CN1562285A - Combination of active constituent of Chinese traditional medicine for curing cardiovascular and cerebrovascular diseases and preparation method - Google Patents

Combination of active constituent of Chinese traditional medicine for curing cardiovascular and cerebrovascular diseases and preparation method Download PDF

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CN1562285A
CN1562285A CN 200410026913 CN200410026913A CN1562285A CN 1562285 A CN1562285 A CN 1562285A CN 200410026913 CN200410026913 CN 200410026913 CN 200410026913 A CN200410026913 A CN 200410026913A CN 1562285 A CN1562285 A CN 1562285A
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rhizoma chuanxiong
salvianolic acid
ethanol
phenols
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徐江平
陆波
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Abstract

A Chinese medicine for preventing and treating cardiovascular and cerebrovascular diseases, such as cerebral infarction, cerebral ischemia, coronary heart disease, etc is prepared from red sage root, Chuan-xiong rhizome and pharmacologically acceptable carrier. It contains darshinolic acid, cnidiumol and ferulaic acid. Its preparing process is also disclosed.

Description

A kind of active ingredient of Chinese herbs composition and method of making the same of preventing and treating cardiovascular and cerebrovascular disease
Technical field
The present invention relates to a kind of Chinese medicine composition and preparation method thereof, relate in particular to a kind of active ingredient of Chinese herbs composition and method of making the same of preventing and treating cardiovascular and cerebrovascular disease.
Background technology
The traditional Chinese medical science thinks that qi depression to blood stasis is a main cause of cardiovascular and cerebrovascular disease morbidity, and the Chinese medicine compound of forming with Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong is used for the qi depression to blood stasis cardiovascular and cerebrovascular disease, and is evident in efficacy.But traditional compound Chinese medicinal preparation exists to become to be hard to tell, mechanism is not clear, the difficult control of quality, the unsteady shortcoming of curative effect.
Radix Salviae Miltiorrhizae is the Chinese medicine of traditional simply blood circulation promoting and blood stasis dispelling, and a large amount of studies show that, the total salvianolic acid of Radix Salviae Miltiorrhizae is the effective ingredient of its blood circulation promoting and blood stasis dispelling, and wherein the effect of salvianolic acid B magnesium is the strongest, and its content height can help to improve the curative effect of disease; Rhizoma Chuanxiong is the Chinese medicine of blood-activating and qi-promoting simply, be widely used in coronary heart disease, anginal treatment, total alkaloids and total phenol property composition are its effective ingredient, and main effect is the total phenol property composition (alkaloid is very low, only be the 1/100-1/10 of total phenol property composition), its content height can help to improve the curative effect of disease.
Existing commercially available GUANXINNING ZHUSHEYE contains the water soluble ingredient of Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong, has blood circulation promoting and blood stasis dispelling, the effect of freeing vessels and nourishing heart; Be used for coronary heart disease, anginal control.In the Sanitation Ministry medicine standard, GUANXINNING ZHUSHEYE (WS3-B-32) is proposed the alcohol deposition method preparation of two steps by Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong two flavor Chinese medicines through water.Studies show that the effective ingredient of Radix Salviae Miltiorrhizae blood circulation promoting and blood stasis dispelling is a total salvianolic acid, wherein the effect of salvianolic acid B magnesium is the strongest, and traditional water extraction alcohol deposition method can not obtain containing the more total salvianolic acid of salvianolic acid B magnesium.The total phenol property composition of Rhizoma Chuanxiong is its effective ingredient, but it is not carried out content control in the standard of GUANXINNING ZHUSHEYE, makes drug quality can not guarantee to stablize.
Summary of the invention
The objective of the invention is to overcome the above-mentioned shortcoming of traditional compound Chinese medicinal preparation of forming by Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, it is the Chinese medicine composition of active component that a kind of effective site mixture with Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong is provided, and this Chinese medicine composition effective ingredient is clear and definite, easy to control the quality, curative effect is reliable.
The object of the present invention is to provide a kind of above-mentioned active ingredient of Chinese herbs preparation of compositions method.
Purpose of the present invention is achieved by the following technical programs:
A kind of Chinese medicine composition of preventing and treating cardiovascular and cerebrovascular disease provided by the invention, comprise active component and medically acceptable carrier, described by weight percentage active component is 0.1~99.9%, carrier is 0.1~99.9%, described active component is the extract total salvianolic acid of Radix Salviae Miltiorrhizae and the extract Rhizoma Chuanxiong total phenols of Rhizoma Chuanxiong, and total salvianolic acid and Rhizoma Chuanxiong total phenols are 1: 0.1~15 by weight ratio; Total phenolic content is 30%~99.9% in the total salvianolic acid, wherein contains salvianolic acid B magnesium 10%~99.9%; Total phenol content 30%~99.9% in the Rhizoma Chuanxiong total phenols, wherein contains ferulic acid 10%~99.9%.
The preferably described by weight percentage active component of Chinese medicine composition of the present invention is 0.1~30%, and carrier is 70~99.9%,
For effectively improving the treatment of diseases effect, be preferably in the Chinese medicine composition of the present invention: described total salvianolic acid and Rhizoma Chuanxiong total phenols are 1: 0.5~10 by weight ratio; Total phenolic content is 80%~90% in the total salvianolic acid, wherein contains salvianolic acid B magnesium 50%~80%; Total phenol content is 80%~90% in the Rhizoma Chuanxiong total phenolic acids, wherein contains ferulic acid 30%~60%.
The preparation method of above-mentioned Chinese medicine composition provided by the invention is, at first from Radix Salviae Miltiorrhizae, extract total salvianolic acid and from Rhizoma Chuanxiong, extract the Rhizoma Chuanxiong total phenols, total salvianolic acid and Rhizoma Chuanxiong total phenols are mixed to scale as active component, mix with medically acceptable carrier according to a conventional method then and carry out preparation.
Because total salvianolic acid character instability, meet violent condition such as acid, alkali, heat and can degrade, so adopt mild condition, acetone percolation that efficient is high, and with the content of total phenolic acid in the total salvianolic acid and salvianolic acid B magnesium wherein as index.The method of extracting total salvianolic acid from Radix Salviae Miltiorrhizae is as follows:
1.1 extract with percolation with acetone, the Radix Salviae Miltiorrhizae after soaking is placed acetone, the concentration of acetone is 30~80%, its consumption is more than 8 times of Radix Salviae Miltiorrhizae weight; Then the acetone percolate is concentrated to about 1/10 of original volume, to there not being the acetone flavor;
1.2 use purification by macroporous resin, with the acetone percolate after concentrating, to extract liquid measure and amount of resin be that 1: 1 ratio is passed through macroporous resin column according to concentrating the back;
1.3 use ethanol purification, macroporous resin that will be by extracting solution is earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 10~60% carries out eluting with the consumption of column volume more than 10 times, collects eluent, and drying promptly gets the total salvianolic acid composition; Total phenolic content is 30%~99.9% in the total salvianolic acid that makes, and wherein contains salvianolic acid B magnesium 10%~99.9%:
In the extracting method of above-mentioned total salvianolic acid, the soak time before the concentration of used acetone, consumption and the percolation is the principal element of total phenolic acid of influence and salvianolic acid B magnesium content's index wherein, carries out L by three factors, three levels 9(3 3) orthogonal test.Result of the test shows that the concentration of preferred acetone is 50~70% in above-mentioned steps 1.1, and its consumption is 9~12 times of Radix Salviae Miltiorrhizae weight, and the soak time influence is little, generally more than 20 minutes; The concentration of preferred alcohol is 20~40% in the described step 1.3.Total phenolic content is 80%~90% in the total salvianolic acid that obtains by selection process, wherein contains salvianolic acid B magnesium 50%~80%.
Total phenolic content colorimetric method for determining in the total salvianolic acid, the salvianolic acid B magnesium salt content is measured with the HPLC method.
Therefore the Rhizoma Chuanxiong total phenols easily is dissolved in water and ethanol, adopts the high ethanol refluxing process of extraction efficiency to extract, and with content of ferulic acid in total phenols and the total phenols as investigating index.The method of extracting the Rhizoma Chuanxiong total phenols from Rhizoma Chuanxiong is as follows:
2.1 use alcohol reflux, be 40%~90% ethanol with concentration, its consumption is that the hot reflux of carrying out more than 10 times of Rhizoma Chuanxiong weight is extracted, extraction time is 2~5 times;
2.2 use ethyl acetate extraction, extracting solution is reclaimed ethanol to there not being the ethanol flavor, with ethyl acetate equal-volume extraction 3 times, merge the back and reclaim ethyl acetate to 1/4 of original volume;
2.3 with the alkali extraction, with aqueous slkali equal-volume extraction 3 times, merging the back is 5~6 with the diluted acid adjust pH earlier, placement is spent the night, and filters;
2.4 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the extracting solution after the extraction;
2.5 use ethanol purification, macroporous resin that will be by step 2.3 extracting solution is earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 10~60% carries out eluting with the consumption of column volume more than 10 times, collects eluent, and drying promptly gets Rhizoma Chuanxiong total phenols composition; Total phenol content 30%~99.9% in the Rhizoma Chuanxiong total phenols that makes wherein contains ferulic acid 10%~99.9%.
In the extracting method of above-mentioned Rhizoma Chuanxiong total phenols, concentration of ethanol and consumption, extraction time, extraction time are the principal elements that influences content of ferulic acid index in total phenols and the total phenols, carry out L by four factors, three levels 9(3 4) orthogonal test.Result of the test shows that wherein the influence of extraction time is the most remarkable, and preferred extraction time is 3 times; Concentration of alcohol and consumption take second place, and the concentration of preferred alcohol is 65~85%, and consumption is 11~13 times of Rhizoma Chuanxiong weight; The extraction time influence is less, and each 0.5h is advisable.Total phenol content is 80%~90% in the Rhizoma Chuanxiong total phenols that obtains by selection process, wherein contains ferulic acid 30%~60%.
Total phenols colorimetric method for determining in the Rhizoma Chuanxiong total phenols, ferulaic acid content is measured with the HPLC method.
Because total salvianolic acid and Rhizoma Chuanxiong total phenols composition are to thermally labile, so adopt freezing and drying lyophilization to carry out concentrate drying, soon the extracting solution concentrating under reduced pressure under low temperature behind the eluting purification is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process, the Rhizoma Chuanxiong total phenols that finally obtains being the total salvianolic acid of yellow loose crystalline powder and be light yellow crystalline powder.
The active component of Chinese medicine composition of the present invention and pharmaceutically acceptable carrier comprise excipient, as starch, water; Lubricant is as magnesium stearate; Disintegrating agent is as microcrystalline Cellulose; Filler is as lactose; Bonding agent, as pregelatinized Starch, dextrin etc., adopt method well known in the art to make various dosage forms, as tablet, capsule, granule, solution, syrup, injection, transfusion etc., take oral or injection (comprising intravenous injection, intravenous drip, intramuscular injection, subcutaneous injection), sticking know well route of administration such as analyse and carry out the treatment of cardiovascular and cerebrovascular disease.
For example, with aforementioned ratio according to a conventional method, described total salvianolic acid and Rhizoma Chuanxiong total phenols mixing back are carried out tabletting with tablet adjuvant mix homogeneously commonly used; Or in incapsulating with capsule adjuvant mix homogeneously commonly used; Or be mixed with injection with water for injection dissolving.
The cardiovascular and cerebrovascular disease that the medicine of above-mentioned Chinese medicine composition is controlled comprises: cerebral infarction, cerebral ischemia, coronary heart disease, angina pectoris, myocardial ischemia, myocardial infarction etc.
When being used for the patient, dosage is 15~250mg (in the total effective ingredient of compositions)/sky, and this dosage determines according to the situation of patient's age and body weight and symptom usually.
The present invention has following beneficial effect: the present invention has overcome that the Chinese medicine compound preparation becomes to be hard to tell, mechanism is not clear, the difficult control of quality, the unsteady shortcoming of curative effect.Chinese medicine composition effective ingredient of the present invention is clear and definite, and quality is controlled easily, and curative effect is reliable, and drug effect obviously is better than single with total salvianolic acid or Rhizoma Chuanxiong total phenols.
The specific embodiment
Embodiment one: the preparation tablets of Chinese medicine composition of the present invention
The preparation method of total salvianolic acid is as follows:
1.1 extract with percolation with acetone, the Radix Salviae Miltiorrhizae after having soaked more than 20 minutes is placed acetone, the concentration of acetone is 50%, its consumption is 9 times of Radix Salviae Miltiorrhizae weight; Then the acetone percolate is concentrated to about 1/10 of original volume, to there not being the acetone flavor;
1.2 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the acetone percolate after concentrating;
1.3 use ethanol purification, will be through the extracting solution of purification by macroporous resin earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 20% carries out eluting with the consumption of column volume more than 10 times, collects eluent, promptly gets the total salvianolic acid composition; Behind high concentration ethanol liquid flush away oil-soluble impurities, carry out the next round purification again;
1.4 carry out concentrate drying with freezing and drying lyophilization, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process :-50 ℃ of pre-freezes 3~4 hours,-10 ℃ of lyophilizing are warming up to 20 ℃ of insulations 2~3 hours, finally obtain being the total salvianolic acid of yellow loose crystalline powder.
Total phenolic content colorimetric method for determining in the total salvianolic acid, the salvianolic acid B magnesium salt content is measured with the HPLC method, and recording total phenolic content is 80%~100%, wherein contains salvianolic acid B magnesium 50%~100%.
The preparation method of Rhizoma Chuanxiong total phenols is as follows:
2.1 use alcohol reflux, be 65% ethanol with concentration, its consumption is that 11 times of Rhizoma Chuanxiong weight carry out hot reflux and extract, extraction time is 2 times;
2.2 use ethyl acetate extraction, extracting solution is reclaimed ethanol to there not being the ethanol flavor, with ethyl acetate equal-volume extraction 3 times, merge the back and reclaim ethyl acetate to 1/4 of original volume;
2.3 with the alkali extraction, with aqueous slkali equal-volume extraction 3 times, merging the back is 5-6 with the diluted acid adjust pH earlier, placement is spent the night, and filters;
2.4 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the extracting solution after the extraction;
2.5 use ethanol purification, will be through the extracting solution of purification by macroporous resin earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 10% carries out eluting with the consumption of column volume more than 10 times, collects eluent, promptly gets Rhizoma Chuanxiong total phenols composition; Behind high concentration ethanol liquid flush away oil-soluble impurities, carry out the next round purification again, total phenol content 30%~100% in the Rhizoma Chuanxiong total phenols that makes wherein contains ferulic acid 10%~100%;
2.6 carry out concentrate drying with freezing and drying lyophilization, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process :-50 ℃ of pre-freezes 3~4 hours,-10 ℃ of lyophilizing are warming up to 20 ℃ of insulations 2~3 hours, finally obtain being the Rhizoma Chuanxiong total phenols of light yellow crystalline powder.
Total phenol content colorimetric method for determining in the Rhizoma Chuanxiong total phenolic acids, ferulic acid is measured with the HPLC method, and recording total phenol content is 80%~100%, wherein contains ferulic acid 50%~100%.
Dosage is as follows:
1. the total salvianolic acid of above-mentioned gained and Rhizoma Chuanxiong total phenols
(being 1: 0.5 by weight ratio) 30g
2. starch 30g
3. lactose 40g
4. carboxymethyl starch sodium 5g
5. is starch slurry (7%) an amount of?
6. magnesium stearate 1% (1.25g)
Make 1000
Technology:
Get the total salvianolic acid and the Rhizoma Chuanxiong total phenols of above-mentioned dosage, pulverized 100 mesh sieves, with starch, lactose, the carboxymethyl starch sodium of above-mentioned dosage, pulverized 100 mesh sieves, mixing again.Total salvianolic acid and Rhizoma Chuanxiong total phenols are added in the starch and lactose of mixing mixing.Add the appropriate amount of starch slurry and mix thoroughly, granulate through 16 order ferrum silk screen nets, dry below 60 ℃, granulate adds the magnesium stearate mixing of above-mentioned dosage, analyzes tabletting behind the content.Can be made into 1000 every tablet tablet that contains 30mg total salvianolic acid and Rhizoma Chuanxiong total phenols.
Embodiment two: the capsule preparation of Chinese medicine composition of the present invention
The preparation method of total salvianolic acid is as follows:
1.1 extract with percolation with acetone, the Radix Salviae Miltiorrhizae after having soaked more than 20 minutes is placed acetone, the concentration of acetone is 60%, its consumption is 10 times of Radix Salviae Miltiorrhizae weight; Then the acetone percolate is concentrated to about 1/10 of original volume, to there not being the acetone flavor;
1.2 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the acetone percolate after concentrating;
1.3 use ethanol purification, will be through the extracting solution of purification by macroporous resin earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 30% carries out eluting with the consumption of column volume more than 10 times, collects eluent, promptly gets the total salvianolic acid composition; Behind high concentration ethanol liquid flush away oil-soluble impurities, carry out the next round purification again;
1.4 carry out concentrate drying with freezing and drying lyophilization, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process :-50 ℃ of pre-freezes 3~4 hours,-10 ℃ of lyophilizing are warming up to 20 ℃ of insulations 2~3 hours, finally obtain being the total salvianolic acid of yellow loose crystalline powder.
Total phenolic content colorimetric method for determining in the total salvianolic acid, the salvianolic acid B magnesium salt content is measured with the HPLC method, and recording total phenolic content is 80%~100%, wherein contains salvianolic acid B magnesium 50%~100%.
The preparation method of Rhizoma Chuanxiong total phenols is as follows:
2.1 use alcohol reflux, be 75% ethanol with concentration, its consumption is that 12 times of Rhizoma Chuanxiong weight carry out hot reflux and extract, extraction time is 3 times;
2.2 use ethyl acetate extraction, extracting solution is reclaimed ethanol to there not being the ethanol flavor, with ethyl acetate equal-volume extraction 3 times, merge the back and reclaim ethyl acetate to 1/4 of original volume;
2.3 with the alkali extraction, with aqueous slkali equal-volume extraction 3 times, merging the back is 5-6 with the diluted acid adjust pH earlier, placement is spent the night, and filters;
2.4 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the extracting solution after the extraction;
2.5 use ethanol purification, will be through the extracting solution of purification by macroporous resin earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 40% carries out eluting with the consumption of column volume more than 10 times, collects eluent, promptly gets Rhizoma Chuanxiong total phenols composition; Behind high concentration ethanol liquid flush away oil-soluble impurities, carry out the next round purification again, total phenol content 30%~100% in the Rhizoma Chuanxiong total phenols that makes wherein contains ferulic acid 10%~100%;
2.6 carry out concentrate drying with freezing and drying lyophilization, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process :-50 ℃ of pre-freezes 3~4 hours,-10 ℃ of lyophilizing are warming up to 20 ℃ of insulations 2~3 hours, finally obtain being the Rhizoma Chuanxiong total phenols of light yellow crystalline powder.
Total phenol content colorimetric method for determining in the Rhizoma Chuanxiong total phenolic acids, ferulic acid is measured with the HPLC method, and recording total phenol content is 80%~100%, wherein contains ferulic acid 50%~100%.
Dosage is as follows:
1. above-mentioned total salvianolic acid and Rhizoma Chuanxiong total phenols
(being 1: 5 by weight ratio) 30g
2. starch 160g
3. micropowder silica gel 10g
Make 1000
Technology:
Get the total salvianolic acid and the acid of Rhizoma Chuanxiong total phenols accumulated snow of above-mentioned dosage, pulverized 100 mesh sieves, add in the starch, micropowder silica gel of above-mentioned dosage, mixing directly incapsulates, and can be made into 1000 every capsule that contains 30mg total salvianolic acid and Rhizoma Chuanxiong total phenols.
Embodiment three: the preparation of Chinese medicine composition composition injection of the present invention
The preparation method of total salvianolic acid is as follows:
1.1 extract with percolation with acetone, the Radix Salviae Miltiorrhizae after having soaked more than 20 minutes is placed acetone, the concentration of acetone is 70%, its consumption is 12 times of Radix Salviae Miltiorrhizae weight; Then the acetone percolate is concentrated to about 1/10 of original volume, to there not being the acetone flavor;
1.2 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the acetone percolate after concentrating;
1.3 use ethanol purification, will be through the extracting solution of purification by macroporous resin earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 40% carries out eluting with the consumption of column volume more than 10 times, collects eluent, promptly gets the total salvianolic acid composition; Behind high concentration ethanol liquid flush away oil-soluble impurities, carry out the next round purification again;
1.4 carry out concentrate drying with freezing and drying lyophilization, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process :-50 ℃ of pre-freezes 3~4 hours,-10 ℃ of lyophilizing are warming up to 20 ℃ of insulations 2~3 hours, finally obtain being the total salvianolic acid of yellow loose crystalline powder.
Total phenolic content colorimetric method for determining in the total salvianolic acid, the salvianolic acid B magnesium salt content is measured with the HPLC method, and recording total phenolic content is 80%~100%, wherein contains salvianolic acid B magnesium 50%~100%.
The preparation method of Rhizoma Chuanxiong total phenols is as follows:
2.1 use alcohol reflux, be 85% ethanol with concentration, its consumption is that 13 times of Rhizoma Chuanxiong weight carry out hot reflux and extract, extraction time is 5 times;
2.2 use ethyl acetate extraction, extracting solution is reclaimed ethanol to there not being the ethanol flavor, with ethyl acetate equal-volume extraction 3 times, merge the back and reclaim ethyl acetate to 1/4 of original volume;
2.3 with the alkali extraction, with aqueous slkali equal-volume extraction 3 times, merging the back is 5-6 with the diluted acid adjust pH earlier, placement is spent the night, and filters;
2.4 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the extracting solution after the extraction;
2.5 use ethanol purification, will be through the extracting solution of purification by macroporous resin earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 60% carries out eluting with the consumption of column volume more than 10 times, collects eluent, promptly gets Rhizoma Chuanxiong total phenols composition; Behind high concentration ethanol liquid flush away oil-soluble impurities, carry out the next round purification again, total phenol content 30%~100% in the Rhizoma Chuanxiong total phenols that makes wherein contains ferulic acid 10%~100%;
2.6 carry out concentrate drying with freezing and drying lyophilization, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process :-50 ℃ of pre-freezes 3~4 hours,-10 ℃ of lyophilizing are warming up to 20 ℃ of insulations 2~3 hours, finally obtain being the Rhizoma Chuanxiong total phenols of light yellow crystalline powder.
Total phenol content colorimetric method for determining in the Rhizoma Chuanxiong total phenolic acids, ferulic acid is measured with the HPLC method, and recording total phenol content is 80%~100%, wherein contains ferulic acid 50%~100%.
Get above-mentioned weight proportion and be 1: 10 total salvianolic acid and Rhizoma Chuanxiong total phenols 150g, add the dissolving of injection water, be mixed with the 10000ml medicinal liquid according to a conventional method, filtration, fine straining, embedding, sterilization, check, 10ml/ prop up 1000 of injections.

Claims (7)

1, a kind of active ingredient of Chinese herbs compositions of preventing and treating cardiovascular and cerebrovascular disease, comprise active component and medically acceptable carrier, described by weight percentage active component is 0.1~99.9%, carrier is 0.1~99.9%, it is characterized in that: described active component is the extract total salvianolic acid of Radix Salviae Miltiorrhizae and the extract Rhizoma Chuanxiong total phenols of Rhizoma Chuanxiong, and total salvianolic acid and Rhizoma Chuanxiong total phenols are 1: 0.1~15 by weight ratio; Total phenolic content is 30%~99.9% in the total salvianolic acid, wherein contains salvianolic acid B magnesium 10%~99.9%; Total phenol content 30%~99.9% in the Rhizoma Chuanxiong total phenols, wherein contains ferulic acid 10%~99.9%.
2, the active ingredient of Chinese herbs compositions of control cardiovascular and cerebrovascular disease according to claim 1 is characterized in that: described by weight percentage active component is 0.1~30%, and carrier is 70~99.9%.
3, the active ingredient of Chinese herbs compositions of control cardiovascular and cerebrovascular disease according to claim 1 and 2 is characterized in that: total salvianolic acid and Rhizoma Chuanxiong total phenols are 1: 0.5~10 by weight ratio; Total phenolic content is 80%~90% in the total salvianolic acid, wherein contains salvianolic acid B magnesium 50%~80%; Total phenol content is 80%~90% in the Rhizoma Chuanxiong total phenolic acids, wherein contains ferulic acid 30%~60%.
4, the active ingredient of Chinese herbs preparation of compositions method of the described control cardiovascular and cerebrovascular disease of claim 1, it is characterized in that: at first from Radix Salviae Miltiorrhizae, extract total salvianolic acid and from Rhizoma Chuanxiong, extract the Rhizoma Chuanxiong total phenols, total salvianolic acid and Rhizoma Chuanxiong total phenols are mixed to scale as active component, mix with medically acceptable carrier according to a conventional method then and carry out preparation;
The method of wherein extracting total salvianolic acid from Radix Salviae Miltiorrhizae is as follows:
1.1 extract with percolation with acetone, the Radix Salviae Miltiorrhizae after soaking is placed acetone, the concentration of acetone is 30~80%, its consumption is more than 8 times of Radix Salviae Miltiorrhizae weight; Then the acetone percolate is concentrated to about 1/10 of original volume, to there not being the acetone flavor;
1.2 use purification by macroporous resin, with the acetone percolate after concentrating, to extract liquid measure and amount of resin be that 1: 1 ratio is passed through macroporous resin column according to concentrating the back;
1.3 use ethanol purification, macroporous resin that will be by extracting solution is earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 10~60% carries out eluting with the consumption of column volume more than 10 times, collects eluent, and drying promptly gets the total salvianolic acid composition; Total phenolic content is 30%~99.9% in the total salvianolic acid that makes, and wherein contains salvianolic acid B magnesium 10%~99.9%;
The method of extracting the Rhizoma Chuanxiong total phenols from Rhizoma Chuanxiong is as follows:
2.1 use alcohol reflux, be 40%~90% ethanol with concentration, its consumption is that the hot reflux of carrying out more than 10 times of Rhizoma Chuanxiong weight is extracted, extraction time is 2~5 times;
2.2 use ethyl acetate extraction, extracting solution is reclaimed ethanol to there not being the ethanol flavor, with ethyl acetate equal-volume extraction 3 times, merge the back and reclaim ethyl acetate to 1/4 of original volume;
2.3 with the alkali extraction, with aqueous slkali equal-volume extraction 3 times, merging the back is 5~6 with the diluted acid adjust pH earlier, placement is spent the night, and filters;
2.4 use purification by macroporous resin,, be that 1: 1 ratio is passed through macroporous resin column according to extracting liquid measure and amount of resin with the extracting solution after the extraction;
2.5 use ethanol purification, macroporous resin that will be by step 2.3 extracting solution is earlier with the deionized-distilled water eluting, the alcoholic solution of reuse 10~60% carries out eluting with the consumption of column volume more than 10 times, collects eluent, and drying promptly gets Rhizoma Chuanxiong total phenols composition; Total phenol content 30%~99.9% in the Rhizoma Chuanxiong total phenols that makes wherein contains ferulic acid 10%~99.9%.
5, according to the active ingredient of Chinese herbs preparation of compositions method of the described control cardiovascular and cerebrovascular disease of claim 4, it is characterized in that: the concentration of acetone is 50~70% in the described step 1.1, and its consumption is 9~12 times of Radix Salviae Miltiorrhizae weight; Concentration of ethanol is 20~40% in the described step 1.3.
6, according to the active ingredient of Chinese herbs preparation of compositions method of the described control cardiovascular and cerebrovascular disease of claim 4, it is characterized in that: concentration of ethanol is 65~85% in the described step 2.1, and its consumption is 11~13 times of Rhizoma Chuanxiong weight, and extraction time is 3 times.
7, active ingredient of Chinese herbs preparation of compositions method according to the described control cardiovascular and cerebrovascular disease of claim 4, it is characterized in that: the Rhizoma Chuanxiong total phenols that total salvianolic acid that described step 1.3 is made and step 2.5 make adopts freezing and drying lyophilization to carry out concentrate drying respectively, extracting solution behind eluting purification concentrating under reduced pressure under low temperature is removed ethanol, continue to be concentrated into about 1/10 of original volume, with 0.45 μ m filtering with microporous membrane, then concentrated solution is carried out drying according to conventional freeze-dry process, the Rhizoma Chuanxiong total phenols that finally obtains being the total salvianolic acid of yellow loose crystalline powder and be light yellow crystalline powder.
CN 200410026913 2004-04-21 2004-04-21 Combination of active constituent of Chinese traditional medicine for curing cardiovascular and cerebrovascular diseases and preparation method Pending CN1562285A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106265907A (en) * 2016-09-05 2017-01-04 神威药业集团有限公司 A kind of GUANXINNING pharmaceutical composition and preparation method thereof
CN113082014A (en) * 2021-04-27 2021-07-09 正大青春宝药业有限公司 Salvianolic acid B compound and preparation and application thereof
CN115501267A (en) * 2022-09-23 2022-12-23 扬州大学 Application of salvia miltiorrhiza-ligusticum chuanxiong hort composite preparation in preparation of medicine for treating nerve injury
WO2024113586A1 (en) * 2022-11-29 2024-06-06 神威药业集团有限公司 Method for preparing guanxinning composition

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106265907A (en) * 2016-09-05 2017-01-04 神威药业集团有限公司 A kind of GUANXINNING pharmaceutical composition and preparation method thereof
CN106265907B (en) * 2016-09-05 2019-07-05 神威药业集团有限公司 A kind of perhexiline pharmaceutical composition and preparation method thereof
CN113082014A (en) * 2021-04-27 2021-07-09 正大青春宝药业有限公司 Salvianolic acid B compound and preparation and application thereof
CN115501267A (en) * 2022-09-23 2022-12-23 扬州大学 Application of salvia miltiorrhiza-ligusticum chuanxiong hort composite preparation in preparation of medicine for treating nerve injury
WO2024113586A1 (en) * 2022-11-29 2024-06-06 神威药业集团有限公司 Method for preparing guanxinning composition

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