CN1554335A - Freeze-dried Danhong powder injection for injection and its preparing method - Google Patents

Freeze-dried Danhong powder injection for injection and its preparing method Download PDF

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CN1554335A
CN1554335A CNA200310125148XA CN200310125148A CN1554335A CN 1554335 A CN1554335 A CN 1554335A CN A200310125148X A CNA200310125148X A CN A200310125148XA CN 200310125148 A CN200310125148 A CN 200310125148A CN 1554335 A CN1554335 A CN 1554335A
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water
radix salviae
salviae miltiorrhizae
injection
solution
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CN1220489C (en
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张晴龙
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QIANLUCHUN SCIENCE AND TECHNOLOGY Co Ltd BEIJING
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QIANLUCHUN SCIENCE AND TECHNOLOGY Co Ltd BEIJING
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Abstract

The present invention features that based on the property of total salvianolic acid, which is a kind of weak acid, may be reacted with alkali to form salt with high stability and has high dissolvability in water; red sage is first extracted with alkali solution and then extracted with resin column, and safflower is ethanol refluxed to maintain its chalcone dimmer and other effective component and then acid solution extracted; and the safflower extract liquid and the red sage extract liquid are finally resin column extracted to raise the content of salvianolic acid, flavone and other effective components. The present invention provides a kind of red freeze dried sage-safflower powder for injection for clinical application in treating coronary heart disease, angina pectoris, cerebral vascular diseases and other diseases.

Description

A kind of Danhong freez-fried powder injecta and preparation method thereof
Affiliated field
The invention belongs to field of traditional Chinese medicine pharmacy, be specifically related to a kind of DANHONG freeze-dried powder injection that contains Radix Salviae Miltiorrhizae, safflower effective part and preparation method thereof.
Background technology
Radix Salviae Miltiorrhizae is the dry root and rhizome of lip type section plant Radix Salviae Miltiorrhizae, according to existing document: Radix Salviae Miltiorrhizae head is stated from Shennong's Herbal, more the successive dynasties book on Chinese herbal medicine has and records, the function that Pharmacopoeia of People's Republic of China (version was an one in 2000) is then concluded Radix Salviae Miltiorrhizae with cure mainly into: " stasis-dispelling and pain-killing; promoting blood circulation to restore menstrual flow, relieving restlessness clears away heart-fire.Be used for menoxenia, the amenorrhea dysmenorrhea, abdominal mass is gathered, breast ventral spine pain, skin infection swells and ache, dysphoria and insomnia; Hepatosplenomegaly, angina pectoris ".Illustrate that Radix Salviae Miltiorrhizae shows many-sided effect in clinical practice.The chemical constituent of Radix Salviae Miltiorrhizae mainly can be divided into water soluble ingredient and liposoluble constituent two large divisions.As everyone knows, traditional application mode of Radix Salviae Miltiorrhizae is a decocting liquid, and therefore, its effective ingredient should be based on water-soluble substances.China pharmaceuticals researcher studies the water soluble ingredient of Radix Salviae Miltiorrhizae, proves that the salvia-soluble effective ingredient mainly is a phenolic acid compound.At present, the extracting method of salvianolic acid compounds mostly is water and carries the back resin column (Chinese invention patent CN1247855A, CN1270809A, CN1384090A, CN1459448A) of crossing, but no matter be that water is carried or hot water is carried the back resin column of crossing, all Radix Salviae Miltiorrhizae total phenolic acids can not be extracted effectively.
Flos Carthami is the traditional drug for invigorating blood circulation and eliminating stasis of the traditional Chinese medical science, is a kind of gynecological good medicine, is again the raw material of natural pigment.Since ancient times, the Flos Carthami quality with red be excellent, Huang takes second place." book on Chinese herbal medicine is looked for the truth " record: " the arduous and temperature of Flos Carthami, color is red goes into blood, invigorates blood circulation for the logical stasis of blood and wants agent." think that effective ingredient is red composition.As the processing to Flos Carthami, Li Shizhen (1518-1593 A.D.) had such argumentation: " picking flowers early morning, it is ripe to smash, and washes in a pan with water, and the cloth bag strand goes yellow juice to smash again, washes in a pan clearly again with sour Semen setariae water from washing rice, and the strand bag removes juice again, covers one night with Herba Artemisiae Annuae, and dry, or pinch into pancake, the receipts of drying in the shade.Be used as medicine and rub broken usefulness with the hands." make medicinal Flos Carthami cake, the contained medicinal ingredient of plate Flos Carthami for remove the water insoluble ingredients behind the water solublity flavochrome with sour water.Document shows that Flos Carthami mainly contains red pigment and flavochrome.Red pigment is a dimeric chalcon, and flavochrome is the mixture of multiple water soluble ingredient, belongs to the chalcone chemical compound.Dimeric chalcon be the antihypertensive activity main component (Meng Ge etc. the special journal .1999 of Kaifeng doctor, 18 (3): 46).At present, the extracting method of safflower effective part mostly is water extraction, has discarded its water insoluble ingredients, not high to the utilization rate of medical material.
DANHONG ZHUSHEYE system is by drug matchings such as Radix Salviae Miltiorrhizae, Flos Carthamis, through processing the compound injection that extracts and make.Multiple diseases such as coronary heart disease, angina pectoris, cerebrovascular had curative effect preferably.Existing ministry standard adopts after the rare alcohol extraction of Radix Salviae Miltiorrhizae, be total to the method that water is put forward with Flos Carthami again, purification effect is bad, its content of effective is not high, to medical material is a kind of great waste, and the injection water preparation exists transportation inconvenience, problems such as quality stability difference, need make improvements, provide better medicine for clinical.
Summary of the invention
The objective of the invention is to overcome deficiency of the prior art, is acidulous material according to Radix Salviae Miltiorrhizae total phenolic acids, is soluble in the alkali salify, dissolubility in the water increases, and the character that compound stability improves behind the salify is behind Radix Salviae Miltiorrhizae employing potass extraction, after the extracting method of resin column; To the dimeric chalcon effective kind part in the Flos Carthami employing alcohol reflux reservation Flos Carthami, the reuse sour water is carried, last and Radix Salviae Miltiorrhizae is crossed the extraction process of resin column, improved the content of phenolic acid and flavonoid effective site in the preparation, for clinical practice provides a kind of productive rate height, cost is low, quality good, the more rational freeze-drying powder injection containing red-rooted salvia safflower of preparation technology.
The present invention is achieved through the following technical solutions:
(1) Radix Salviae Miltiorrhizae is pulverized, and is that aqueous alkali more than 10 is carried 2~3 times with pH, and temperature is 80~100 ℃, and each 60~120min, merge extractive liquid, are extracting solution A;
(2) Flos Carthami is with 40~80% alcohol reflux 2~3 times, and each 60~120min reclaims ethanol to there not being the alcohol flavor, extracting solution B;
(3) will add 5~50 times of water gagings with the Flos Carthami medicinal residues behind the ethanol extraction, be that 3~5 sour water is carried 2~3 times with pH, and temperature is 20~80 ℃, each 30~120min, merge extractive liquid,, extracting solution C;
(4) merge extractive liquid, A and C, centrifugal, get supernatant, concentrating under reduced pressure, transfer pH 6.5~7, last macroporous resin column earlier is washed till no Molish reaction with deionized water, continues to be washed till eluent with 20~90% ethanol and adds 1% ferric chloride reagent and do not have tangible phenolic hydroxyl group reaction, eluent and concentrated ammonia solution and only do not develop the color.Reclaim alcohol eluen, concentrate extracting solution D;
(5) merge extractive liquid, B and D replenish water for injection to ormal weight, stir evenly, cold preservation, filtration, add freeze-dried excipient, transfer pH 6.5~7, filtrate adds proper amount of active carbon and boils 15min, puts coldly, is filtered to clear and bright, get solution, sterilization back packing, lyophilization, gland is promptly.
The macroporous adsorbent resin that is used for purification effective site can be nonpolar, low pole or polar macroporous adsorption resin, and preferred low pole macroporous adsorbent resin comprises AB-8 and D 101Resin.
Freeze-dried excipient can be an acceptable freeze-dried excipient commonly used arbitrarily on the galenic pharmacy.Preferred freeze-dried excipient is one or both the compound excipient in mannitol, lactose, sucrose or the glucose.
A kind of freeze-drying powder injection containing red-rooted salvia safflower preparation technology of the present invention, according to Radix Salviae Miltiorrhizae total phenolic acids is acidulous material, be soluble in the alkali salify, dissolubility in the water increases, and the character that compound stability improves behind the salify, behind Radix Salviae Miltiorrhizae employing potass extraction, purifying process after macroporous resin, greatly improved extraction ratio (the potass extraction Radix Salviae Miltiorrhizae of Radix Salviae Miltiorrhizae total phenolic acids, the content of its salvianolic acid B is 10 times that water is carried), be better than Chinese invention patent CN1247855A, CN1270809A, CN1384090A, CN1459448A carry back last resin column to Radix Salviae Miltiorrhizae water technology; After Flos Carthami adopted alcohol reflux, sour water was carried, and crosses the extraction process of resin column again with Radix Salviae Miltiorrhizae, has kept the dimeric chalcon effective kind part in the Flos Carthami, and acid extraction guaranteed the stability of Carthamus yellow, was better than the water extraction process of traditional method; Preparation technology of the present invention adopts macroporous adsorption resin technology, improved the content of phenolic acid and flavonoid effective site in the preparation, is better than the DANHONG ZHUSHEYE preparation technology of ministry standard WS-11220 (ZD-1220)-2002.A kind of Danhong freeze dried powder injection agent that application the inventive method makes is loose porous, solubility good, and water content is low, meets national standard, its production process sterile working, cold drying, active component is not destroyed, and vacuum or noble gas are filled, be difficult for taking place oxidation, period of storage is long, and stability is improved, thereby has prolonged the effect duration of this medicine, be convenient to store, transport and sell, also be convenient to guarantee product quality.Experiment shows that freeze-drying powder injection containing red-rooted salvia safflower is better than existing DANHONG ZHUSHEJI to acute blood stasis rat model whole blood viscosity improvement effect.
Below by experiment a kind of freeze-drying powder injection containing red-rooted salvia safflower of the present invention is further described.
Experiment one: the comparative experiments of water extraction and potass extraction Radix Salviae Miltiorrhizae total phenolic acids
The pharmacological action of salvianolic acid B is strong in total phenolic acid composition of Radix Salviae Miltiorrhizae, and content is the highest in medical material, therefore by measuring the content of salvianolic acid B, can compare the quality of red sage root water soluble ingredient extracting method.
1 instrument and reagent
Day island proper Tianjin LC-10AT high performance liquid chromatograph; Day island proper Tianjin SPD-6A UV-detector; The salvianolic acid B reference substance, Kunming is with holding medical company limited; Acetonitrile is a chromatographically pure;
Methanol, formic acid are analytical pure; Water is the deionization redistilled water.
2 methods and result
2.1 chromatographic condition
Chromatographic column: BeckmanC 16Chromatographic column (4.6 * 25cm, 5 μ m); Mobile phase: methanol-acetonitrile-water-formic acid=42: 5: 52: 1, flow velocity: 1ml/min detects wavelength 285nm;
Column temperature: room temperature; Salvianolic acid B reference substance retention time is 14min, quantitative approach: external standard method.
2.2 content assaying method
2.2.1 it is an amount of that the salvianolic acid B reference substance is got in the reference substance solution preparation, the accurate title, decide, and adds water and make the salvianolic acid B solution that mass concentration is 0.1mg/ml, as salvianolic acid B reference substance stock solution.The accurate stock solution 5ml that draws puts in the brown measuring bottle of 50ml, and thin up shakes up to scale, as the salvianolic acid B reference substance solution.
2.2.2 the need testing solution preparation is got dry porphyrize and crossed the about 0.2g of Radix Salviae Miltiorrhizae fine powder of 40 mesh sieves, accurate title is fixed, adds water 40ml, behind the supersound process 20min, filters, and filtrate places the brown measuring bottle of 50ml, adds water and is diluted to scale, shakes up and promptly gets need testing solution A.Other gets dry porphyrize and crosses the about 0.2g of Radix Salviae Miltiorrhizae fine powder of 40 mesh sieves, and accurate the title decides, and adds pH and be 10 aqueous alkali 40ml, behind the supersound process 20min, filter, filtrate places the brown measuring bottle of 50ml, transfer about pH to 6, add water and be diluted to scale, shake up and promptly get need testing solution B.
2.2.3 the making of standard curve
Salvianolic acid B is in the scope of 4.0~16.0 μ g/ml, and concentration and peak area are good linear relationship, r=0.9995, regression equation: y=1.6482 * 10 6C-1732.
2.2.4 the accurate test sample 20 μ l that draw of precision test, continuous sample introduction 3 times, the RSD of salvianolic acid B are 2.1%.
2.2.5 the response rate is tested, and precision is weighed into a certain amount of salvianolic acid B reference substance in the Radix Salviae Miltiorrhizae solution A of measuring content of danshinolic acid B, handles and measures by identical method, the average recovery rate of salvianolic acid B is 96.5%, and RSD is 1.3%.
2.3 sample determination is drawn test sample 20 μ l, sample introduction calculates content according to standard curve, the results are shown in Table 1.
Measurement result (the mgg of content of danshinolic acid B in table 1 sample -1)
Measure lot number
Sample
1 2 3 4 5 X
Radix Salviae Miltiorrhizae test sample A 54 49 51 53 58 53
Radix Salviae Miltiorrhizae test sample B 463 625 557 672 481 559.6
Experiment two: freeze-drying powder injection containing red-rooted salvia safflower, DANHONG ZHUSHEYE are to the influence of hemorheology of rat
One, experiment material
60 of SD rats are provided by No.1 Military Medical Univ.'s Experimental Animal Center, and body weight 200 ± 20g is male.Epinephrine, the biochemical-pharmaceutical factory, Shanghai; DANHONG ZHUSHEYE, three river pharmaceutical Co. Ltds produce; Danshen freeze-drying preparation (the contained crude drug amount of Danshen freeze-drying preparation 10mg and DANHONG ZHUSHEYE 1ml is suitable), Tianzhijiao Medication Development Co., Ltd., Guangdong's laboratory provides; Radix Salviae Miltiorrhizae Injection, honest day fine pharmaceutical Co. Ltd.
Two, experimental technique
60 of rats are divided 6 groups at random: A normal control group (normal saline group), B blood stasis model group, C DANHONG ZHUSHEJI group 0.15ml/kg, D DANHONG ZHUSHEJI group 0.3ml/kg, E freeze-drying powder injection containing red-rooted salvia safflower group 1.5mg/kg, F freeze-drying powder injection containing red-rooted salvia safflower group 3mg/kg, G positive control Radix Salviae Miltiorrhizae Injection group 0.3ml/kg.Every day 1 time, continuous im administration 7d, 30min after the last administration, except that matched group with the 0.9%NS, all the other respectively organize equal subcutaneous injection 0.1% epinephrine (0.9mg/kg), behind the 30min rat are put into frozen water cryostat 8min, inject the equivalent epinephrine again behind the 2h at interval, preparation blood stasis model.Abdominal aortic blood 5ml, anticoagulant heparin is measured 10s -1, 40s -1, 200s -1Whole blood viscosity, plasma viscosity, packed cell volume.Laboratory temperature is controlled at (20 ± 1) ℃.
Three, experimental result
Compare with normal group, basic, normal, high whole blood viscosity, plasma viscosity, Fibrinogen, the packed cell volume of cutting rate of blood stasis model group all obviously raises (P<0.01), illustrates that model is reliable.Compare with model group, freeze-drying powder injection containing red-rooted salvia safflower and injection group, positive control Radix Salviae Miltiorrhizae Injection group all can obviously be improved hemorheology index (P<0.05); Freeze-drying powder injection containing red-rooted salvia safflower group curative effect is better than the injection group, and experimental result sees Table 2.
Table 2 vermilion injection to the hemorheological influence of acute blood stasis rat model (x ± s,
n=10)
Group agent QI and blood viscosity
The plasma viscosity packed cell volume
Do not measure 10s -140s -1200s -1
A - 20.77±5.27 11.51±2.84 6.91±1.01 1.55±0.09 0.40±0.04
B - 38.16±9.05 * 16.64±2.34 * 8.39±0.69 * 1.80±0.07 * 0.48±0.03 *
1.5mg/
C 21.64±5.37 a 11.73±2.23 a 6.46±0.43 a 1.68±0.04 a 0.39±0.03 a
kg
D 3mg/kg 16.74±2.48 a 9.81±1.27 a 6.43±0.53 a 1.67±0.13 a 0.39±0.03 a
0.15ml
E 28.47±9.47 a 14.36±3.17 7.55±0.58 a 1.70±0.14 0.40±0.03 a
/kg
0.3ml/
F 23.67±4.82 a 11.98±3.43 a 6.85±0.56 a 1.68±0.07 a 0.39±0.04 a
kg
0.3ml/
G 22.06±4.93 a 11.08±2.07 a 6.53±0.80 a 1.66±0.11 a 0.40±0.05 a
kg
Annotate: * and normal group be P<0.01 relatively, aCompare P<0.05 with model group
The specific embodiment
Embodiment one: 1000 bottles of specifications
(1) Radix Salviae Miltiorrhizae 1500g pulverizes, and is that aqueous alkali 10 or more is carried 2 times with pH, and temperature is 80 ℃, the first time 60min, the second time 120min, merge extractive liquid, is extracting solution A;
(2) Flos Carthami 500g, with 40% alcohol reflux 3 times, each 90min reclaims ethanol to there not being the alcohol flavor, extracting solution B;
(3) will add 5 times of water gagings with the Flos Carthami medicinal residues behind the ethanol extraction, be that 3~5 sour water is carried 3 times with pH, and temperature is 20 ℃, each 120min, merge extractive liquid,, extracting solution C;
(4) merge extractive liquid, A and C, centrifugal, get supernatant, concentrating under reduced pressure, transfer pH 6.5~7, last macroporous resin earlier is washed till no Molish reaction with deionized water, continues to be washed till eluent with 20% ethanol and adds 1% ferric chloride reagent and do not have tangible phenolic hydroxyl group reaction, eluent and concentrated ammonia solution and only do not develop the color.Reclaim alcohol eluen, concentrate extracting solution D;
(5) merge extractive liquid, B and D, replenish water for injection to ormal weight, stir evenly, cold preservation, filtration, add injection mannitol 200g, add injection lactose 200g, transfer PH 6.5~7, filtrate adds proper amount of active carbon and boils 15min, puts coldly, is filtered to clear and bright, get solution, sterilization back packing, lyophilization, gland is promptly.
Embodiment two: 100 bottles of specifications
(1) Radix Salviae Miltiorrhizae 150g pulverizes, and is that aqueous alkali more than 10 is carried 3 times with pH, and temperature is 80 ℃, 60min at every turn, and merge extractive liquid, is extracting solution A;
(2) Flos Carthami 50g, with 80% alcohol reflux 2 times, each 60min reclaims ethanol to there not being the alcohol flavor, extracting solution B;
(3) will add 50 times of water gagings with the Flos Carthami medicinal residues behind the ethanol extraction, be that 3~5 sour water is carried 2 times with pH, and temperature is 80 ℃, each 30min, merge extractive liquid,, extracting solution C;
(4) merge extractive liquid, A and C, centrifugal, get supernatant, concentrating under reduced pressure, transfer pH 6.5~7, last macroporous resin earlier is washed till no Molish reaction with deionized water, continues to be washed till eluent with 90% ethanol and adds 1% ferric chloride reagent and do not have tangible phenolic hydroxyl group reaction, eluent and concentrated ammonia solution and only do not develop the color.Reclaim alcohol eluen, concentrate extracting solution D;
(5) merge extractive liquid, B and D replenish water for injection to ormal weight, stir evenly, cold preservation, filtration, add injection mannitol 30g, transfer PH 6.5~7, filtrate adds proper amount of active carbon and boils 15min, puts coldly, is filtered to clear and bright, get solution, sterilization back packing, lyophilization, gland is promptly.
Embodiment three: 500 bottles of specifications
(1) Radix Salviae Miltiorrhizae 750g pulverizes, and is that aqueous alkali more than 10 is carried 2 times with pH, and temperature is 100 ℃, 60min at every turn, and merge extractive liquid, is extracting solution A;
(2) Flos Carthami 250g, with 60% alcohol reflux 2 times, each 90min reclaims ethanol to there not being the alcohol flavor, extracting solution B;
(3) will add 10 times of water gagings with the Flos Carthami medicinal residues behind the ethanol extraction, be that 3~5 sour water is carried 3 times with pH, and temperature is 40 ℃, each 90min, merge extractive liquid,, extracting solution C;
(4) merge extractive liquid, A and C, centrifugal, get supernatant, concentrating under reduced pressure, transfer pH 6.5~7, last macroporous resin earlier is washed till no Molish reaction with deionized water, continues to be washed till eluent with 40% ethanol and adds 1% ferric chloride reagent and do not have tangible phenolic hydroxyl group reaction, eluent and concentrated ammonia solution and only do not develop the color.Reclaim alcohol eluen, concentrate extracting solution D;
(5) merge extractive liquid, B and D replenish water for injection to 10000ml, add mannitol, glucose 250g, stirring and dissolving, and aseptic filtration, cillin bottle is distributed into every bottle of 20ml, lyophilization, packing, promptly.
Embodiment four: 200 bottles of specifications
(1) Radix Salviae Miltiorrhizae 300g pulverizes, and is that aqueous alkali 10 or more is carried 2 times with pH, and temperature is 90 ℃, the first time 90min, the second time 120min, merge extractive liquid, is extracting solution A;
(2) Flos Carthami 100g, with 60% alcohol reflux 2 times, 90min for the first time, 120min for the second time reclaims ethanol to there not being the alcohol flavor, extracting solution B;
(3) will add 25 times of water gagings with the Flos Carthami medicinal residues behind the ethanol extraction, be that 3~5 sour water is carried 2 times with pH, and temperature is 60 ℃, 90min for the first time, 120min for the second time, merge extractive liquid,, extracting solution C;
(4) merge extractive liquid, A and C, centrifugal, get supernatant, concentrating under reduced pressure, transfer pH 6.5~7, last macroporous resin earlier is washed till no Molish reaction with deionized water, continues to be washed till eluent with 60% ethanol and adds 1% ferric chloride reagent and do not have tangible phenolic hydroxyl group reaction, eluent and concentrated ammonia solution and only do not develop the color.Reclaim alcohol eluen, concentrate extracting solution D;
(5) merge extractive liquid, B and D, replenish water for injection to ormal weight, stir evenly, cold preservation, filtration, add injection mannitol 50g, add injection lactose 50g, transfer PH 6.5~7, filtrate adds proper amount of active carbon and boils 15min, puts coldly, is filtered to clear and bright, get solution, sterilization back packing, lyophilization, gland is promptly.

Claims (6)

1 one kinds of Danhong freez-fried powder injectas is characterized in that what it was made up of phenolic acid that extracts and the flavonoid effective site extracted from Flos Carthami from Radix Salviae Miltiorrhizae.
2 phenolic acid effective kind parts according to claim 1 is characterized in that it is that after extracting solution was adjusted to neutrality, last macroporous adsorptive resins was used the alcoholic solution eluting after using the active component of potass extraction Radix Salviae Miltiorrhizae earlier, and purification makes.
3 flavonoid effective sites according to claim 1, it is characterized in that it is earlier to keep dimeric chalcon effective kind part in the Flos Carthami with alcohol reflux, the reuse sour water is carried, acid water extracting liquid and Radix Salviae Miltiorrhizae extract be adjusted to neutral back resin column, use the alcoholic solution eluting, purification makes.
4 according to claim 2 and the 3 described macroporous adsorbent resins that are used for purification effective site, it is characterized in that it can be nonpolar, low pole or polar macroporous adsorption resin, and preferred low pole macroporous adsorbent resin comprises AB-8 and D 101
5 according to claim 2 and the 3 described macroporous adsorptive resins purification of using, and with the alcoholic solution eluting, it is characterized in that used concentration of ethanol is 20~90%.
The preparation method of 6 one kinds of freeze-drying powder injection containing red-rooted salvia safflowers is characterized in that may further comprise the steps:
(1) Radix Salviae Miltiorrhizae is pulverized, and is that aqueous alkali more than 10 is carried 2~3 times with pH, and temperature is 80~100 ℃, each 60~120min, and merge extractive liquid, is extracting solution A;
(2) Flos Carthami is with 40~80% alcohol reflux 2~3 times, and each 60~120min reclaims ethanol to there not being the alcohol flavor, extracting solution B;
(3) will add 5~50 times of water gagings with the Flos Carthami medicinal residues behind the ethanol extraction, be that 3~5 sour water is carried 2~3 times with pH, and temperature is 20~80 ℃, each 30~120min, merge extractive liquid,, extracting solution C;
(4) merge extractive liquid, A and C, centrifugal, get supernatant, concentrating under reduced pressure, transfer pH6.5~7, last macroporous resin column earlier is washed till no Molish reaction with deionized water, continues to be washed till eluent with 20~90% ethanol and adds 1% ferric chloride reagent and do not have tangible phenolic hydroxyl group reaction, eluent and concentrated ammonia solution and only do not develop the color.Reclaim alcohol eluen, concentrate extracting solution D;
(5) merge extractive liquid, B and D replenish water for injection to ormal weight, stir evenly, cold preservation, filtration, add freeze-dried excipient, transfer PH6.5~7, filtrate adds proper amount of active carbon and boils 15min, puts coldly, is filtered to clear and bright, get solution, sterilization back packing, lyophilization, gland is promptly.
CN 200310125148 2003-12-26 2003-12-26 Freeze-dried Danhong powder injection for injection and its preparing method Expired - Fee Related CN1220489C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1301707C (en) * 2005-03-18 2007-02-28 邹巧根 Danhong freeze dried powder injection agent and its preparation method
CN1911219B (en) * 2005-08-12 2010-05-05 山东绿叶天然药物研究开发有限公司 Medicine composition, and its application
CN101455292B (en) * 2008-12-31 2012-06-27 华南理工大学 Preparation method of molasses-phenolate
CN105012387A (en) * 2015-07-06 2015-11-04 江苏神龙药业有限公司 Method for rapid preparation of salvia extract for injection

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1301707C (en) * 2005-03-18 2007-02-28 邹巧根 Danhong freeze dried powder injection agent and its preparation method
CN1911219B (en) * 2005-08-12 2010-05-05 山东绿叶天然药物研究开发有限公司 Medicine composition, and its application
CN101455292B (en) * 2008-12-31 2012-06-27 华南理工大学 Preparation method of molasses-phenolate
CN105012387A (en) * 2015-07-06 2015-11-04 江苏神龙药业有限公司 Method for rapid preparation of salvia extract for injection

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