CN107260803A - The preparation method of Sodium Danshensu content in a kind of raising red sage roo drip liquid - Google Patents
The preparation method of Sodium Danshensu content in a kind of raising red sage roo drip liquid Download PDFInfo
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Abstract
The present invention relates to new technical field of traditional Chinese medicine preparation, a kind of preparation method for improving Sodium Danshensu content in red sage roo drip liquid is disclosed, the red sage roo drip liquid is prepared from by major ingredient and auxiliary material, major ingredient is the red sage root, shared mass percent is 70 80%, remaining as auxiliary material, is consisted of the following composition：The processing and treating method of water for injection, glucose, sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root comprises the following steps：（1）In the decoction step of the red sage root, decoction number of times is reduced, stirring number of times is added, while with the addition of yellow rice wine, the active ingredient of the red sage root can be made to be dissolved in decoction liquor rapidly, it is to avoid destruction of the multiple decoction to danshensu and other active ingredients；（2）It is distributed to by compared with low temperature alcohol extracting, alcohol soluble substance can twice be destroyed in extract solution, recovery rate is improved；（3）In PH regulation, the degree and sequencing of regulation have a great impact for danshensu and impurity content.
Description
Technical field
The invention belongs to new technical field of traditional Chinese medicine preparation, and in particular to one kind improves Sodium Danshensu content in red sage roo drip liquid
Preparation method.
Background technology
Red sage roo drip liquid is salviamiltiorrhizabung preparation, with work(such as promoting blood circulation and removing blood stasis, freeing vessels and nourishing heart, activating blood circulation and reducing swelling, nourishing blood and tranquilization
Effect, is clinically used for treatment coronary heart diseases and angina pectoris, the disease such as feel oppressed in the heart.The active component of the red sage root has water-soluble phenolic acids and fat
Dissolubility diterpene quinones.Active ingredient in red sage roo drip liquid is to extract water-soluble phenolic the acrylic component such as danshensu, original in the red sage root
Catechu aldehyde, protocatechuic acid, Rosmarinic acid, methyl rosmarinate, alkannic acid, caffeic acid, Salvia japonica row alcohol and salviandic acid A, B,
C etc..Danshensu can substantially suppress hematoblastic aggregation, and substantially increase the mobility of platelet membrane, point out it to have coronary heart disease
Effect.Shi Jutong etc. reports that danshensu can improve the negative electrical charge of red blood cell, makes to be difficult aggregation each other；WBV is reduced, is suppressed
Platelet aggregation, pays plasmin system living；Increase the mechanical strength of erythrocyte membrane, reduce the destruction of red blood cell.Heavy dose of red sage root
Element can increase fragility of blood vessels, and this may have platelet aggregation-against with danshensu and promote fiber degradation function relevant.Danshensu
The fibrinolytic of body can be improved, improves hemorheological property, improve the deformability of red blood cell and reconcile the viscosity of blood, change
Each internal organs of kind whole body（Heart, liver, lungs and pancreas that especially medicine is arrived first at) microcirculation disorder, contribute to body
The correction of the severe complication such as the rehabilitation of tissue and adult respiratory distress syndrome (ARDS).Danshensu is unstable in nature, therefore
It is made in red sage roo drip liquid sodium salt, effect is as danshensu, but in existing process technology, the handling process of the red sage root
Destruction for content of Danshensu is very serious, and in decoction, alcohol precipitation, soda acid processing, phenol acid ingredient is by a certain degree of
Influence.
The content of the invention
The purpose of the present invention for it is existing the problem of there is provided it is a kind of raising red sage roo drip liquid in Sodium Danshensu content
Preparation method, can targetedly improve technological process, and the content of Sodium Danshensu is maintained at into highest level.
The present invention is achieved by the following technical solutions：
The preparation method of Sodium Danshensu content in a kind of raising red sage roo drip liquid, the red sage roo drip liquid prepared by major ingredient and auxiliary material and
Into major ingredient is the red sage root, and shared mass percent is 70-80%, remaining as auxiliary material, is consisted of the following composition：Water for injection, grape
The processing and treating method of sugar, sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root comprises the following steps：
（1）The Danshen Tablets for selecting high-quality are cleaned up, ultramicro grinding to 50-80 mesh, add the clear water of 10-15 times of volume,
Decocted 1-2 hours at 110-120 DEG C, it is in decoction every stirring in 10-20 minutes once, a length of 3-5 minutes during stirring every time, stirring
While mixing, the yellow rice wine that volume fraction is 0.4-0.6% is added dropwise, after decoction terminates, filters while hot, obtained filtrate is by decompression
Relative density is concentrated into for 1.16-1.17；
（2）The ethanol of 10-12 times of volume is added into the filtrate of above-mentioned gained, is soaked 20-25 minutes, is flowed back at 60-70 DEG C
Extract 1-2 hours, filtering adds 3-5 times of volume into obtained filter residue, the alcohol of same concentrations flows back at the same temperature
Extract 1-1.2 hours, filtering, the filtered fluid that 2 times are obtained merges, remove alcohol by being concentrated under reduced pressure, obtain Salvia mitiorrhiza liquid standby；
（3）The pH value of Salvia mitiorrhiza liquid, first step are adjusted for 30-40% sodium hydroxide solution using the mass fraction newly prepared
Save as 8.5-9.5, then heating is boiled, and maintains fluidized state 10-20 minute, reuse hydrochloric acid of the molar concentration for 1-2mol/L
PH to 5.5-6.5 is adjusted, ethanol is added after cooling, alcohol content is reached 50-60%, after stirring, refrigerates 4-6 hours, carries out
It is concentrated under reduced pressure except alcohol, is handled using activated carbon decolorizing and produce red sage root refined liquid.
It is used as further improvement of these options, step（1）Described filtrate relative density is determined at 70 DEG C.
It is used as further improvement of these options, step（2）The mass concentration of used ethanol is 80-90%.
It is used as further improvement of these options, step（3）In be concentrated under reduced pressure into relative density for 1.12-1.14.
Wherein the consumption of auxiliary material is scaled with major ingredient equal proportion.
The present invention has advantages below compared with prior art：The preparation of Sodium Danshensu content in a kind of raising red sage roo drip liquid
Method, the red sage roo drip liquid is prepared from by major ingredient and auxiliary material, and major ingredient is the red sage root, and shared mass percent is 70-80%, remaining
For auxiliary material, consist of the following composition：Water for injection, glucose, sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root
Processing and treating method comprise the following steps：（1）In the decoction step of the red sage root, decoction number of times is reduced, is increased in decoction
Stirring number of times, while with the addition of yellow rice wine, can be such that the active ingredient of the red sage root is dissolved in decoction liquor rapidly, it is to avoid repeatedly decoct
Boil the destruction to danshensu and other active ingredients；（2）By compared with low temperature alcohol extracting, can make twice alcohol soluble substance not be destroyed and
It is distributed in extract solution, recovery rate is improved；（3）Found through overtesting, in PH regulation, the degree and priority of regulation
Order has a great impact for danshensu and impurity content, and the variation tendency of Sodium Danshensu and protocatechualdehyde is much like, only
Be Sodium Danshensu content it is larger compared to the content of protocatechualdehyde, therefore both can be combined discussions, because the two is heated
It is all unstable, therefore in order to avoid concentration is removed in alcohol, component content has declined, and pH value adjusting method of the invention inhibits two
The phenolic hydroxyl group ionization of person, improves its content.
Embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
The preparation method of Sodium Danshensu content in a kind of raising red sage roo drip liquid, the red sage roo drip liquid prepared by major ingredient and auxiliary material and
Into major ingredient is the red sage root, and shared mass percent is 70%, remaining as auxiliary material, is consisted of the following composition：Water for injection, glucose,
The processing and treating method of sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root comprises the following steps：
（1）The Danshen Tablets for selecting high-quality are cleaned up, ultramicro grinding to 50 mesh, add the clear water of 10 times of volumes, are decocted at 110 DEG C
Boil 1 hour, in decoction every stirring in 10 minutes once, every time a length of 3 minutes during stirring, while stirring, volume integral is added dropwise
Number is 0.4% yellow rice wine, after decoction terminates, is filtered while hot, and obtained filtrate is 1.16 by being concentrated under reduced pressure into relative density；
（2）The ethanol of 10 times of volumes is added into the filtrate of above-mentioned gained, is soaked 20 minutes, refluxing extraction 1 hour at 60 DEG C,
Filtering, alcohol refluxing extraction 1 hour, mistake at the same temperature of 3 times of volumes, same concentrations are added into obtained filter residue
Filter, the filtered fluid that 2 times are obtained merges, and removes alcohol by being concentrated under reduced pressure, obtains Salvia mitiorrhiza liquid standby；
（3）Using pH value of the mass fraction newly prepared for 30% sodium hydroxide solution regulation Salvia mitiorrhiza liquid, tentatively it is adjusted to
8.5, then heating is boiled, and maintains fluidized state 10 minutes, is reused the hydrochloric acid that molar concentration is 1mol/L and is adjusted PH to 5.5,
Ethanol is added after cooling, alcohol content is reached 50%, after stirring, refrigerates 4 hours, is concentrated under reduced pressure except alcohol, uses activity
Carbon decoloring processing produces red sage root refined liquid.
It is used as further improvement of these options, step（1）Described filtrate relative density is determined at 70 DEG C.
It is used as further improvement of these options, step（2）The mass concentration of used ethanol is 80%.
It is used as further improvement of these options, step（3）In be concentrated under reduced pressure into relative density for 1.12.
Embodiment 2
The preparation method of Sodium Danshensu content in a kind of raising red sage roo drip liquid, the red sage roo drip liquid prepared by major ingredient and auxiliary material and
Into major ingredient is the red sage root, and shared mass percent is 75%, remaining as auxiliary material, is consisted of the following composition：Water for injection, glucose,
The processing and treating method of sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root comprises the following steps：
（1）The Danshen Tablets for selecting high-quality are cleaned up, ultramicro grinding to 65 mesh, add the clear water of 12 times of volumes, are decocted at 115 DEG C
Boil 1.5 hours, in decoction every stirring in 15 minutes once, every time a length of 4 minutes during stirring, while stirring, volume is added dropwise
Fraction is 0.5% yellow rice wine, after decoction terminates, is filtered while hot, and obtained filtrate is 1.16 by being concentrated under reduced pressure into relative density；
（2）The ethanol of 11 times of volumes is added into the filtrate of above-mentioned gained, is soaked 22 minutes, refluxing extraction 1.5 is small at 65 DEG C
When, filtering adds 4 times of volumes into obtained filter residue, refluxing extraction 1.1 is small at the same temperature for the alcohol of same concentrations
When, filtering, the filtered fluid that 2 times are obtained merges, and removes alcohol by being concentrated under reduced pressure, obtains Salvia mitiorrhiza liquid standby；
（3）Using pH value of the mass fraction newly prepared for 35% sodium hydroxide solution regulation Salvia mitiorrhiza liquid, tentatively it is adjusted to
9.0, then heating is boiled, and maintains fluidized state 15 minutes, reuse the hydrochloric acid that molar concentration is 1.5mol/L adjust PH to
6.0, ethanol is added after cooling, alcohol content is reached 55%, after stirring, refrigerates 5 hours, is concentrated under reduced pressure except alcohol, used
Activated carbon decolorizing processing produces red sage root refined liquid.
It is used as further improvement of these options, step（1）Described filtrate relative density is determined at 70 DEG C.
It is used as further improvement of these options, step（2）The mass concentration of used ethanol is 85%.
It is used as further improvement of these options, step（3）In be concentrated under reduced pressure into relative density for 1.13.
Embodiment 3
The preparation method of Sodium Danshensu content in a kind of raising red sage roo drip liquid, the red sage roo drip liquid prepared by major ingredient and auxiliary material and
Into major ingredient is the red sage root, and shared mass percent is 80%, remaining as auxiliary material, is consisted of the following composition：Water for injection, glucose,
The processing and treating method of sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root comprises the following steps：
（1）The Danshen Tablets for selecting high-quality are cleaned up, ultramicro grinding to 80 mesh, add the clear water of 15 times of volumes, are decocted at 120 DEG C
Boil 2 hours, in decoction every stirring in 20 minutes once, every time a length of 5 minutes during stirring, while stirring, volume integral is added dropwise
Number is 0.6% yellow rice wine, after decoction terminates, is filtered while hot, and obtained filtrate is 1.17 by being concentrated under reduced pressure into relative density；
（2）The ethanol of 12 times of volumes is added into the filtrate of above-mentioned gained, is soaked 25 minutes, refluxing extraction 2 hours at 70 DEG C,
Filtering, alcohol refluxing extraction 1.2 hours, mistake at the same temperature of 5 times of volumes, same concentrations are added into obtained filter residue
Filter, the filtered fluid that 2 times are obtained merges, and removes alcohol by being concentrated under reduced pressure, obtains Salvia mitiorrhiza liquid standby；
（3）Using pH value of the mass fraction newly prepared for 40% sodium hydroxide solution regulation Salvia mitiorrhiza liquid, tentatively it is adjusted to
8.5-9.5, then heating is boiled, and maintains fluidized state 20 minutes, reuse the hydrochloric acid that molar concentration is 2mol/L adjust PH to
6.5, ethanol is added after cooling, alcohol content is reached 60%, after stirring, refrigerates 6 hours, is concentrated under reduced pressure except alcohol, used
Activated carbon decolorizing processing produces red sage root refined liquid.
It is used as further improvement of these options, step（1）Described filtrate relative density is determined at 70 DEG C.
It is used as further improvement of these options, step（2）The mass concentration of used ethanol is 90%.
It is used as further improvement of these options, step（3）In be concentrated under reduced pressure into relative density for 1.14.
Comparative example 1-3
Prepare red sage root refined liquid using existing red sage root method of purification, remaining composition and proportioning according to embodiment 1-3 method,
Correspond.
Contrast test
Red sage roo drip liquid is prepared using embodiment 1-3 and comparative example 1-3 processing method respectively, and with the red sage root on the market
Drip solution carries out the contrast of component content measure as a control group, randomly selects 5 parts for every group and is tested, the method for composition measurement
Using high performance liquid chromatography, the average value of each group measurement result is as shown in the table：
| Project | Sodium Danshensu（mg/g） | Protocatechualdehyde（mg/g） | Tanshin polyphenolic acid B（mg/g） | Total phenol（mg/g） |
| Embodiment 1 | 6.8 | 1.02 | 0.15 | 34.8 |
| Embodiment 2 | 7.2 | 1.05 | 0.16 | 35.3 |
| Embodiment 3 | 6.9 | 1.03 | 0.14 | 34.9 |
| Comparative example 1 | 3.8 | 0.65 | 0.07 | 27.6 |
| Comparative example 2 | 4.0 | 0.68 | 0.09 | 27.8 |
| Comparative example 3 | 3.8 | 0.64 | 0.08 | 27.5 |
| Control group | 3.4 | 0.42 | 0.06 | 23.9 |
By contrast test this it appears that：The preparation method of the present invention has brought up to the content of Sodium Danshensu compared with Gao Shui
It is flat, while other active ingredients are also improved.
Claims (4)
1. a kind of preparation method for improving Sodium Danshensu content in red sage roo drip liquid, it is characterised in that the red sage roo drip liquid is by leading
Material and auxiliary material are prepared from, and major ingredient is the red sage root, and shared mass percent is 70-80%, remaining as auxiliary material, is consisted of the following composition：
The processing and treating method of water for injection, glucose, sodium hydrogensulfite, hydrochloric acid, sodium hydroxide and nitrogen, the wherein red sage root includes following
Step：
（1）The Danshen Tablets for selecting high-quality are cleaned up, ultramicro grinding to 50-80 mesh, add the clear water of 10-15 times of volume,
Decocted 1-2 hours at 110-120 DEG C, it is in decoction every stirring in 10-20 minutes once, a length of 3-5 minutes during stirring every time, stirring
While mixing, the yellow rice wine that volume fraction is 0.4-0.6% is added dropwise, after decoction terminates, filters while hot, obtained filtrate is by decompression
Relative density is concentrated into for 1.16-1.17；
（2）The ethanol of 10-12 times of volume is added into the filtrate of above-mentioned gained, is soaked 20-25 minutes, is flowed back at 60-70 DEG C
Extract 1-2 hours, filtering adds 3-5 times of volume into obtained filter residue, the alcohol of same concentrations flows back at the same temperature
Extract 1-1.2 hours, filtering, the filtered fluid that 2 times are obtained merges, remove alcohol by being concentrated under reduced pressure, obtain Salvia mitiorrhiza liquid standby；
（3）The pH value of Salvia mitiorrhiza liquid, first step are adjusted for 30-40% sodium hydroxide solution using the mass fraction newly prepared
Save as 8.5-9.5, then heating is boiled, and maintains fluidized state 10-20 minute, reuse hydrochloric acid of the molar concentration for 1-2mol/L
PH to 5.5-6.5 is adjusted, ethanol is added after cooling, alcohol content is reached 50-60%, after stirring, refrigerates 4-6 hours, carries out
It is concentrated under reduced pressure except alcohol, is handled using activated carbon decolorizing and produce red sage root refined liquid.
2. a kind of preparation method for improving Sodium Danshensu content in red sage roo drip liquid as claimed in claim 1, it is characterised in that step
Suddenly（1）Described filtrate relative density is determined at 70 DEG C.
3. a kind of preparation method for improving Sodium Danshensu content in red sage roo drip liquid as claimed in claim 1, it is characterised in that step
Suddenly（2）The mass concentration of used ethanol is 80-90%.
4. a kind of preparation method for improving Sodium Danshensu content in red sage roo drip liquid as claimed in claim 1, it is characterised in that step
Suddenly（3）In be concentrated under reduced pressure into relative density for 1.12-1.14.
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| CN107789318A (en) * | 2017-10-31 | 2018-03-13 | 齐芳 | A kind of preparation method for improving danshen injections bioactivity |
| CN108785381A (en) * | 2018-09-17 | 2018-11-13 | 吉林四长制药有限公司 | A kind of preparation method of pharmaceutical composition for angiocardiopathy |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107789318A (en) * | 2017-10-31 | 2018-03-13 | 齐芳 | A kind of preparation method for improving danshen injections bioactivity |
| CN108785381A (en) * | 2018-09-17 | 2018-11-13 | 吉林四长制药有限公司 | A kind of preparation method of pharmaceutical composition for angiocardiopathy |
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Application publication date: 20171020 |