CN101002828B - Method for preparing Danhong injection, and products thereof - Google Patents
Method for preparing Danhong injection, and products thereof Download PDFInfo
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- CN101002828B CN101002828B CN2007100006578A CN200710000657A CN101002828B CN 101002828 B CN101002828 B CN 101002828B CN 2007100006578 A CN2007100006578 A CN 2007100006578A CN 200710000657 A CN200710000657 A CN 200710000657A CN 101002828 B CN101002828 B CN 101002828B
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Abstract
A Chinese medicine 'Danhong injection' is prepared from red sage root and safflower through respective extracting, concentrating, removing impurities, testing the content of active components, proportional mixing, and conventionally preparing injection. Its product is also disclosed.
Description
Technical field
The present invention relates to a kind of preparation method of injection, relating in particular to a kind of is the preparation method of the injection that is used for the treatment of cardiovascular disease such as coronary heart disease, angina pectoris that forms of feedstock production and the product that is prepared by method with vegetable crude drug Radix Salviae Miltiorrhizae and Flos Carthami, belongs to biomedicine field.
Background technology
It is not smoothgoing puckery that DANHONG (Radix Salviae Miltiorrhizae, Flos Carthami) injection is widely used in chest pain, cardiopalmus, facial hemiparalysis, speech that treatment coronary heart disease, angina pectoris, myocardial infarction, ischemic encephalopathy, cerebral thrombosis and pulmonary heart disease cause clinically, numb limbs and tense tendons, movable unfavorable disease such as grade all has better curative effect.Traditional preparation method is earlier with the rare alcohol extraction of red rooted salvia of recipe quantity, and filtering residue is carried with the flos carthami mixing water of recipe quantity again, merging filtrate, concentrate, accent etc. oozes, transfers PH, cold preservation 24h, filters, and supplies liquid measure, fill and must product.
Because Chinese medicine has the notion of " genuine medicinal materials ",, just very likely cause the kind of effective ingredient in the medical material and content to produce than big-difference if therefore the medical material kind is different with the place of production.With the Radix Salviae Miltiorrhizae is example, documents and materials and author's experimentation show: because the kind of Radix Salviae Miltiorrhizae is different with the place of production, the content difference of contained effective ingredient danshensu and protocatechualdehyde is also bigger in the medical material, fluctuation range is respectively 318-680% (mg/g) and 42.5-88% (mg/g), and content can differ more than 1 times.Flos Carthami and for example, the author studies show that with medical material place of production difference, the content of Flavonoid substances is 20-30% (g/g) in the Flos Carthami, gap is also very big.This just makes different manufacturers in all parts of the country only bigger with the feed intake contained active constituent content difference of different batches related preparations of producing of Radix Salviae Miltiorrhizae, the flos carthami of recipe quantity, causes the control of product quality difficulty bigger, and product percent of pass is low.The producer that has is defective because of active constituent content in the product detects, and causes product to be scrapped in batch, causes the significant wastage of manpower, financial resources and resource; That have in addition because of product defective, just in product, add the index composition merely, as danshensu, protocatechualdehyde, rutin etc., thereby influence natural drug is brought into play whole curative effect as the system of each component fixed mixing ratio wherein superiority, finally influenced the stable performance of clinical efficacy.
Summary of the invention
Technical problem to be solved by this invention is to overcome the deficiencies in the prior art, and a kind of preparation method of new DANHONG ZHUSHEYE is provided, and is relatively stable by the prepared content of effective that obtains in the product of this method, realizes quality control easily.
Technical problem to be solved by this invention realizes by following technological approaches:
A kind of preparation method of DANHONG ZHUSHEYE may further comprise the steps:
(1) prepare extracting solution I: the medicinal ethanol percolate extraction of Radix Salviae Miltiorrhizae, reclaim ethanol, add gelatin and remove tannin, to filter, filtrate is condensed into clear paste, and clear paste is filtered, and filtrate cold preservation gets extracting solution I;
(2) preparation extracting solution II: Flos Carthami hot water lixiviate, lixiviating solution filters, and filtrate is condensed into clear paste, and clear paste is filtered, and filtrate cold preservation gets extracting solution II;
(3) extracting solution I 50-80ml and extracting solution II10-15ml are mixed, add proper amount of water for injection (add the volume that makes solution behind the water for injection to the 800-950ml all can), adding sodium chloride accent etc. oozes, mixing filters, adjust pH to 3.5～6.5 add the injection water to 1000ml, fine straining, fill, sterilization, promptly.
In the above-mentioned preparation method, in the step (1): salvia piece was not had the medical material surface with 50～95% medicinal alcohols (preferably using 60～70% medicinal alcohols), 40～75 ℃ (preferably using 70 ℃) soaks 0.5～3.0h (being preferably 1h), insulation percolation is down extracted, and control fluid speed is 1～15ml/min.cm
2(be preferably 3～5ml/min.cm
2), shunt ethanol at any time, the control liquid outlet quantity is 8～10 times of Radix Salviae Miltiorrhizae weight (w/v); Described concentrate is meant that it is the clear paste of 0.50～2.00 (being preferably relative density is 1.10～1.20) that filtrate is condensed into 65 ℃ of relative densities when measuring; Described clear paste filters and is meant clear paste with 0.45 μ m micro-pore-film filtration; Described cold preservation is meant 0～4 ℃ of following cold preservation.
In the step (2): Flos Carthami is with 70～95 ℃ of hot water (being preferably 80～90 ℃ of hot water) lixiviate secondary, each 0.5～3.0h (being preferably each 1h), add for the first time 70～95 ℃ of hot water of 5～20 times of amounts (being preferably 8 times of amounts) (being preferably 80～90 ℃ of hot water), add 70～95 ℃ of hot water of 3～10 times of amounts (being preferably 6 times of amounts) (being preferably 80～90 ℃ of hot water) for the second time; Described concentrate is meant that it is the clear paste of 0.50～2.00 (being preferably relative density is 1.10～1.20) that filtrate is condensed into 65 ℃ of relative densities when measuring; Described clear paste filters and is meant clear paste with 0.45 μ m micro-pore-film filtration; Described cold preservation is meant 0～4 ℃ of following cold preservation.
In the step (3): described fine straining is meant with 0.45 μ m micro-pore-film filtration.
After testing, among resulting extracting solution I of above-mentioned preparation method and the extracting solution II, active constituent content is high and stable, contains Radix Salviae Miltiorrhizae with danshensu (C among wherein every 1ml extracting solution I
9H
10O
5) and protocatechualdehyde (C
7H
6O
3) the total amount meter greater than 10mg; Contain total flavones with rutin (C among every 1ml extracting solution II
27H
30O
16) count greater than 500mg.
By the DANHONG ZHUSHEYE that the inventive method prepares, contain danshensu (C in every 1ml injection
9H
10O
5) 0.48～9.6mg (being preferably 0.48～4.8mg, 0.48～2.4mg, 0.48～1.2mg, 0.5～1.2mg, 0.6～1.2mg, 0.7～1.2mg, 0.8～1.2mg, 0.8mg successively), protocatechualdehyde (C
7H
6O
3) 0.06～1.8mg (being preferably 0.06～1.2mg, 0.06～0.8mg, 0.06～0.6mg, 0.06～0.4mg, 0.06～0.1mg, 0.06～0.08mg, 0.06～0.08mg, 0.06mg successively), total flavones is (with rutin (C
27H
30O
16) meter) 5.4～114mg (being preferably 5.4～60mg, 5.4～32mg, 5.4～18mg, 5.6～16mg, 6.6～13mg, 7.6～12.8mg, 8.6～12.8mg, 8.6mg successively), this injection content of beary metal is lower than 9.4ppm; PH value is 3.5～6.5.
The inventive method is extracted Radix Salviae Miltiorrhizae, two kinds of raw materials of Flos Carthami respectively, concentrate respectively, roguing, measure the extract active constituent content respectively after, be hybridly prepared into injection by a certain percentage.Preparation method of the present invention can make the product active constituent content accurate, constant product quality, and quality control is simple and direct, easy; The inventive method can suitably be adjusted the ratio of intermediate according to the height of intermediate active constituent content during formulated product, reach and save medical material, handled easily, the purpose of shortening production cycle.
The specific embodiment
The invention will be further described below by embodiment.Should be pointed out that these embodiment only are illustrations of the present invention, should not be construed as limitation of the present invention.
Embodiment 1
1, gets salvia piece 7.5kg, add 60% ethanol and do not have the decoction pieces surface, behind (70 ℃) warm macerating 1h, adorn percolator in the water-bath, 70 ℃ of 60% warm ethanol percolate extraction of reuse, control fluid speed 3ml/min.cm
2When liquid outlet quantity reaches 75L, stop percolation, shift percolate and to the ethanol recycling can, reclaim ethanol.Water liquid transfers in the jacketed pan, be heated to and do not have the alcohol flavor, it is an amount of to add 5% gelatin solution, being stirred to does not have the precipitation generation, filters, and the logical vapour of filtrate reuse jacketed pan is concentrated into the clear paste that relative density is 1.10 (65 ℃), stop vapour, cross the microporous filter membrane of 0.45 μ m, filtrate is put in 0～4 ℃ of cold room and to be stored standbyly, is extracting solution I (about 2.5L);
Extracting solution I active constituent content measuring:
Measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol-1% glacial acetic acid solution (13: 87) is a mobile phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the danshensu peak should be not less than 5000.
The preparation of reference substance solution: precision takes by weighing danshensu sodium, the protocatechualdehyde reference substance is an amount of, adds water respectively and makes the solution that every 1ml contains 50 μ g, promptly.
The preparation of need testing solution: accurate amount is drawn extracting solution I 5ml, puts in the 20ml measuring bottle, and thin up shakes up to scale; The accurate again liquid 1ml that draws after diluting puts in the 20ml measuring bottle, and thin up shakes up promptly to scale.
Algoscopy: accurate respectively reference substance and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Measurement result: the every 1ml of extracting solution I contains Radix Salviae Miltiorrhizae with danshensu (C
9H
10O
5) and protocatechualdehyde (C
7H
6O
3) total amount count 12mg.
2, get Flos Carthami dry product 2.5kg, in the dress extractor, insulation is down with 90 ℃ of hot water lixiviate secondaries, each 1h, add for the first time 20L hot water, add 15L hot water for the second time, the filter back merges secondary filtrate, the dress jacketed pan, being concentrated into relative density is the clear paste of 1.10 (65 ℃), stops vapour, crosses 0.45 μ m microporous filter membrane, filtrate is standby in 0～4 ℃ of cold preservation, is extracting solution II (about 0.8L).
Extracting solution II effective ingredient (total flavones) assay:
Measure according to spectrophotography (appendix VB of Chinese Pharmacopoeia version in 2000).
The preparation of reference substance solution: precision takes by weighing the control substance of Rutin 20mg that is dried to constant weight through 120 ℃, puts in the 100ml measuring bottle, and it is an amount of to add 50% methanol, and jolting makes dissolving and is diluted to scale, shakes up, and promptly gets (every 1ml contains anhydrous rutin 0.2mg).
The preparation of standard curve: precision is measured reference substance solution 1.0ml, 2.0ml, 3.0ml, 4.0ml, 5.0ml, put respectively in the 10ml measuring bottle, respectively add 50% methanol, add 5% sodium nitrite solution 0.3ml to 5ml, shake up, placed 6 minutes, and added 10% aluminum nitrate solution 0.3ml, shake up, placed 6 minutes, hydro-oxidation sodium test solution 4ml adds 50% methanol again to scale, shakes up.With corresponding solution is blank.According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2000 B), measure trap at 500nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
Algoscopy: the accurate extracting solution II 5ml that draws, to put in the 100ml measuring bottle, thin up shakes up to scale; The accurate again liquid 1ml that draws after diluting puts in the 100ml measuring bottle, and thin up shakes up to scale.Precision is measured the liquid 1ml after the dilution for the second time, puts in the 10ml measuring bottle, adds 50% methanol to scale, shakes up, as blank.Precision is measured the liquid 1ml after diluting for the second time in addition, puts in the 10ml measuring bottle method under the sighting target directrix curve preparation, from " adding 50% methanol " to 5ml, measure trap immediately in accordance with the law, read the weight that is equivalent to rutin the need testing solution from standard curve, calculate, promptly.
Measurement result: the every 1ml of extracting solution II contains total flavones with rutin (C
27H
30O
16) meter=545mg.
3. after extracting solution I 50ml and extracting solution II 11ml mix, add the nearly 850ml of injection water, add sodium chloride 7g, miscible, filter, adjust pH is 4, adds the injection water to 1000ml, with 0.45 μ m filtering with microporous membrane, fill, 2ml/ props up, flowing steam, and sterilization 30min gets 500.
Embodiment 2
1. get in the salvia piece 10kg dress strap clamp layer percolator, add 70% ethanol and do not have the medical material surface, interlayer reaches 70 ℃ to the interior liquid temperature of tube for flowing steam, and 1h is soaked in insulation, and the beginning percolation replenishes ethanol, and controlling the percolate flow velocity is 5ml/min.cm
2, 70 ℃ of logical vapour insulations are when effluent reaches 80L, stop percolation, percolate is transferred to alcohol distillation column and reclaims ethanol, and water liquid is transferred in the jacketed pan, add 5% gelatin solution, stir, do not produce until there being precipitation, after leaving standstill 0.5h, filter, filtrate concentrates, to relative density is the clear paste of 1.10 (65 ℃), with 0.45 μ m filtering with microporous membrane, in 0～4 ℃ of cold room, store standbyly, be extracting solution I (about 3.5L).
High effective liquid chromatography for measuring according to embodiment 1: the every 1ml of extracting solution I contains Radix Salviae Miltiorrhizae with danshensu (C
9H
10O
5) and protocatechualdehyde (C
7H
6O
3) total amount count 10.5mg.
2. get Flos Carthami dry product 3.4kg, in the dress strap clamp layer extractor, add 28L water, the logical vapour of interlayer is heated to water liquid and reaches 90 ℃, stops vapour insulation 1h, filters, add 21L water again in extractor, logical vapour is heated to 90 ℃, insulation 1h, filter, merge filtrate twice, be transferred in the triple effect evaporator concentrated, when concentrated solution reaches relative density and is 1.10 (65 ℃), with 0.45 μ m filtering with microporous membrane, in 0～4 ℃ of cold room, store standbyly, be extracting solution II (about 1.2L).
According to the spectrophotometry of embodiment 1, the every 1ml of extracting solution II contains total flavones in rutin=520mg.
3. with after extracting solution I 50ml and the extracting solution II 10ml mixing, add the nearly 900ml of injection water, add sodium chloride 7g, percolation filters, adjust pH is 6, adds the injection water to 1000ml, with 0.45 μ m filtering with microporous membrane, fill, 10ml/ props up, flowing steam, and distillation sterilization 30min gets 100.
Embodiment 3
1, gets salvia piece 7.5kg, add 50% ethanol and do not have the decoction pieces surface, behind (40 ℃) warm macerating 3h, adorn percolator in the water-bath, 40 ℃ of 50% warm ethanol percolate extraction of reuse, control fluid speed 1ml/min.cm
2When liquid outlet quantity reaches 60L, stop percolation, shift percolate and to the ethanol recycling can, reclaim ethanol.Water liquid transfers in the jacketed pan, be heated to and do not have the alcohol flavor, it is an amount of to add 5% gelatin solution, being stirred to does not have the precipitation generation, filters, and the logical vapour of filtrate reuse jacketed pan is concentrated into the clear paste that relative density is 0.60 (65 ℃), stop vapour, cross the microporous filter membrane of 0.45 μ m, filtrate is put in 0～4 ℃ of cold room and to be stored standbyly, is extracting solution I (about 2.0L);
High effective liquid chromatography for measuring according to embodiment 1: the every 1ml of extracting solution I contains Radix Salviae Miltiorrhizae with danshensu (C
9H
10O
5) and protocatechualdehyde (C
7H
6O
3) total amount count 10.4mg.
2, get Flos Carthami dry product 2.5kg, in the dress extractor, insulation is down with 70 ℃ of hot water lixiviate secondaries, each 3h, add for the first time 12.5L hot water, add 7.5L hot water for the second time, the filter back merges secondary filtrate, the dress jacketed pan, being concentrated into relative density is the clear paste of 0.60 (65 ℃), stops vapour, crosses 0.45 μ m microporous filter membrane, filtrate is standby in 0～4 ℃ of cold preservation, is extracting solution II (about 0.5L).
According to the spectrophotometry of embodiment 1, the every 1ml of extracting solution II contains total flavones in rutin=510mg.
3, get extracting solution I 80ml, extracting solution II 15ml adds the nearly 920ml of injection water, adds sodium chloride 7g, and percolation filters, adjust pH is 3.5, adds the injection water to 1000ml, with 0.45 μ m filtering with microporous membrane, fill, 10ml/ props up, flowing steam, and distillation sterilization 30min gets 100.
Embodiment 4
1, gets salvia piece 7.5kg, add 95% ethanol and do not have the decoction pieces surface, behind (75 ℃) warm macerating 0.5h, adorn percolator in the water-bath, 75 ℃ of 95% warm ethanol percolate extraction of reuse, control fluid speed 15ml/min.cm
2When liquid outlet quantity reaches 75L, stop percolation, shift percolate and to the ethanol recycling can, reclaim ethanol.Water liquid transfers in the jacketed pan, be heated to and do not have the alcohol flavor, it is an amount of to add 5% gelatin solution, being stirred to does not have the precipitation generation, filters, and the logical vapour of filtrate reuse jacketed pan is concentrated into the clear paste that relative density is 2.00 (65 ℃), stop vapour, cross the microporous filter membrane of 0.45 μ m, filtrate is put in 0～4 ℃ of cold room and to be stored standbyly, is extracting solution I (about 2.0L);
High effective liquid chromatography for measuring according to embodiment 1: the every 1ml of extracting solution I contains Radix Salviae Miltiorrhizae with danshensu (C
9H
10O
5) and protocatechualdehyde (C
7H
6O
3) total amount count 10.6mg.
2, get Flos Carthami dry product 2.5kg, in the dress extractor, insulation is down with 95 ℃ of hot water lixiviate secondaries, each 0.5h, add for the first time 40L hot water, add 25L hot water for the second time, the filter back merges secondary filtrate, the dress jacketed pan, being concentrated into relative density is the clear paste of 2.00 (65 ℃), stops vapour, crosses 0.45 μ m microporous filter membrane, filtrate is standby in 0～4 ℃ of cold preservation, is extracting solution II (about 0.7L).
According to the spectrophotometry of embodiment 1, the every 1ml of extracting solution II contains total flavones in rutin=515mg.
3, get extracting solution I 60ml, extracting solution II 15ml adds the nearly 900ml of injection water, adds sodium chloride 7g, and percolation filters, adjust pH is 6.5, adds the injection water to 1000ml, with 0.45 μ m filtering with microporous membrane, fill, 10ml/ props up, flowing steam, and distillation sterilization 30min gets 100.
Test example 1 Different Extraction Method is to the influence of danshensu, protocatechualdehyde and total flavones yield
1, Different Extraction Method is to the influence of danshensu, protocatechualdehyde yield in the Radix Salviae Miltiorrhizae
The Radix Salviae Miltiorrhizae traditional extraction process is a medical material with the Diluted Alcohol warm macerating of 20-40% 2 times, and medicinal residues reuse water temperature is soaked 2 times, each 1 hour; Method of the present invention is that medical material uses the ethanol of 50-95% to extract 0.5-3 hour at 40-75 ℃ of following percolation.
Precision takes by weighing 6 parts of red rooted salvias, every part of 10g.3 parts are adopted traditional method for extracting, and every part adds 10 times of weight Diluted Alcohols and 10 times of weight water extraction respectively, filter, and merging filtrate, being concentrated into relative density is the clear paste of 1.10-1.20 (65 ℃); In addition 3 batches adopt respectively method of the present invention (batch 1: medical material with 70% ethanol 70 ℃ of following percolation extractions 1 hour; Batches 2: medical material extracted 3 hours at 40 ℃ of following percolation with 60% ethanol; Batches 3: medical material extracted 1 hour at 75 ℃ of following percolation with 65% ethanol) percolation extracts, and treats to stop percolation when effluent reaches 100ml, and being concentrated into relative density is the clear paste of 1.10-1.20 (65 ℃).Measure content according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000), the results are shown in Table 1:
Table 1, Different Extraction Method are to the influence (mg/ml) of danshensu, protocatechualdehyde total yield
| Batch | The tradition extraction method | Extraction method of the present invention |
| 1 | 9.18 | 12.00 |
| 2 | 10.30 | 11.36 |
| 3 | 9.85 | 11.78 |
2, Different Extraction Method is to the influence of total flavones yield in the Flos Carthami
The traditional extracting method of Flos Carthami is to adopt warm water (30 ℃～40 ℃) to soak each 1 hour 2 times; Method of the present invention is with hot water lixiviate 2 times, each 1 hour.
Precision takes by weighing 6 parts on Flos Carthami, every part of 1.0g.3 parts are adopted traditional extraction process, and every part adds water 100ml (batch 30 ℃ of warm water soaking of 1 usefulness at every turn; Batch 35 ℃ of warm water soaking of 2 usefulness; Batch 40 ℃ of warm water soaking of 3 usefulness), extract 2 times, filter, merging filtrate, being concentrated into relative density is the clear paste of 1.10-1.20 (65 ℃);
3 parts are adopted method of the present invention to extract 2 times in addition, add hot water (batch 80 ℃ of hot water extraction of 1 usefulness every part of first time; Batch 70 ℃ of hot water extraction of 2 usefulness; Batch 95 ℃ of hot water extraction of 3 usefulness) 8ml adds water 6ml for the second time, filters, and merging filtrate, being concentrated into relative density is the clear paste of 1.10-1.20 (65 ℃).Measure content according to spectrophotography (appendix VB of Chinese Pharmacopoeia version in 2000), the results are shown in Table 2:
Table 2, Different Extraction Method are to the influence (mg/ml) of total flavones yield in the Flos Carthami
| Batch | The tradition extraction method | Extraction method of the present invention |
| 1 | 532 | 545 |
| Batch | The tradition extraction method | Extraction method of the present invention |
| 2 | 398 | 520 |
| 3 | 465 | 538 |
By table 1, table 2 result as can be known, adopt the effective ingredient intermediate yield of the inventive method preparation generally than traditional method height.
Test example 2 different preparation methoies are to the influence of danshensu, protocatechualdehyde and general flavone content in the product
The preparation method of traditional DANHONG ZHUSHEYE is the red rooted salvia 20-40% rare alcohol extraction of elder generation with recipe quantity, filtering residue is carried with the flos carthami mixing water of recipe quantity again, merging filtrate, concentrate, accent etc. oozes, transfers pH, cold preservation 24h, filters, and supplies liquid measure, fill and must product; The inventive method is that Radix Salviae Miltiorrhizae, two kinds of raw materials of Flos Carthami extract respectively, concentrate respectively, roguing, measure the extract active constituent content respectively after, the technology of mixed preparing by a certain percentage.
Precision takes by weighing 6 parts of red rooted salvias, every part of 750g; 6 parts on Flos Carthami, every part of 250g.3 parts are adopted traditional method for extracting, filter, and merging filtrate, being concentrated into relative density is the clear paste of 1.10-1.20 (65 ℃), is extracting solution A1, A1 is mixed with injection by prescription again; Measure active constituent content in the prepared injection according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2000) and spectrophotography (appendix VB of Chinese Pharmacopoeia version in 2000), the results are shown in Table 3:
Danshensu, protocatechualdehyde and content of total flavone (mg/ml) in table 3, the different preparation method product
By table 3 result as can be known, by the DANHONG ZHUSHEYE of method of the present invention preparation owing to prepare by a certain percentage, so content of effective is relatively stable, controlled in the product according to intermediate active constituent content measuring result; And the active constituent content fluctuating is very big in the product of traditional method preparation, is difficult for carrying out quality control.
Claims (17)
1. method for preparing DANHONG ZHUSHEYE may further comprise the steps:
(1) preparation extracting solution I: Radix Salviae Miltiorrhizae reclaims ethanol with the extraction of 50-95% medicinal alcohol percolation, adds gelatin and removes tannin, filters, and filtrate is condensed into clear paste, and clear paste is filtered, and filtrate cold preservation gets extracting solution I;
(2) preparation extracting solution II: Flos Carthami hot water lixiviate, lixiviating solution filters, and filtrate is condensed into clear paste, and clear paste is filtered, and filtrate cold preservation gets extracting solution II;
(3) according to the height of intermediate active constituent content, extracting solution I 50～80ml and extracting solution II 10～15ml are mixed, add water for injection, add sodium chloride accent etc. and ooze, mixing filters, adjust pH to 3.5～6.5, add water for injection to 1000ml, fine straining, fill, sterilization obtains the DANHONG ZHUSHEYE that content of beary metal is lower than 9.4ppm.
2. according to the preparation method of claim 1, it is characterized in that: step there was not the medical material surface with salvia piece with 50～95% medicinal alcohols in (1), and 40～75 ℃ are soaked 0.5～3.0h, and insulation percolation is down extracted, and control fluid speed is 1～15ml/min.cm
2, shunt ethanol at any time, the control liquid outlet quantity is 8～10 times of Radix Salviae Miltiorrhizae weight; Described concentrate is meant that it is 0.50～2.00 clear paste that filtrate is condensed into 65 ℃ of relative densities when measuring; Described clear paste filters and is meant clear paste with 0.45 μ m micro-pore-film filtration; Described cold preservation is meant 0～4 ℃ of following cold preservation.
3. according to the preparation method of claim 2, it is characterized in that: step there was not the medical material surface with salvia piece with 60～70% medicinal alcohols in (1), and 70 ℃ are soaked 1h; Control fluid speed is 3～5ml/min.cm
2Described concentrate is meant that it is 1.10～1.20 clear paste that filtrate is condensed into 65 ℃ of relative densities when measuring.
4. according to the preparation method of claim 1, it is characterized in that: Flos Carthami is with 70～95 ℃ of hot water lixiviates 2 times in the step (2), and each lixiviate 0.5～3.0h adds 70～95 ℃ of hot water of 5～20 times of weight the first time, adds 70～95 ℃ of hot water of 3～10 times of weight the 2nd time; Described concentrate is meant that it is 0.50～2.00 clear paste that filtrate is condensed into 65 ℃ of relative densities when measuring; Described clear paste filters and is meant clear paste with 0.45 μ m micro-pore-film filtration; Described cold preservation is meant 0～4 ℃ of following cold preservation.
5. according to the preparation method of claim 4, it is characterized in that: Flos Carthami is with 80～90 ℃ of hot water lixiviates 2 times in the step (2), and each 1h adds 8 times for the first time and measures 80～90 ℃ of hot water, adds 80～90 ℃ of hot water of 6 times of weight the 2nd time; Described concentrate is meant that it is 1.10～1.20 clear paste that filtrate is condensed into 65 ℃ of relative densities when measuring.
6. according to the preparation method of claim 1, it is characterized in that: the fine straining described in the step (3) is meant with 0.45 μ m micro-pore-film filtration.
7. according to the preparation method of claim 1, it is characterized in that: among the prepared extracting solution I of step (1), the content of Radix Salviae Miltiorrhizae is in the total amount of danshensu and protocatechualdehyde in this extracting solution of every 1ml, and its content is greater than 10mg; Among the prepared extracting solution II of step (2), contain total flavones in rutin in this extracting solution of every 1ml, its content is greater than 500mg.
8. a DANHONG ZHUSHEYE is characterized in that the product for preparing according to any one described method of claim 1-7.
9. according to the DANHONG ZHUSHEYE of claim 8, it is characterized in that containing danshensu 0.48～9.6mg in the described injection of every 1ml, protocatechualdehyde 0.06～1.8mg, total flavones 5.4～114mg, wherein general flavone content is in rutin; This injection content of beary metal is lower than 9.4ppm; PH value is 3.5～6.5.
10. according to the DANHONG ZHUSHEYE of claim 9, it is characterized in that containing danshensu 0.48～4.8mg in the described injection of every 1ml protocatechualdehyde 0.06～1.2mg, total flavones 5.4～60mg.
11., it is characterized in that containing danshensu 0.48～2.4mg in the described injection of every 1ml protocatechualdehyde 0.06～0.8mg, total flavones 5.4～32mg according to the DANHONG ZHUSHEYE of claim 10.
12., it is characterized in that containing danshensu 0.48～1.2mg in the described injection of every 1ml protocatechualdehyde 0.06～0.6mg, total flavones 5.4～18mg according to the DANHONG ZHUSHEYE of claim 11.
13., it is characterized in that containing danshensu 0.5～1.2mg in the described injection of every 1ml protocatechualdehyde 0.06～0.4mg, total flavones 5.6～16mg according to the DANHONG ZHUSHEYE of claim 12.
14., it is characterized in that containing danshensu 0.6～1.2mg in the described injection of every 1ml protocatechualdehyde 0.06～0.1mg, total flavones 6.6～13mg according to the DANHONG ZHUSHEYE of claim 13.
15., it is characterized in that containing danshensu 0.7～1.2mg in the described injection of every 1ml protocatechualdehyde 0.06～0.08mg, total flavones 7.6～12.8mg according to the DANHONG ZHUSHEYE of claim 14.
16., it is characterized in that containing danshensu 0.8～1.2mg in the described injection of every 1ml protocatechualdehyde 0.06～0.08mg, total flavones 8.6～12.8mg according to the DANHONG ZHUSHEYE of claim 15.
17., it is characterized in that containing danshensu 0.8mg in the described injection of every 1ml protocatechualdehyde 0.06mg, total flavones 8.6mg according to the DANHONG ZHUSHEYE of claim 16.
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| CN101002828B true CN101002828B (en) | 2010-11-03 |
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| CN104688817A (en) * | 2015-03-20 | 2015-06-10 | 广东中西达一新药开发有限公司 | Application of danhong injection liquid as Na+/taurocholate cotransporting polypeptide inhibitor |
| CN105434659A (en) * | 2015-12-08 | 2016-03-30 | 广东艾希德药业有限公司 | Injection treating rheumatic or rheumatoid diseases and preparation method thereof |
| CN105616490A (en) * | 2016-02-16 | 2016-06-01 | 天津中医药大学 | Application of Radix salvia miltiorrhiza and Flos carthami extract in preparing medicine |
| CN107519238A (en) * | 2017-10-22 | 2017-12-29 | 惠州市常青春医药美容保健品实业有限公司 | Analgesia for liver cancer and breast cancer end-stage patients is lengthened the life parenteral solution and its application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1418678A (en) * | 2002-11-27 | 2003-05-21 | 于文勇 | Medicine compositions for treating cardiovascular cranialvascular disease, and its prepn. method |
| CN1520859A (en) * | 2003-01-28 | 2004-08-18 | 黄衍民 | Cerebrovascular and cardiovascular disease treating injection containing red-rooted salvia and safflower |
| CN1640421A (en) * | 2004-01-07 | 2005-07-20 | 山西亚宝药业集团股份有限公司 | Injection danhong of radix salviae miltorrhizae and flos carthami, and its preparing method and quality control method |
| CN1686275A (en) * | 2005-03-18 | 2005-10-26 | 邹巧根 | Danhong freeze dried powder injection agent and its preparation method |
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2007
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1418678A (en) * | 2002-11-27 | 2003-05-21 | 于文勇 | Medicine compositions for treating cardiovascular cranialvascular disease, and its prepn. method |
| CN1520859A (en) * | 2003-01-28 | 2004-08-18 | 黄衍民 | Cerebrovascular and cardiovascular disease treating injection containing red-rooted salvia and safflower |
| CN1640421A (en) * | 2004-01-07 | 2005-07-20 | 山西亚宝药业集团股份有限公司 | Injection danhong of radix salviae miltorrhizae and flos carthami, and its preparing method and quality control method |
| CN1686275A (en) * | 2005-03-18 | 2005-10-26 | 邹巧根 | Danhong freeze dried powder injection agent and its preparation method |
Non-Patent Citations (1)
| Title |
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| 罗海燕.注射用丹红（粉针）的药学研究.成都中医药大学2004届博士学位论文.2004,(2004),第1,7,8,15-20,30-55,101页. * |
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