 CN CNB2006100581128A patent/CN1313132C/en active Active
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120121743A1 (en) * | 2009-07-30 | 2012-05-17 | Sebastien Garnier | Schisandra sphenanthera fruit extract and cosmetic, dermatological and nutraceutical compositions comprising same |
| US8586107B2 (en) * | 2009-07-30 | 2013-11-19 | Laboratoires Expanscience | Schisandra sphenanthera fruit extract and cosmetic, dermatological, and nutraceutical compositions comprising same |
| CN111214609A (en) * | 2020-03-02 | 2020-06-02 | 浙江新光药业股份有限公司 | Application of a kind of Huangqi Shengmai Decoction in the preparation of pulmonary arterial hypertension medicine |
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