CN103432199A - Preparation method of pharmaceutical composition, and pharmaceutical composition prepared thereby - Google Patents
Preparation method of pharmaceutical composition, and pharmaceutical composition prepared thereby Download PDFInfo
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Abstract
The invention provides a preparation method of a pharmaceutical composition containing root of red-rooted salvia. The method comprises the following steps: with water or ethanol solution as an extracting solvent under control of pressure, heating, refluxing and extracting the root of red-rooted salvia; preferably, firstly heating, refluxing and extracting the root of red-rooted salvia by the ethanol solution under control of pressure, and then heating, refluxing and extracting dregs of the root of red-rooted salvia by water. The pharmaceutical composition provided by the invention also can contain pseudo-ginseng, borneol and the like. The preparation method comprises the following steps: independently or simultaneously putting the root of red-rooted salvia and the pseudo-ginseng into an extracting system under control of pressure; and with the water or ethanol solution as the extracting solvent, heating, refluxing and extracting. The invention also provides the pharmaceutical composition prepared by the preparation method. Compared with atmospheric reflux extraction, the preparation method disclosed by the invention has the advantages that the content of effective components of the root of red-rooted salvia can be significantly increased; the damage to the components of the root of red-rooted salvia caused by high temperature and long heating time is reduced; meanwhile, the extracting time and solvent consumption can be shortened and reduced.
Description
Technical field
The invention belongs to field of traditional Chinese, be specifically related to a kind of preparation method of the pharmaceutical composition that contains Radix Salviae Miltiorrhizae.
Background technology
Radix Salviae Miltiorrhizae is the most frequently used Chinese medicine of Cardiovarscular, in this most preparation in treatment field, all contains Radix Salviae Miltiorrhizae, even take Radix Salviae Miltiorrhizae as monarch drug.Therefore, the extraction efficiency of effective component in red sage, have significant impact to the curative effect of above-mentioned preparation.
The main pharmacodynamics composition of Radix Salviae Miltiorrhizae comprises: the water soluble ingredient that the salvianolic acid B (shown in structural formula as I) of take is representative, and with Tanshinone II
athe liposoluble constituent that (shown in structural formula as I I) and danshensu are representative.No matter be salvianolic acid B, or tanshinone ⅡA, all responsive to heat, to be heated for a long time, structure is easily by bad.
At present, Radix Salviae Miltiorrhizae single preparations of ephedrine and the compound preparation that comprises Radix Salviae Miltiorrhizae, extracting method is taked reflux under normal pressure more.For example 2010 editions " technique of the FUFANG DANSHEN PIAN of recording on Chinese pharmacopoeia is: Radix Salviae Miltiorrhizae adds alcohol heating reflux 1.5 hours, and extracting solution filters, and filtrate recycling ethanol also is concentrated into appropriate, standby; Medicinal residues add 50% alcohol heating reflux 1.5 hours, and extracting solution filters, and filtrate is concentrated in right amount, standby; Medicinal residues decoct with water 2 hours, and decocting liquid filters, and filtrate is concentrated in right amount.Radix Notoginseng powder is broken into fine powder, with above-mentioned concentrated solution and appropriate amount of auxiliary materials granulation, drying; The Borneolum Syntheticum porphyrize, mix with above-mentioned granule, and in flakes, sugar coating or film-coat, obtain in compacting.
The shortcoming of normal heating reflux technique is: the extraction process time is long, energy consumption is high; The effective ingredient rate of transform is low, and the extracted amount of impurity is large.In addition, under the Radix Salviae Miltiorrhizae normal pressure, alcohol extraction and water extraction temperature are all very high, all can reach 80～100 ℃.Tanshinone IIA and salvianolic acid B are heated for a long time, easily by high temperature, are destroyed.Therefore, the compound red sage root preparation that above-mentioned prior art makes, loss of effective components is serious, and drug effect can not guarantee, and energy consumption is high, efficiency is low, can not meet the requirement of green manufacturing, low-carbon environment-friendly.
Therefore, be necessary the Radix Salviae Miltiorrhizae extraction process that exploitation makes new advances, to improve the rate of transform and the production efficiency of effective ingredient, guarantee curative effect, reduce production costs simultaneously.
Summary of the invention
For the deficiency of existing extractive technique, the invention provides the preparation method of the pharmaceutical composition that a kind of raw material contains Radix Salviae Miltiorrhizae.The method comprises under pressure controlling extracts Radix Salviae Miltiorrhizae, realizes rapid extraction, has protected active ingredient, avoids its degraded loss, shortens extraction time again, energy savings.Preparation method of the present invention has overcome long, the shortcoming such as energy consumption is high, the effective ingredient rate of transform is low of the time that traditional atmospheric pressure reflux extracts.
For solving the problems of the technologies described above, the present invention has adopted following technical scheme:
A kind of preparation method of pharmaceutical composition, the raw material of described pharmaceutical composition comprises Radix Salviae Miltiorrhizae, described preparation method comprises the steps:
Under pressure controlling, take water or alcoholic solution as extracting solvent, heating and refluxing extraction Radix Salviae Miltiorrhizae.
Preferably: under pressure controlling, first use alcoholic solution heating and refluxing extraction Radix Salviae Miltiorrhizae, Radix Salviae Miltiorrhizae decoction dregs is the water heating and refluxing extraction again.
Described drug regimen raw material also comprises Radix Notoginseng; Described preparation method comprises the steps:
Under pressure controlling, Radix Salviae Miltiorrhizae and Radix Notoginseng are placed in an extraction system independently of one another or together, take water or alcoholic solution as extracting solvent, heating and refluxing extraction.
In preparation method of the present invention, preferred system pressure is 50-700mbar.
Preferred, when described extraction solvent is water, system pressure is 50～500mbar; Or, when described extraction solvent is alcoholic solution, system pressure is 125～700mbar.
In preparation method of the present invention, in described alcoholic solution, the percent by volume of ethanol is 40%～100%, and surplus is water;
Preferably, the percent by volume of ethanol is 40%-50%, and surplus is water; Or the percent by volume of ethanol is 75%-95%, surplus is water.
Preparation method of the present invention, the volume/weight ratio of described extraction solvent and medical material is preferably 4～20:1; 6～12:1 more preferably; Most preferably be 10～12:1.
Preparation method of the present invention, preferably extract 1-3 time, each 30～120min; More preferably extract extraction time 60～90min 1 time.
Preparation method of the present invention, Radix Salviae Miltiorrhizae or Radix Notoginseng are pulverized or do not pulverize.In order to adapt to suitability for industrialized production, Radix Salviae Miltiorrhizae or Radix Notoginseng can directly be extracted with decoction pieces.
As a preferred embodiment of the present invention, the invention provides a kind of preparation method of pharmaceutical composition, the raw material of described pharmaceutical composition comprises Radix Salviae Miltiorrhizae, specifically comprises the steps:
Salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, take water as extracting solvent, the volume/weight ratio 10～12:1 of water and Radix Salviae Miltiorrhizae, shift to an earlier date soaked overnight, adjusting pressure is 400～500mbar, and 75～85 ℃ of lower boiling refluxs extract 1～3 time, each 70～90min, filter, and filtrate is concentrated;
Or
Salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling refluxs extract 1～3 time, each 70～110min, filter, and filtrate recycling ethanol is also concentrated;
Or
I. salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling reflux 70～110min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, then take water as extracting solvent, extracting the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400～500mbar, and 75～85 ℃ of lower boiling reflux 70～90min filter, and filtrate is concentrated;
III. the concentrated solution that combining step I and Step II obtain;
Or
I. salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling reflux 70～110min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, the alcoholic solution of concentration expressed in percentage by volume 40～50% of take again be to extract solvent, extract the volume/weight ratio 8～10:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 450～550mbar, 65～75 ℃ of lower boiling reflux 50～70min, filter, filtrate recycling ethanol is also concentrated, standby;
III. the Radix Salviae Miltiorrhizae decoction dregs that Step II obtains, then take water as extracting solvent, extracting the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400～500mbar, and 75～85 ℃ of lower boiling reflux 70～90min filter, and filtrate is concentrated;
IV. the concentrated solution that combining step I to III obtains.
Preferably, also comprise the steps:
The concentrated solution that above-mentioned preparation method obtains or merging concentrated solution, add pharmaceutically acceptable adjuvant, is prepared into acceptable preparation clinically.
As another preferred embodiment of the present invention, the present invention also provides a kind of preparation method of pharmaceutical composition, and described pharmaceutical composition raw material comprises the medical material of following weight portion:
Radix Salviae Miltiorrhizae 1-50 part, Radix Notoginseng 1-15 part, Borneolum Syntheticum 0-8 part;
Described preparation method specifically comprises the steps:
I. the salvia piece of described weight portion or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling reflux 70～110min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, the alcoholic solution of concentration expressed in percentage by volume 40～50% of take again be to extract solvent, extract the volume/weight ratio 8～10:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 450～550mbar, 65～75 ℃ of lower boiling reflux 50～70min, filter, filtrate recycling ethanol is also concentrated, standby;
III. the Radix Salviae Miltiorrhizae decoction dregs that Step II obtains, then take water as extracting solvent, extracting the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400～500mbar, and 75～85 ℃ of lower boiling reflux 70～90min filter, and filtrate is concentrated;
IV. the concentrated solution that combining step I to III obtains;
V. the Radix Notoginseng powder of described weight portion is broken into fine powder, with step IV obtain merging concentrated solution and pharmaceutically the acceptable adjuvant mix, granule processed;
VI. the Borneolum Syntheticum porphyrize of described weight portion, the granule obtained with step V mixes, and is prepared into acceptable preparation clinically.
Or the above-mentioned preparation method that comprises the pharmaceutical composition of Radix Salviae Miltiorrhizae, Radix Notoginseng, Borneolum Syntheticum can also preferably include the scheme of following concrete steps:
I. the Radix Salviae Miltiorrhizae of described weight portion and notoginseng decoction piece or be ground into Radix Salviae Miltiorrhizae or the Radix Notoginseng of coarse powder, take water as extracting solvent, and the envelope-bulk to weight ratio that extracts solvent and medical material is 10～12:1, and adjusting pressure is 400～500mbar, 75～85 ℃ of lower boiling reflux 50～70min, filter, filtrate is concentrated, precipitate with ethanol, get supernatant, reclaim ethanol, be condensed into thick paste, standby;
II. the Borneolum Syntheticum porphyrize of described weight portion, the thick paste obtained with step I merges, and adds pharmaceutically acceptable adjuvant, is prepared into acceptable preparation clinically.
Pharmaceutical composition prepared by the preparation method that another object of the present invention is to provide above-mentioned.
Pharmaceutically acceptable adjuvant of the present invention, comprise excipient, such as lactose, sucrose, starch, D-mannital etc., binding agent, such as cellulose, sucrose, dextrin, hydroxypropyl cellulose, polyvinylpyrrolidone etc., disintegrating agent, such as starch, carboxymethyl cellulose etc., lubricant, such as magnesium stearate etc., surfactant, surfactant, such as tween 80, sodium lauryl sulfate etc., solvent, such as water, dehydrated alcohol, soybean oil, Polyethylene Glycol etc., antiseptic, such as p-Hydroxybenzoate etc., but be not limited to these.
The intake of pharmaceutical composition of the present invention or administered dose, according to the age of taking object, body weight etc. and different, as the medicine of blood circulation promoting and blood stasis dispelling, common adult (with the 60kg weighing machine) 100mg-5g every day, preferably once a day or minute absorb or take for several times 300mg-3g.
Radix Salviae Miltiorrhizae mainly contains water solublity and fat-soluble two effective constituents, wherein salvianolic acid B and Tanshinone II
abe respectively the representative composition of water solublity and fat-soluble effective ingredient, salvianolic acid B is the four poly-Caffeic acids compounds that two molecule danshensus and the condensation of a part prolithospermic acid form, and chemical property is very unstable, is subject to pyrolytic; Tanshinone II
ameet light, heat is all unstable.The present invention adopts the method for decompression extraction by salvianolic acid B and Tanshinone II
aextract under the state of low-temperature boiling, avoided the decomposition of effective ingredient.
The present invention first filters out the key process parameter that the Radix Salviae Miltiorrhizae decompression is extracted, and then each parameter is carried out preferably.Specifically by following process:
Extraction temperature of the present invention refers under certain system pressure, extracts the boiling point of solvent.Therefore, for certain extraction solvent, this extracts temperature by the unique decision of system pressure.For the ease of research, below to extract temperature, replace system pressure.After optimizing the extraction temperature, according to the relation of pressure and solvent boiling point, can know preferred system pressure.
1.Plackett-Burman key process parameter is extracted in the decompression of design screening Radix Salviae Miltiorrhizae
Take that effective component in red sage---salvianolic acid B and tanshinone ⅡA are evaluation index, in conjunction with Radix Salviae Miltiorrhizae, other detect index, comprise total solid yield, content of tannin, polyoses content, by the weight proportion analysis, determine and using salvianolic acid B, tanshinone ⅡA and total solid yield as comprehensive evaluation index; Use Plackett-Burman designs, and screens and clearly affect the key process parameter of the extraction effect that reduces pressure from numerous parameters such as medical material solvent ratios amount, medical material solvent loading, extraction time, extraction time, medical material granularity, extraction temperature, extraction pressure.
Experimental result shows: the appreciable impact factor of extracting the water soluble ingredient salvianolic acid B is: extraction time, extraction temperature and amount of water (liquid ratio); Extract the liposoluble constituent Tanshinone II
athe appreciable impact factor be: concentration of alcohol (extraction solvent), extraction time and extraction temperature.
2Box-Behnken design-effect surface method is optimized Radix Salviae Miltiorrhizae decompression extraction process and suitability study thereof
It is evaluation index that the water solublity heat-sensitive ingredients salvianolic acid B of take extracts content, adopts the Box-Behnken design to investigate the impact on Radix Salviae Miltiorrhizae decompression extraction process by water of extraction time, extraction temperature and amount of water (liquid ratio); With fat-soluble heat-sensitive ingredients Tanshinone II
aextraction content is evaluation index, adopt the Box-Behnken design to investigate the impact on Radix Salviae Miltiorrhizae decompression alcohol extraction process of concentration of alcohol (extraction solvent), extraction time and extraction temperature, result is carried out to multiple linear regression and binomial fitting, select optimum process condition by the effect surface method, and carry out analyses and prediction and experimental verification.Investigate medical material immersion, extraction time to salvianolic acid B and Tanshinone II by experiment of single factor
athe impact of extraction process.The optimum decompression of gained salvianolic acid B and tanshinone IIA extraction process and normal pressure extraction are carried out to experimental comparison.
2.1 take salvianolic acid B as index to the decompression extraction conditions preferred
Experimental design
Selected X1 (extraction time): 60～120min, X2 (extraction temperature): 50～80 ℃, X3 (liquid ratio): 6～12 times is the investigation object, and Y (content of salvianolic acid B) is evaluation index, optimizes Radix Salviae Miltiorrhizae decompression water extraction optimal extract process.Box-Behnken Design design factor and level are in Table 1, BBD experimental design and the results are shown in Table 2.
Table 1 Radix Salviae Miltiorrhizae decompression water extraction BBD design factor and level
BBD design and result are extracted in the decompression of table 2 Radix Salviae Miltiorrhizae
Regression analysis
The content model the results of analysis of variance of salvianolic acid B is in Table 3, and model is (P<0.05) significantly, and default matching is not significantly (P>0.05) all.The content model equation of salvianolic acid B shows factor X2, X3, X1
2and X3
2impact significantly.The content model equation r of salvianolic acid B
2=0.8793, show that this Regression Model Simulator is all right, the representativeness of regression equation is fine, can the Accurate Prediction practical situation.Regression equation is as follows:
Y=-15.197+0.459X
1+0.073X
2+3.113X
3-1.884×10
-3X
1X
2+0.025X
1X
3+0.031X
2X
3-3.310×10
-3X
1 2-2.955×10
-4X
2 2-0.353X
3 2。
Table 3 the results of analysis of variance
Effect surface is analyzed
According to Regression Analysis Result, fix certain variable in 3 influence factors, draw the diagram of block of two other variable about the content of salvianolic acid B, see Fig. 1-Fig. 3.
According to effect surface, illustrate, be optimized analysis in conjunction with Design Expert7.0 software, study the situation that affects of each factor pairing effect value, experimental result shows: the optimised process that the decompression of red sage root water soluble ingredient salvianolic acid B is extracted is: extraction time 89min, extract 80 ℃ of temperature, liquid ratio 11:1, extraction time 1 time and soaked overnight in advance, the extraction content experiment value of salvianolic acid B on average can reach 50.06mg/g, and between predictive value, deviation ratio is-1.70%, the mathematical model of foundation conforms to the laboratory observation data.
2.2 take tanshinone ⅡA as index to the decompression extraction conditions preferred
Experimental design
According to the preliminary experiment situation, 2 times of amounts of ethanol consumption (liquid ratio) stuck-at-１, selected X
1(concentration of alcohol): 50～90%, X
2(extraction time): 30～90min, X
3(extraction temperature): 40～70 ℃ for investigating object, Y (Tanshinone II
acontent) be evaluation index, use BBD to test preferred fat soluble ingredient of red sage root Tanshinone II
athe decompression extraction process.Box-Behnken Design(BBD) empirical factor and level in Table 4, BBD experiment table with the results are shown in Table 5.
BBD empirical factor and level are extracted in table 4 Radix Salviae Miltiorrhizae alcohol extraction decompression
BBD experiment table and result are extracted in the decompression of table 5 Radix Salviae Miltiorrhizae
Regression analysis
Result is carried out to multiple linear regression and binomial fitting, Tanshinone II
acontent model the results of analysis of variance in Table 6, model is (P<0.05) significantly, default matching is not significantly (P>0.05) all.Tanshinone II
athe content model equation show factor X
1, X
2, X
3, X
2x
3, X
1 2, X
2 2and X
3 2impact significantly.Tanshinone II
acontent model equation r
2=0.9976, show that this Regression Model Simulator situation is very good, the representativeness of regression equation is fine, can the Accurate Prediction practical situation.Regression equation:
Y=-5.766+0.107X
1+5.786×10
-3X
2+0.082X
3-2.298×10
-5X
1X
2-2.267×10
-5X
1X
3+1.197X
2X
3×10
-4-6.091×10
-4X
1 2-6.944×10
-5X
2 2-7.527×10
-4X
3 2。
Table 6 the results of analysis of variance
Effect surface is analyzed
According to Regression Analysis Result, fix certain variable in 3 influence factors, draw two other variable to Tanshinone II
athe diagram of block of content influence, be shown in Fig. 4-Fig. 6.
As can be seen from Figure 4, concentration of alcohol and extraction time are to Tanshinone II
acontent certain synergism, Tanshinone II are arranged
acontent all become positive correlation with concentration of alcohol and extraction time.As can be seen from Figure 5, concentration of alcohol and extraction temperature are to Tanshinone II
acontent certain reciprocal effect effect, Tanshinone II are arranged
acontent become positive correlation with concentration of alcohol, but with the increase of extracting temperature first increases and then decreases, reach maximum between 55～60 ℃.As can be seen from Figure 6, extraction time and extraction temperature are to Tanshinone II
acontent significant reciprocal effect effect, Tanshinone II are arranged
acontent with extraction time with the equal first increases and then decreases of increase of extracting temperature, at extraction time 75～80min, extract in 55～60 ℃ of scopes of temperature and reach maximum.
BBD predicts the outcome
Use Design expert7.0 software responses surface analysis, Radix Salviae Miltiorrhizae decompression extraction process is optimized optimal value and is: concentration of alcohol 85%(85.16 rounds), extraction time 78min(78.41, round), while extracting temperature 59 ℃ (58.94, round), its Tanshinone II
athe content prediction theoretical value be respectively 1.428mg/g.
The technological experiment cumulative evidence
With concentration of alcohol 85%, extraction time 78min, extracting 12 times of 59 ℃ of temperature and liquid ratios is the extraction process condition, carries out altogether 5 parallel laboratory tests, result is got its meansigma methods, calculation deviation rate ［ deviation ratio=(actual value-predictive value)/predictive value * 100% ］.Experimental result is in Table 7.Tanshinone II as can be known from the results
abetween extraction content experiment value and predictive value, deviation is less, shows that set up mathematical model has good predictability, selected process conditions favorable reproducibility, and the BBD effect surface is analyzed gained fat soluble ingredient of red sage root Tanshinone II
ait is with a high credibility that optimised process is extracted in decompression.
Table 7 Radix Salviae Miltiorrhizae decompression extraction process experiment cumulative evidence result
Based on above-mentioned experiment, optimized respectively under pressure controlling, take water or alcoholic solution as extracting the preferred processing condition of solvent extraction Radix Salviae Miltiorrhizae.
Under described pressure controlling, take water or alcoholic solution as extracting the method for solvent extraction Radix Salviae Miltiorrhizae, as required, can apply independently of one another, for example, under pressure controlling, a water extracts Radix Salviae Miltiorrhizae, or only with alcoholic solution, extracts Radix Salviae Miltiorrhizae.In order more fully to extract the effective ingredient in Radix Salviae Miltiorrhizae, above-mentioned two kinds of extracting method can be combined: first take ethanol as extracting the fat-soluble composition of solvent extraction Radix Salviae Miltiorrhizae, then take the water soluble ingredient of water in extracting the solvent extraction Radix Salviae Miltiorrhizae decoction dregs.Can also be perhaps to extract the solvent extraction Radix Salviae Miltiorrhizae with the alcoholic solution of variable concentrations, then take the water soluble ingredient of water in extracting the solvent extraction Radix Salviae Miltiorrhizae decoction dregs.Concrete, the preparation method of the preferred Radix Salviae Miltiorrhizae extract of the present invention can be:
Technical scheme 1:
Salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, take water as extracting solvent, the volume/weight ratio 10～12:1 of water and Radix Salviae Miltiorrhizae, soaked overnight in advance, adjusting pressure is 400～500mbar, 75～85 ℃ of lower boiling reflux extractions 1! 3 times, preferably 3 times, each 70～90min, filter, and filtrate is concentrated.
Technical scheme 2: salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling refluxs extract 1～3 time, each 70～110min, filter, and filtrate recycling ethanol is also concentrated.
Technical scheme 3, comprise the steps:
I. salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling reflux 70～110min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, then take water as extracting solvent, extracting the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400～500mbar, and 75～85 ℃ of lower boiling reflux 70～90min filter, and filtrate is concentrated;
III. the concentrated solution that combining step I and Step II obtain.
I. salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80～95% of take be to extract solvent, extract the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350～450mbar, 55～65 ℃ of lower boiling reflux 70～110min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, the alcoholic solution of concentration expressed in percentage by volume 40～50% of take again be to extract solvent, extract the volume/weight ratio 8～10:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 450～550mbar, 65～75 ℃ of lower boiling reflux 50～70min, filter, filtrate recycling ethanol is also concentrated, standby;
III. the Radix Salviae Miltiorrhizae decoction dregs that Step II obtains, then take water as extracting solvent, extracting the volume/weight ratio 10～12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400～500mbar, and 75～85 ℃ of lower boiling reflux 70～90min filter, and filtrate is concentrated;
IV. the concentrated solution that combining step I to III obtains, obtain.
With version in 2010, " extracting method of the Radix Salviae Miltiorrhizae of putting down in writing in Chinese pharmacopoeia (atmospheric pressure reflux extraction method) relatively, the red rooted salvia of same amount, in technique scheme 4 gained Danshens of the present invention, the gained content of danshinolic acid B has improved 28.79% than normal pressure extraction process, and yield of extract has reduced by 9.01%; In the tanshinol extract, tanshinone IIA content has improved 15.38%, and yield of extract has reduced by 37.86% than normal pressure technique.The atmospheric pressure reflux extraction method technique that pressure controlling of the present invention extracts Radix Salviae Miltiorrhizae and prior art compares, in Table 8-table 9.
Table 8 pressure controlling extracts with atmospheric pressure reflux and extracts the impact of salvianolic acid B extraction content is compared
Table 9 pressure controlling extracts with atmospheric pressure reflux and extracts Tanshinone II
aextract the impact of content relatively
Conclusion: it is that science is feasible that the decompression extraction process of the liposoluble constituent that the Determination of water-soluble active constituents of radix that salvianolic acid B is representative and the tanshinone IIA of take be representative is take in the optimization of Box-Behnken effect surface method, and the method degree of accuracy is high, favorable reproducibility, predictability are strong.Than normal pressure, extract, in extract, salvianolic acid B and tanshinone IIA content all improve, and total extractum all reduces, and illustrates at effective ingredient and proposes in more situation, and impurity may propose still less.In addition, under decompression state, extraction time extracts short than atmospheric pressure reflux, illustrate that the inventive method is not only efficient, and energy-conservation.
The pharmaceutical composition that comprises Radix Salviae Miltiorrhizae, the pharmaceutical composition that the Radix Salviae Miltiorrhizae of particularly take is principal agent, as the compound red sage root preparation of crude drug by Radix Salviae Miltiorrhizae, Radix Notoginseng, Borneolum Syntheticum, can separately extract and prepare Radix Salviae Miltiorrhizae extract Radix Salviae Miltiorrhizae according to technical scheme of the present invention, or be extracted according to technical scheme of the present invention together with the crude drug of Radix Salviae Miltiorrhizae and other applicable solvent extraction.
In a word, advantage of the present invention is as follows:
1. adopt extracting method involved in the present invention, can significantly improve salvianolic acid B and Tanshinone II in Radix Salviae Miltiorrhizae
aextraction ratio.
2. adopt technique involved in the present invention, can effectively shorten production cycle and energy savings.
3. adopt technique involved in the present invention, can reduce the extraction of impurity component, make the manufactured goods dose reduce to original 1/2-1/3.
The accompanying drawing explanation
Below in conjunction with accompanying drawing, the present invention will be further described.
1. what Fig. 1 showed is that fixedly liquid ratio (X3) is 11 o'clock, extraction time (X1) and extraction temperature (X2) diagram of block on content of danshinolic acid B (Y) impact.
2. Fig. 2 shows is when extracting temperature (X2) and being 80 ℃, the diagram of block that extraction time (X1) and liquid ratio (X3) affect content of danshinolic acid B (Y).
3. what Fig. 3 showed is, while the fixed extraction time (X1) being 89min, to extract temperature (X2) and liquid ratio (X3) diagram of block on content of danshinolic acid B (Y) impact.
4. Fig. 4 shows is fixed extraction temperature (X3) while being 55 ℃, the diagram of block that concentration of alcohol (X1) and extraction time (X2) affect tanshinone IIA content (Y).
5. what Fig. 5 showed is while the fixed extraction time (X2) being 60min, concentration of alcohol (X1) and extraction temperature (X3) diagram of block on tanshinone IIA content (Y) impact.
6. what Fig. 6 showed is when fixedly concentration of alcohol (X1) is 70%, extraction time (X2) and extraction temperature (X3) diagram of block on tanshinone IIA content (Y) impact.
The specific embodiment
In order to understand better the present invention, below in conjunction with embodiment, the present invention is described in further details, but the scope of protection of present invention is not limited to this.
1 one kinds of pharmaceutical compositions of embodiment
Prescription: Radix Salviae Miltiorrhizae 450g
Preparation by the following method:
I. getting Radix Salviae Miltiorrhizae 450g and be placed in extraction vessel, add 5.4L95% ethanol (concentration expressed in percentage by volume), is 350mbar by digital display vacuum pump evacuation controlled pressure, and 65 ℃ of lower boiling refluxs extract 70min, filters, and filtrate recycling ethanol also is concentrated into appropriate, standby.
II. Radix Salviae Miltiorrhizae decoction dregs adds 3.6L50% ethanol (concentration expressed in percentage by volume), regulates pressure 550mbar, and 65 ℃ of lower boiling reflux 50min filter, and filtrate recycling ethanol also is concentrated into appropriate, standby.
III. Radix Salviae Miltiorrhizae decoction dregs adds 4.95L water, regulates pressure 500mbar, and 75 ℃ of lower boiling reflux 90min filter, and filtrate is concentrated in right amount.
IV. the concentrated solution that combining step I-III obtains, be concentrated into dryly, obtains.
In the present embodiment, described pharmaceutical composition yield is: 43%, and salvianolic acid content is 5.02%, Tanshinone II
acontent is 0.15%.
2 one kinds of medicament composition capsule agent of embodiment
Prescription (1000 capsules): Radix Salviae Miltiorrhizae 500g, starch 90g
Preparation by the following method:
I. getting Radix Salviae Miltiorrhizae 500g and be placed in extraction vessel, add 5.5L85% ethanol (concentration expressed in percentage by volume), is 450mbar by digital display vacuum pump evacuation controlled pressure, and 55 ℃ of lower boiling refluxs extract 100min, filters, and filtrate recycling ethanol also is concentrated into appropriate, standby.
II. Radix Salviae Miltiorrhizae decoction dregs adds 5L40% ethanol (concentration expressed in percentage by volume), regulates pressure 450mbar, and 75 ℃ of lower boiling reflux 70min filter, and filtrate recycling ethanol also is concentrated into appropriate, standby.
III. Radix Salviae Miltiorrhizae decoction dregs adds 5L water, regulates pressure 400mbar, and 85 ℃ of lower boiling reflux 70min filter, and filtrate is concentrated in right amount.
IV. the concentrated solution that combining step I-III obtains, add 90g starch, granule processed, encapsulated 1000.
In the present embodiment, described medicament composition capsule agent, every (0.30g) is containing salvianolic acid B 22.82mg, containing Tanshinone II
a0.69mg.The Radix Salviae Miltiorrhizae extractum total recovery is: 42.05%.
3 one kinds of medicinal composition tablets of embodiment
Prescription: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g, starch 80g, magnesium stearate 1g.
Preparation by the following method:
I. getting Radix Salviae Miltiorrhizae 450g and be placed in extraction vessel, add 4.5L95% ethanol (concentration expressed in percentage by volume), is 390mbar by digital display vacuum pump evacuation controlled pressure, and 60 ℃ of lower boiling refluxs extract 90min, filters, and filtrate recycling ethanol also is concentrated into appropriate, standby.
II. Radix Salviae Miltiorrhizae decoction dregs adds 3.6L50% ethanol (concentration expressed in percentage by volume), regulates pressure 520mbar, and 70 ℃ of lower boiling reflux 60min filter, and filtrate recycling ethanol also is concentrated into appropriate, standby.
III. Radix Salviae Miltiorrhizae decoction dregs adds 4.5L water, regulates pressure 465mbar, and 80 ℃ of lower boiling reflux 80min filter, and filtrate is concentrated in right amount.
IV. get Radix Notoginseng 141g, be ground into fine powder, the concentrated solution obtained with step I-III and starch 80g, magnesium stearate 1g granulation, drying.
V. Borneolum Syntheticum 8g porphyrize, the granule obtained with step IV mixes, and is pressed into 1000, and sugar coating or film-coat, obtain.
In the present embodiment, described medicinal composition tablets, every (0.32g) is containing salvianolic acid B 22.5mg, containing Tanshinone II
a0.63mg.The Radix Salviae Miltiorrhizae extractum total recovery is: 42.37%.
4 one kinds of medicament composition dropping pills agent of embodiment
Raw medicinal material prescription: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g
Preparation by the following method:
I. get Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, be placed in extraction vessel, add 5.9L water, adjusting pressure is 465mbar, and 80 ℃ of lower boiling refluxs extract 60min, and decocting liquid filters, filtrate is concentrated, add 95% ethanol, making the ethanol concentration expressed in percentage by volume is 70%, the standing precipitation that makes, get supernatant, reclaim ethanol, be condensed into thick paste, standby.
II. Borneolum Syntheticum 8g porphyrize.Taking polyethylene glycol is appropriate, and heating makes melting, and the thick paste that adds step I to obtain and Borneolum Syntheticum fine powder, mix, and splashes in cooling liquid paraffin, makes drop pill, or makes film coating after drop pill, obtains.
In the present embodiment, described medicament composition dropping pills, every ball (25mg) is containing salvianolic acid B 1.84mg, containing Tanshinone II
a0.26mg, containing danshensu 0.17mg, Radix Salviae Miltiorrhizae and Radix Notoginseng extractum total recovery are: 37.82%.
5 one kinds of medicament composition granule agent of embodiment
Raw medicinal material prescription: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g
Preparation by the following method:
I. getting Radix Salviae Miltiorrhizae 450g, add 4.5L95% ethanol, is 390mbar by digital display vacuum pump evacuation controlled pressure, and 60 ℃ of lower boiling reflux 90min filter, and filtrate recycling ethanol also is concentrated into appropriate, standby.
II. Radix Salviae Miltiorrhizae decoction dregs adds 3.6L50% ethanol, regulates pressure 520mbar, and 70 ℃ of lower boiling reflux 60min filter, and filtrate recycling ethanol also is concentrated into appropriate, standby.
III. Radix Salviae Miltiorrhizae decoction dregs adds 4.5L water, regulates pressure 465mbar, 80 ℃ of lower boiling reflux 80min, and decocting liquid filters, and filtrate is concentrated in right amount.
IV. the concentrated solution that combining step I-III obtains, spray drying, make dried cream powder.
V. get Radix Notoginseng 141g, be ground into fine powder, the dried cream powder that adds step IV to obtain and appropriate dextrin, mix granulation, drying.
VI. Borneolum Syntheticum 8g porphyrize, use anhydrous alcohol solution, is sprayed on equably on granule, and film coating, make 330g, packing, and every bag of 1g, obtain.
In the present embodiment, described medicament composition granule agent, every bag (1g) is containing salvianolic acid B 45.5mg, containing Tanshinone II
a3.7mg.The Radix Salviae Miltiorrhizae extractum yield is: 40.5%.
6 one kinds of drug combination injections of example
Prescription: Radix Salviae Miltiorrhizae 1500g
Preparation by the following method:
Get Radix Salviae Miltiorrhizae 1500g, add water 1.5L, regulator control system pressure is 0.055MPa, and decompression is extracted three times, 1 hour for the first time, and second and third time each 0.5 hour, collecting decoction, filter, and filtrate decompression is concentrated into 750ml.Add ethanol precipitation secondary, making for the first time containing the alcohol amount is 75%, and making for the second time containing the alcohol amount is 85%, each all cold preservation filters after placing, filtrate recycling ethanol, and be concentrated into about 250ml, inject water to 400ml, mix, cold preservation is placed, filter, with 10% sodium hydroxide solution, regulate pH value to 6.8, boil half an hour, filter, inject water to 1000ml, embedding, sterilizing, obtain.
In the present embodiment, described drug combination injection, every bottle (2ml) is containing salvianolic acid B 75mg.
7 one kinds of medicinal composition tablets of embodiment
Raw medicinal material prescription: Radix Salviae Miltiorrhizae 450g, Radix Notoginseng 141g, Borneolum Syntheticum 8g
Preparation by the following method:
Be ground into Radix Salviae Miltiorrhizae or the Radix Notoginseng of coarse powder, take water as extracting solvent, the envelope-bulk to weight ratio that extracts solvent and medical material is 10:1, and adjusting pressure is 450mbar, 75 ℃ of lower boiling reflux 70min, filter, and filtrate is concentrated, precipitate with ethanol, get supernatant, reclaim ethanol, be condensed into thick paste, standby;
II. Borneolum Syntheticum porphyrize, the thick paste obtained with step I merges, and adds appropriate amount of starch and magnesium stearate, granule processed, tabletting, obtain.
In the present embodiment, described medicinal composition tablets, every (0.3g) is containing salvianolic acid B 20mg, containing Tanshinone II
a0.5mg.
8 one kinds of DANSHEN KELI of embodiment
Prescription: Radix Salviae Miltiorrhizae 500g
Preparation by the following method:
Get Radix Salviae Miltiorrhizae 500g, add 95% ethanol 1.5L, regulator control system pressure is 390mbar, decompression is extracted three times, 1 hour for the first time, second and third time each 0.5 hour, collecting decoction, filter, it is 1.15-1.27 that filtrate decompression is concentrated into density, adds a certain amount of pregelatinized Starch and magnesium stearate, granule processed, granulate, obtain.
In the present embodiment, described medicament composition granule agent, every bag (1g) is containing the about 0.52mg of tanshinone ⅡA.
Claims (10)
1. the preparation method of a pharmaceutical composition, is characterized in that, described pharmaceutical composition raw material comprises Radix Salviae Miltiorrhizae, and described preparation method comprises the steps:
Under pressure controlling, take water or alcoholic solution as extracting solvent heating and refluxing extraction Radix Salviae Miltiorrhizae.
2. preparation method according to claim 1, is characterized in that, described preparation method comprises the steps:
Under pressure controlling, first use alcoholic solution heating and refluxing extraction Radix Salviae Miltiorrhizae, Radix Salviae Miltiorrhizae decoction dregs is the water heating and refluxing extraction again.
3. preparation method according to claim 1, is characterized in that, described drug regimen raw material also comprises Radix Notoginseng; Described preparation method comprises the steps:
Under pressure controlling, Radix Salviae Miltiorrhizae and Radix Notoginseng are placed in an extraction system independently of one another or together, take water or alcoholic solution as extracting solvent, heating and refluxing extraction.
4. according to the described preparation method of any one in claims 1 to 3, it is characterized in that, system pressure is 50-700 mbar;
Preferably, described extraction solvent is water, and system pressure is 50 ~ 500mbar; Or described extraction solvent is aquiferous ethanol, system pressure is 125 ~ 700mbar.
5. according to the described preparation method of any one in claim 1 to 4, it is characterized in that, in described alcoholic solution, the percent by volume of ethanol is 40% ~ 100%, and surplus is water;
Preferably, the percent by volume of ethanol is 40%-50%, and surplus is water; And/or the percent by volume of ethanol is 75%-95%, surplus is water.
6. according to the described preparation method of any one in claim 1 to 5, it is characterized in that, the volume/weight ratio of described extraction solvent and medical material is 4-20:1;
Preferably, the volume/weight ratio of described extraction solvent and medical material is 6-15:1;
Preferred, the volume/weight ratio of described extraction solvent and medical material is 10-12:1.
7. according to the described preparation method of any one in claim 1 to 6, it is characterized in that, extract 1-3 time, each 30 ~ 120min;
Preferably, extract extraction time 60 ~ 90min 1 time.
8. the preparation method of a pharmaceutical composition, is characterized in that, described pharmaceutical composition raw material comprises Radix Salviae Miltiorrhizae, and described preparation method specifically comprises the steps:
Salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, take water as extracting solvent, the volume/weight ratio 10 ~ 12:1 of water and Radix Salviae Miltiorrhizae, shift to an earlier date soaked overnight, adjusting pressure is 400 ~ 500mbar, and 75 ~ 85 ℃ of lower boiling refluxs extract 1 ~ 3 time, each 70 ~ 90min, filter, and filtrate is concentrated;
Or
Salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80 ~ 95% of take be to extract solvent, extract the volume/weight ratio 10 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350 ~ 450mbar, 55 ~ 65 ℃ of lower boiling refluxs extract 1 ~ 3 time, each 70 ~ 110 min, filter, and filtrate recycling ethanol is also concentrated;
Or
I. salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80 ~ 95% of take be to extract solvent, extract the volume/weight ratio 10 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350 ~ 450mbar, 55 ~ 65 ℃ of lower boiling reflux 70 ~ 110 min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, then take water as extracting solvent, extracting the volume/weight ratio 10 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400 ~ 500mbar, and 75 ~ 85 ℃ of lower boiling refluxs extract 70 ~ 90min, filter, and filtrate is concentrated;
III. the concentrated solution that combining step I and Step II obtain;
Or
I. salvia piece or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80 ~ 95% of take be to extract solvent, extract the volume/weight ratio 10 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350 ~ 450mbar, 55 ~ 65 ℃ of lower boiling reflux 70 ~ 110 min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, then take the alcoholic solution of concentration expressed in percentage by volume 40 ~ 50% and be to extract solvent, the volume/weight ratio 8 ~ 10:1 of solvent and Radix Salviae Miltiorrhizae extracted, adjusting pressure is 450 ~ 550mbar, and 65 ~ 75 ℃ of lower boiling reflux 50 ~ 70min filter, filtrate recycling ethanol is also concentrated, standby;
III. the Radix Salviae Miltiorrhizae decoction dregs that Step II obtains, then take water as extracting solvent, extracting the volume/weight ratio 10 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400 ~ 500mbar, and 75 ~ 85 ℃ of lower boiling reflux 70 ~ 90min filter, and filtrate is concentrated;
IV. the concentrated solution that combining step I to III obtains.
9. the preparation method of a pharmaceutical composition, is characterized in that, described pharmaceutical composition raw material comprises the medical material of following weight portion:
Radix Salviae Miltiorrhizae 1-50 part, Radix Notoginseng 1-15 part, Borneolum Syntheticum 0-8 part;
Described preparation method specifically comprises the steps:
I. the salvia piece of described weight portion or be ground into the Radix Salviae Miltiorrhizae of coarse powder, the alcoholic solution of concentration expressed in percentage by volume 80 ~ 95% of take be to extract solvent, extract the volume/weight ratio 10 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 350 ~ 450mbar, 55 ~ 65 ℃ of lower boiling reflux 70 ~ 110 min, filter, filtrate recycling ethanol is also concentrated, standby;
II. the Radix Salviae Miltiorrhizae decoction dregs that step I obtains, then take concentration expressed in percentage by volume 40 ~ 50% ethanol as extracting solvent, extract the volume/weight ratio 8 ~ 10:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 450 ~ 550mbar, and 65 ~ 75 ℃ of lower boiling reflux 50 ~ 70min filter, filtrate recycling ethanol is also concentrated, standby;
III. the Radix Salviae Miltiorrhizae decoction dregs that Step II obtains, then take water as extracting solvent, extracting the volume/weight ratio 6 ~ 12:1 of solvent and Radix Salviae Miltiorrhizae, adjusting pressure is 400 ~ 500mbar, and 75 ~ 85 ℃ of lower boiling reflux 70 ~ 90min filter, and filtrate is concentrated;
IV. the concentrated solution that combining step I to III obtains;
V. the Radix Notoginseng powder of described weight portion is broken into fine powder, with step IV obtain merging concentrated solution and pharmaceutically the acceptable adjuvant mix, granule processed;
VI. the Borneolum Syntheticum porphyrize of described weight portion, the granule obtained with step V mixes, and is prepared into acceptable preparation clinically;
Or
I. the Radix Salviae Miltiorrhizae of described weight portion and notoginseng decoction piece or be ground into Radix Salviae Miltiorrhizae and the Radix Notoginseng of coarse powder, take water as extracting solvent, and the envelope-bulk to weight ratio that extracts solvent and medical material is 10 ~ 12:1, and adjusting pressure is 400 ~ 500mbar, 75 ~ 85 ℃ of lower boiling reflux 50 ~ 70min, filter, filtrate is concentrated, precipitate with ethanol, get supernatant, reclaim ethanol, be condensed into thick paste, standby;
II. the Borneolum Syntheticum porphyrize of described weight portion, the thick paste obtained with step I merges, and adds pharmaceutically acceptable adjuvant, is prepared into acceptable preparation clinically.
10. the pharmaceutical composition that in claim 1 to 9 prepared by the described preparation method of any one.
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| CN110448594A (en) * | 2019-08-16 | 2019-11-15 | 金鸿药业股份有限公司 | A kind of preparation process and compound red sage root preparation of compound red sage root preparation |
| CN113662892A (en) * | 2021-08-12 | 2021-11-19 | 楚香(上海)生物科技有限公司 | Anti-aging regulatory protein plant extraction activator and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104974033A (en) * | 2013-12-22 | 2015-10-14 | 贵州景峰注射剂有限公司 | Method for extracting tanshinol |
| CN105267355A (en) * | 2015-11-13 | 2016-01-27 | 颈复康药业集团有限公司 | Extraction method of pharmaceutic preparation and building method of its prediction model |
| CN105267355B (en) * | 2015-11-13 | 2019-06-25 | 颈复康药业集团有限公司 | A kind of extracting method of pharmaceutical preparation and its method for building up of prediction model |
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| CN110448594B (en) * | 2019-08-16 | 2021-07-23 | 金鸿药业股份有限公司 | Preparation process of compound salvia miltiorrhiza preparation and compound salvia miltiorrhiza preparation |
| CN113662892A (en) * | 2021-08-12 | 2021-11-19 | 楚香(上海)生物科技有限公司 | Anti-aging regulatory protein plant extraction activator and preparation method thereof |
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Application publication date: 20131211 |