CN100518802C - Extraction of effective parts for Danshen root and rhizoma chuanxiong - Google Patents
Extraction of effective parts for Danshen root and rhizoma chuanxiong Download PDFInfo
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- CN100518802C CN100518802C CNB2005100492929A CN200510049292A CN100518802C CN 100518802 C CN100518802 C CN 100518802C CN B2005100492929 A CNB2005100492929 A CN B2005100492929A CN 200510049292 A CN200510049292 A CN 200510049292A CN 100518802 C CN100518802 C CN 100518802C
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Abstract
A process for extracting the active components from red sage root and Chuan-xiong rhizome to prepare Chinese medicine 'Guanxinning' for preventing and treating cardiovascular and cerebrovascular diseases includes such steps as extracting in water or alcohol solution at 40-100 deg.C 1-5 times, collecting liquid extract, purifying, vacuum concentrating and drying.
Description
(1) technical field
The present invention relates to the extracting method of the Chinese medicine compound GUANXINNING effective site formed by Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong.
(2) background technology
Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong and the various preparations that comprise this medicine thereof are clinical treatment cardiovascular and cerebrovascular disease Chinese medicine commonly used.From the eighties to by Radix Salviae Miltiorrhizae, the liquid drugs injection that the compound recipe that Rhizoma Chuanxiong is formed is made has carried out clinical research, passed through the efficacy analysis of 387 examples, demonstration is by the blood circulation promoting medicine Radix Salviae Miltiorrhizae, the compound injection treatment angina pectoris that Rhizoma Chuanxiong is formed truly has curative effect preferably, treatment back angina pectoris disease effective percentage is 91.73%, undesired electrocardiogram effective percentage is 44.39%, angina pectoris symptom is light, in, effective percentage is roughly the same in the different classifications of severe, point out this liquid drugs injection not only to gently, medium-sized angina pectoris case effectively and to heavy angina pectoris case has curative effect preferably equally, treatment back angina pectoris symptom at large within a short period of time (1～4 week) controlled.5 examples are treated front and back Capacity Plan and Electrocardiographic phenomenon because of the patients with coronary heart disease of this liquid drugs injection treatment, and the result illustrates that tentatively this liquid drugs injection has certain cardiotonic, and the effect that increases cardiac output is arranged, and tiny tremulous pulse is had dilating effect.Have the coronary circulation of improvement and anticoagulant effect thereby further illustrate this liquid drugs injection, significantly coronary blood flow increasing improves blood supply of cardiac muscle, and the formation of prevention and minimizing thrombosis is dwindled the thromboembolism scope, and lesion degree alleviates.
At present, water soluble ingredient to Radix Salviae Miltiorrhizae has carried out systematic study, separate and obtain salvianolic acid A (1), B (2), C (3), D (4), E (5), F (8), G (9), H (11), I (12), J (13), the glycoside phenolic acid compounds such as (14) of rosmarinic acid (6), shikonin (7), different salvianolic acid (10), rosmarinic acid.(Lian-niang.Li，J.chinese?pharmacenticalsciences?1997.6，57～64)。The pharmacological results illustrates that these phenolic acid compounds have very strong anti peroxidation of lipid, antithrombotic, improve effects such as blood circulation.Water soluble ingredient to Rhizoma Chuanxiong also has more detailed research, and the ligustrazine of separation and Extraction and ferulic acid from Rhizoma Chuanxiong are synthetic, and are widely used in clinical.
At present, the dosage form of the compound effective component of being made up of Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong is single liquid drugs injection; Instability because of the phenolic acid compound chemical property, in preparation and storage process, easily decompose rotten, so the contained composition of the liquid drugs injection of present clinical usefulness is mainly active more weak danshensu and protocatechualdehyde, and active other stronger salvianolic acid constituents, decompose rotten remaining little because of technology heated time length causes as salvianolic acid B, ferulic acid, pharmacologically active is had a greatly reduced quality.
(3) summary of the invention
The present invention is to be the extracting method of Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese for a kind of stable performance, GUANXINNING that pharmacologically active is good are provided.
For reaching goal of the invention the technical solution used in the present invention be:
The extracting method of a kind of Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese is characterized in that described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong mass ratio are 1:1, and described method is carried out as follows:
(1) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces add water or the pure aqueous solution that quality is 3～20 times of quality of medicinal materials, extract 1～5 time down at 40～100 ℃, and merge extractive liquid, promptly gets medicinal liquid;
(2) step (1) gained medicinal liquid is carried out purification;
(3) step (2) gained medicinal liquid is drying to obtain Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese extract at 30～80 ℃ of following concentrating under reduced pressure.
Described purification removal of impurity step is a precipitate with ethanol.
Described purification removal of impurity step is last macroporous adsorbent resin eluting.
Described purification removal of impurity step also can be precipitate with ethanol and last macroporous adsorbent resin eluting hockets.
Described macroporous adsorbent resin is a styrene tyle macroporous adsorption resin.
Drying is drying under reduced pressure, carries out under 30～80 ℃ in the described step (3).
Drying is a spray drying in the described step (3).
Especially, described method is carried out as follows:
(1) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces add water or the pure aqueous solution that quality is 3～20 times of quality of medicinal materials, extract 1～5 time down at 40～100 ℃, and merge extractive liquid, promptly gets medicinal liquid;
(2) to be evaporated to concentration under 30～80 ℃ be 0.5～5g/mL to step (1) gained medicinal liquid, and it is 40～90% to containing the alcohol amount that concentrated solution adds alcohol, leaves standstill, and precipitate with ethanol 1～5 time is drawn supernatant, filters, and promptly gets medicinal liquid;
(3) step (2) gained medicinal liquid promptly gets Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese extract at 30～80 ℃ of following concentrating under reduced pressure at 30～80 ℃ of following drying under reduced pressure.
Perhaps, described method is carried out as follows:
(1) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces are in the aqueous solution of the water of 3～20 times of quality of medicinal materials or alcohol in quality, 40～100 ℃ down extract 1～5 time after, merge extractive liquid, promptly gets medicinal liquid;
(2) macroporous adsorbent resin is gone up in the centrifugal back of step (1) gained medicinal liquid, and after being washed till effluent and not having alphanaphthol reaction with deionized water, reuse 10～90% ethanol elutions to eluent does not have tangible phenolic hydroxyl group reaction;
(3) the gained medicinal liquid promptly gets described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese at 30～80 ℃ of following concentrating under reduced pressure at 30～80 ℃ of following drying under reduced pressure.
Further, described method is carried out as follows:
A) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces are in the water or 50～85% ethanol water of 8～14 times of quality of medicinal materials in quality, 40～100 ℃ extract 2～3 times down after, merge extractive liquid, promptly gets medicinal liquid;
B) to be evaporated to concentration under 40～65 ℃ be 1.5～3g/mL to step (1) gained medicinal liquid, and it is 60～85% to containing the alcohol amount that concentrated solution adds ethanol, leaves standstill, and precipitate with ethanol 2～3 times filters, and promptly gets medicinal liquid;
C) the gained medicinal liquid is at 40～65 ℃ of following concentrating under reduced pressure, and 40～65 ℃ of following drying under reduced pressure promptly get described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese.
Or described method is carried out as follows:
(1) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces are in the aqueous solution of the water of 3～20 times of quality of medicinal materials or alcohol in quality, 40～100 ℃ down extract 1～5 time after, merge extractive liquid, promptly gets medicinal liquid;
(2) to be evaporated to concentration under 30～80 ℃ be 0.5～5g/mL to step (1) gained medicinal liquid, and it is 40～90% to containing the alcohol amount that concentrated solution adds alcohol, leaves standstill, and precipitate with ethanol 1～5 time is drawn supernatant, promptly gets medicinal liquid;
(3) step (2) gained medicinal liquid adds suitable quantity of water dissolving gained medicinal liquid behind decompression recycling ethanol, after centrifugal, medicinal liquid is gone up earlier macroporous adsorbent resin, after being washed till effluent and not having alphanaphthol reaction with deionized water, reuse 10～90% ethanol elutions to eluent does not have tangible phenolic hydroxyl group reaction, collects eluent;
(4) the gained eluent is at 30～80 ℃ of following concentrating under reduced pressure, and 30～80 ℃ of following drying under reduced pressure promptly get described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese.
Further, described method is carried out as follows:
(1) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces are in the water or 50～85% ethanol water of 8～14 times of quality of medicinal materials in quality, 40～100 ℃ extract 2～3 times down after, merge extractive liquid, promptly gets medicinal liquid;
(2) to be evaporated to concentration under 40～65 ℃ be 1.5～3g/mL to step (1) gained medicinal liquid, and it is 60～85% to containing the alcohol amount that concentrated solution adds ethanol, leaves standstill, and precipitate with ethanol 1～3 time is drawn supernatant, filters, and promptly gets medicinal liquid;
(3) step (2) gained medicinal liquid adds suitable quantity of water dissolving gained medicinal liquid behind decompression recycling ethanol, after centrifugal, medicinal liquid is gone up styrene tyle macroporous adsorption resin earlier, after being washed till effluent and not having alphanaphthol reaction with deionized water, reuse 10～90% ethanol elutions to eluent does not have tangible phenolic hydroxyl group reaction, collects eluent;
(4) the gained eluent is at 40～65 ℃ of following concentrating under reduced pressure, and 40～65 ℃ of following drying under reduced pressure promptly get described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese.
The beneficial effect of the extracting method of Radix Salviae Miltiorrhizae of the present invention and Rhizoma Chuanxiong effective ingredient in Chinese is mainly reflected in: (1) technical process is simple, do not need High Temperature High Pressure and special installation, safety, easy operating, and cost is low, use extracting method of the present invention, a large amount of protein that can be removed, saccharide, impurity such as starch, the content height of total phenolic acid, impurity is few, because the strict temperature of having controlled extraction and concentration process, its effective site content is more than 60%, wherein the content of salvianolic acid B occupies 5～50% of effect position, and physiologically active is strong; (2) utilize not only steady quality of Radix Salviae Miltiorrhizae that the inventive method obtains, Rhizoma Chuanxiong total phenolic acids, and be rich in the active component of salviamiltiorrhizabung and Rhizoma Chuanxiong, have anti-cerebral ischemia, pharmacological actions such as anti-apoptotic, therefore can be used for preparing good effect, safe and reliable control cardiovascular and cerebrovascular diseases medicament.
(4) specific embodiment
The present invention is described further below in conjunction with specific embodiment:
Embodiment 1: Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong effective site are extracted
Radix Salviae Miltiorrhizae, each 5kg decoction pieces of Rhizoma Chuanxiong add deionized water and soaked 24 hours at 50 ℃, and 60 ℃ of temperature are carried 3 times, respectively add 80L, 60L, 60L water, and each samming is carried 2 hours, and extracting solution is evaporated to 10L at 50 ℃, adds 80% ethanol 14L after the cooling, and standing over night is filtered.Decompression filtrate recycling ethanol, the gained concentrated solution is by AB-8 type macroporous adsorbent resin, be washed till alphanaphthol reaction with deionized water, continue to add ferric chloride potassium ferricyanide reagent and do not have tangible phenolic hydroxyl group reaction with 70% ethanol elution to eluent, eluent is evaporated under 40 ℃ in right amount, 40 ℃ of following drying under reduced pressure promptly get 150 gram Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong total phenolic acids.
The detection method of total phenolic acid and salvianolic acid B:
(1) salvianolic acid B: measure with the HPLC method, detect wavelength 285nm, the standard substance salvianolic acid B is provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
(2) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong total phenolic acids: content=F (A-B)-B
Wherein: A is that spectrophotometry is total phenolic content that contrast is calculated with the salvianolic acid B
B is the content of danshinolic acid B of high effective liquid chromatography for measuring
F is a correction factor
Total phenolic acid is except salvianolic acid B (molecular weight 718), also contain protocatechualdehyde (molecular weight 138), danshensu (molecular weight 162), alkannic acid (molecular weight 538), caffeic acid (molecular weight 180), ferulic acid phenolic acid compounds such as (molecular weight 194), the molecular weight between them differs bigger.Being that contrast is higher with total phenolic content result of spectrophotometry with the salvianolic acid B, mainly is because the molecular weight of other phenolic acid compounds is lower than due to the molecular weight of salvianolic acid B.Therefore, with the ratio of above-mentioned 6 phenolic acid compound mean molecule quantities and salvianolic acid B molecular weight as correction factor, the total phenolic content after proofreading and correct with this with measure 6 phenolic acid compound content sum basically identicals such as protocatechualdehyde respectively with the HPLC method.
Ferulic acid, protocatechualdehyde, danshensu, caffeic acid, alkannic acid, salvianolic acid B are provided by Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Testing result: every gram dry extract contains 0.325 gram salvianolic acid B; Every gram dry extract contains the total phenolic acid of 0.826 gram.
Embodiment 2: Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong effective site are extracted
Radix Salviae Miltiorrhizae, each 5kg decoction pieces of Rhizoma Chuanxiong add water 100 ℃ of heating extraction 3 times.For the first time add 80L water, heated 2 hours, second and third time respectively adds 60L water, heats respectively 1.5 hours.Extracting solution adds 95% ethanol and reaches 75% to containing the alcohol amount at 60 ℃ of decompression 6.7L after the cooling, standing over night is filtered.Decompression filtrate recycling ethanol, 60 ℃ are evaporated in right amount, and 60 ℃ of following drying under reduced pressure promptly get Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong total phenolic acids dry powder 1.3Kg.
Embodiment 3: Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong effective site are extracted
Radix Salviae Miltiorrhizae, each 5kg decoction pieces of Rhizoma Chuanxiong add 70% alcohol reflux 3 times, add 70% ethanol 40L for the first time, heat 2 hours, and second and third time respectively adds 30L water, heats respectively 2 hours.Extracting solution adds 95% ethanol and reaches 75% to containing the alcohol amount at 60 ℃ of decompression 6.7L after the cooling, standing over night is filtered.Decompression filtrate recycling ethanol is concentrated into 5L, adds 95% ethanol after the cooling and reaches 90% to containing the alcohol amount, and standing over night is filtered, and filtrate is evaporated in right amount for 60 ℃, and spray drying promptly gets Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong total phenolic acids dry powder 0.7Kg.
Claims (1)
1. the extracting method of Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese is characterized in that described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong mass ratio are 1:1, and described method is carried out as follows:
(1) Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong decoction pieces are in the water of 8～14 times of quality of medicinal materials in quality, and after extracting 2～3 times under 40～100 ℃, merge extractive liquid, promptly gets medicinal liquid;
(2) to be evaporated to concentration under 40～65 ℃ be 1.5～3g/mL to step (1) gained medicinal liquid, and it is 60～85% to containing the alcohol amount that concentrated solution adds ethanol, leaves standstill, and precipitate with ethanol 1～3 time is drawn supernatant, filters, and promptly gets medicinal liquid;
(3) the gained medicinal liquid is at 40～65 ℃ of following concentrating under reduced pressure, and 40～65 ℃ of following drying under reduced pressure promptly get described Radix Salviae Miltiorrhizae and Rhizoma Chuanxiong effective ingredient in Chinese.
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| 中华人民共和国卫生部药品标准中药成方制剂. 中华人民共和国卫生部药典委员会，174. 1998 |
| 中华人民共和国卫生部药品标准中药成方制剂. 中华人民共和国卫生部药典委员会，174. 1998 * |
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