CN1895353B - Preparation of compound Danshen tablets - Google Patents
Preparation of compound Danshen tablets Download PDFInfo
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- CN1895353B CN1895353B CN200610036097A CN200610036097A CN1895353B CN 1895353 B CN1895353 B CN 1895353B CN 200610036097 A CN200610036097 A CN 200610036097A CN 200610036097 A CN200610036097 A CN 200610036097A CN 1895353 B CN1895353 B CN 1895353B
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Abstract
A process for preparing the compound danshin tablet includes such steps as extracting the liposoluble component containing danshinone from red sage root by supercritical CO2, extracting danshinolic acid by a alcohol deposition method, extracting arasaponin from notoginseng by alcohol, mixing them with starch, drying, granulating, adding borneol powder, stirring, die pressing and coating.
Description
Technical field
The present invention relates to herbal pharmaceutical, more specifically saying so is applicable to a kind of Chinese medicine manufacture method for the treatment of cardiovascular disease.
Background technology
The Chinese medicine compound Radix Salviae Miltiorrhizae Tabellae has recorded in the Pharmacopoeia of the People's Republic of China of version in 1985,1990,2000,2005, to the composition of FUFANG DANSHEN PIAN, and the weight of every kind of composition has clear and definite record and also on the books to the preparation method of FUFANG DANSHEN PIAN in the pharmacopeia.According to the method for making in the version pharmacopeia in 2005: Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g, Radix Salviae Miltiorrhizae added alcohol heating reflux 1.5 hours, extracting solution filters, filtrate recycling ethanol also is concentrated in right amount, and standby: medicinal residues add 50% alcohol heating reflux 1.5 hours, and extracting solution filters, filtrate recycling ethanol also is concentrated into an amount of, 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, makes granule, drying with above-mentioned concentrated solution and an amount of adjuvant.The Borneolum Syntheticum porphyrize with above-mentioned granule mixing, is pressed into 3000, the bag film-coat.
There are following problem in prescription and preparation method according to the pharmacopeia record:
1, the amount of the contained active component of raw material Radix Salviae Miltiorrhizae of various places differs, and except indivedual areas, the FUFANG DANSHEN PIAN active component contents that most of area produces can not guarantee, drug effect also is difficult to guarantee, sees Table 1 and table 2.
Table 1 medicine detects 2000 the 9th 7 phases of volume Shaoxing medicine inspecting institute
| Manufacturer | Date of manufacture | Tanshinone I I AContent, the mg/ sheet |
| The new light in Zhejiang | 99.08.20 | 0.393 |
| The new light in Zhejiang | 99.02.26 | 0.398 |
| The Guangdong Phaleria macrocarpa | 98.12.29 | 0.176 |
| The two dragons in Jinhua | 99.03.12 | 0.163 |
| Jiangxi three more | 98.12.02 | 0.115 |
| Wide army Longhua | 99.03.02 | 0.144 |
| Wide army Longhua | 99.05.18 | 0.118 |
| Wide army Longhua | 99.04.16 | 0.103 |
| The Guangdong Longchuan | 98.09.05 | 0.126 |
| Manufacturer | Date of manufacture | Tanshinone I I AContent, the mg/ sheet |
| The Guangdong Longchuan | 98.12.01 | 0.068 |
| Hongsuihe River, Guangxi | 99.04.04 | 0.076 |
| Guangzhou China difficult to understand | 98.05.18 | 0.052 |
| Heyuan | 98.09.05 | 0.101 |
The attached n=3 of institute of table 2 Chinese Hospitals pharmaceutical journal 2000 the 20th volumes the 5th phase Guiyang Medical College
Last table has been announced the testing result of 33 batches of medicines, and its qualification rate only is 27.2%.Cause above result's main cause to have two, one, raw materials used defective, the 2nd, TANSHINONES is degraded in the leaching process.
2, document (Fructus Perillae core etc. the tanshinol extract concentrate, chemical composition change research in the drying process. Chinese patent medicine 1997,19 (11): 5) report: the tanshinol extract is in distillation, evaporation, dry run, chemical change has taken place in tanshinone, and the principal element of quickening to change is water and heat.
According to document (Lin Hengbiao etc. the stability study of tanshinone. traditional Chinese medical science research .2005,18 (8): result 16), the tanshinone alcoholic solution remains 87.62% behind the placement 24h down at 80 ℃, the tanshinone aqueous solution is remaining 28.20% at 80 ℃ after down placing 24h, also explanation wet with heat be the principal element of the degraded of tanshinone.
Document (is looked into one-tenth, extract the craft discussion of tanshinone. the time precious traditional Chinese medical science traditional Chinese medicines .2002,13 (9): 517) result who has compared Radix Salviae Miltiorrhizae ethanol extraction and supercritical extraction method is that super critical extraction is better than ethanol extraction method, its reason be with short production cycle, need not heating, therefore avoided the degradation reaction of tanshinone.Test data sees Table 3.
The result of table 3 Radix Salviae Miltiorrhizae Different Extraction Method relatively
| Technology | Content |
| Alcohol extracting method | 0.170 |
| Super critical extraction | 0.246 |
Can know from above bibliographical information, wet is influence the principal element that tanshinone is degraded with heat, and to have ethanol, 50% ethanol, moisture to get indescribably concentrated owing to officinal method, and heated time is long, and moisture is also many, therefore extracts in the concentration process and degrades unavoidably.
Above document description can not guarantee the content of active component in the FUFANG DANSHEN PIAN by officinal manufacture method, just can not ensure the quality of products, and has directly caused guaranteeing drug effect.And adopt supercritical carbon dioxide that Radix Salviae Miltiorrhizae is extracted, it only is abundant extraction to liposoluble constituents such as tanshinones in the Radix Salviae Miltiorrhizae, that is to say can not be to the abundant extraction of active component all in the Radix Salviae Miltiorrhizae, so, single also can not guarantee its quality and drug effect with supercritical carbon dioxide extraction technology, this is an one, and it two is that the Radix Notoginseng of putting down in writing in the pharmacopeia is to be used as medicine with fine powder, so also caused drug dose big, used inconvenient.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of FUFANG DANSHEN PIAN can fully be extracted effective ingredient in the medical material, improves effective ingredient concentration in the medicine, improves curative effect.
Another object of the present invention is to reduce taking dose.
Technical solution of the present invention is:
1. extract the active effective ingredient of Radix Salviae Miltiorrhizae
A) get red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure is 15～45Mpa, 30～60 ℃ of extraction temperature, resolve pressure 1～10Mpa, 35～60 ℃ of resolution temperatures, carbon dioxide flow are 5～15L/h, entrainer ethanol flow 1～5mL/min, extraction time 2～5h, extract are evaporated to the extractum that relative density is 1.20～1.40 (55～60 ℃).
B) with the water extraction twice of the Radix Salviae Miltiorrhizae slag after the supercritical extraction, add the water of 6～15 times of amounts for the first time, 55～100 ℃ were refluxed 1～3 hour, filtered; The water that adds for the second time 5～15 times of amounts, 55～100 ℃ were refluxed 1～3 hour, filter, merging filtrate and to be evaporated to relative density be 1.10～1.30 (55～60 ℃) concentrated solution, adding ethanol to amount of alcohol is 50～70%, left standstill 12～24 hours, and got supernatant, under 55～60 ℃ of conditions, be concentrated into relative density and be 1.30～1.40 extractum.
2. extract the active effective ingredient of Radix Notoginseng
The pseudo-ginseng section, twice of alcohol extraction, add for the first time 5～10 times of 65～95% alcohol reflux 1～3h, filter, add for the second time 5～8 times of 50～70% alcohol reflux 1～3h, merge extractive liquid, and to be evaporated to relative density under 55～60 ℃ of conditions be 1.10～1.30 clear paste, spray drying gets the yellowish-brown powder.
3. produce FUFANG DANSHEN PIAN
Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, mixing, and compacting is wrapped film-coat in flakes.
Better manufacture method of the present invention
1. extract the active effective ingredient of Radix Salviae Miltiorrhizae
A) get red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 20～32Mpa, 35～55 ℃ of extraction temperature, resolve pressure 1～10Mpa, 35～60 ℃ of resolution temperatures, carbon dioxide flow are 5～15L/h, entrainer ethanol flow 1～5mL/min, extraction time 2～5h, extract are evaporated to the extractum that relative density is 1.20～1.40 (55～60 ℃).
B) with the water extraction twice of the Radix Salviae Miltiorrhizae slag after the supercritical extraction, add the water of 6～15 times of amounts for the first time, 60～85 ℃ were refluxed 1～3 hour, filtered; The water that adds for the second time 5～15 times of amounts, 60～85 ℃ were refluxed 1～3 hour, filter, merging filtrate and to be evaporated to relative density be 1.10～1.30 (55～60 ℃) concentrated solution, adding ethanol to amount of alcohol is 50～70%, left standstill 12～24 hours, and got supernatant, under 55～60 ℃ of conditions, be concentrated into relative density and be 1.30～1.40 extractum.
2. extract the active effective ingredient of Radix Notoginseng
The pseudo-ginseng section, twice of alcohol extraction, add for the first time 5～10 times of 70～90% alcohol reflux 1～3h, filter, add for the second time 5～8 times of 54～66% alcohol reflux 1～3h, merge extractive liquid, and to be evaporated to relative density under 55～60 ℃ of conditions be 1.10～1.30 clear paste, spray drying gets the yellowish-brown powder.
3. produce FUFANG DANSHEN PIAN
Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, mixing, and compacting is wrapped film-coat in flakes.
Better manufacture method of the present invention
1. extract the active effective ingredient of Radix Salviae Miltiorrhizae
A) get red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 23～28Mpa, 40～50 ℃ of extraction temperature, resolve pressure 1～10Mpa, 35～60 ℃ of resolution temperatures, carbon dioxide flow are 5～15L/h, entrainer ethanol flow 1～5mL/min, extraction time 2～5h, extract are evaporated to the extractum that relative density is 1.20～1.40 (55～60 ℃).
B) with the water extraction twice of the Radix Salviae Miltiorrhizae slag after the supercritical extraction, add the water of 6～15 times of amounts for the first time, 65～75 ℃ were refluxed 1～3 hour, filtered; The water that adds for the second time 5～15 times of amounts, 65～75 ℃ were refluxed 1～3 hour, filter, merging filtrate and to be evaporated to relative density be 1.10～1.30 (55～60 ℃) concentrated solution, adding ethanol to amount of alcohol is 50～70%, left standstill 12～24 hours, and got supernatant, under 55～60 ℃ of conditions, be concentrated into relative density and be 1.30～1.40 extractum.
2. extract the active effective ingredient of Radix Notoginseng
The pseudo-ginseng section, twice of alcohol extraction, add for the first time 5～10 times of 75～85% alcohol reflux 1～3h, filter, add for the second time 5～8 times of 58～62% alcohol reflux 1～3h, merge extractive liquid, and to be evaporated to relative density under 55～60 ℃ of conditions be 1.10～1.30 clear paste, spray drying gets the yellowish-brown powder.
3. produce FUFANG DANSHEN PIAN
Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, mixing, and compacting is wrapped film-coat in flakes.
Best manufacture method of the present invention
1. extract the active effective ingredient of Radix Salviae Miltiorrhizae
A) get red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 25Mpa, 40 ℃ of extraction temperature, resolve pressure 6Mpa, 45 ℃ of resolution temperatures, carbon dioxide flow are 10L/h, entrainer ethanol flow 2mL/min, extraction time 3h, extract are evaporated to the extractum that relative density is 1.40 (55～60 ℃).
B) with the water extraction twice of the Radix Salviae Miltiorrhizae slag after the supercritical extraction, add the water of 10 times of amounts for the first time, 70 ℃ were refluxed 2 hours, filtered; The water that adds for the second time 10 times of amounts, 70 ℃ were refluxed 2 hours, filter, merging filtrate and to be evaporated to relative density be 1.20 (55～60 ℃) concentrated solution, adding ethanol to amount of alcohol is 60%, left standstill 12～24 hours, and got supernatant, under 55～60 ℃ of conditions, be concentrated into relative density and be the extractum of 1.30～1.40 (55～60) ℃.
2. extract the active effective ingredient of Radix Notoginseng
The pseudo-ginseng section, alcohol extraction twice adds 6 times of 80% alcohol reflux 2h for the first time, filter, add for the second time 6 times of 60% alcohol reflux 2h, merge extractive liquid, and to be evaporated to relative density under 55～60 ℃ of conditions be 1.20 clear paste, spray drying gets the yellowish-brown powder.
3. produce FUFANG DANSHEN PIAN
Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, mixing, and compacting is wrapped film-coat in flakes.
According to data, the decomposing cause of tanshinone mainly is wet and hot, and the process conditions of supercritical carbon dioxide extraction generally are to carry out under 25Mpa, 40 ℃ condition, extract with a concentrated step and finish, it is used that to carry dosage secretly few, do not add entry etc. in addition, therefore adopt supercritical carbon dioxide extraction method to replace original alcohol heating reflux to extract Radix Salviae Miltiorrhizae, substantially solved tanshinone because thermal sensitivity causes the problem of degraded in process of production, no matter all be higher than traditional extraction process from yield and effective ingredient concentration.
Adopt supercritical carbon dioxide extraction method to extract Radix Salviae Miltiorrhizae, Tanshinone I I
AYield can be up to 80%; And traditional extraction technique, Tanshinone I I
AYield be lower than 50%.Also illustrated and changed technology outstanding feature afterwards.
Table 4 tanshinone yield relatively
| Formula ratio g | The amount of making/sheet | Tanshinone/% in the Radix Salviae Miltiorrhizae | Tanshinone mg/ sheet in the product | Tanshinone yield % | |
| The pharmacopeia FUFANG DANSHEN PIAN | 450 | 1000 | 0.21 | 0.398 | 42.1 |
| FUFANG DANSHEN PIAN of the present invention (concentrating sheet) | 1350 | 1000 | 0.21 | 2.3 | 81.1 |
Supercritical carbon dioxide extraction fat-soluble tanshinone, but also have an important activity position salvianolic acid in the Radix Salviae Miltiorrhizae, salvianolic acid is a water-soluble substances, so the Radix Salviae Miltiorrhizae slag that the present invention crosses supercritical carbon dioxide extraction carries out water extraction.Except that containing water miscible salvianolic acid, also contain other impurity such as water-soluble sugar in the Radix Salviae Miltiorrhizae slag, in order to improve the purity of salvianolic acid, also be simultaneously for preparation of the present invention concentrates sheet extract amount can not be excessive, otherwise can not satisfy the requirement of the amount of making.Therefore by the method for precipitate with ethanol some water-solubility impurities beyond the salvianolic acid are removed.
Radix Salviae Miltiorrhizae of the present invention extracts by the water extract-alcohol precipitation method behind supercritical carbon dioxide extraction again, compares with the pharmacopeia manufacture method.
The comparison of table 5 inventive method and official method
Generally about 8%, behind the Radix Notoginseng ethanol extraction in the inventive method, arasaponin content is about about 50% in concentrating powder for the content of arasaponin in the Radix Notoginseng fine powder, and extraction ratio is generally 80%.
List related content explanation in the quality standard of pharmacopeia FUFANG DANSHEN PIAN and FUFANG DANSHEN PIAN of the present invention (concentrate sheet) below.
The quality standard of the FUFANG DANSHEN PIAN of table 5 FUFANG DANSHEN PIAN of the present invention and official method relatively
| FUFANG DANSHEN PIAN | FUFANG DANSHEN PIAN (concentrating sheet) | |
| Tanshinone | Must not be less than the 0.20mg/ sheet | Must not be less than the 0.60mg/ sheet |
| Salvianolic acid B | Must not be less than the 5.0mg/ sheet | Must not be less than the 18.0mg/ sheet |
| Day dose | One time 3,3 times on the one. | One time 1,3 times on the one. |
Can learn that from last table active constituent content makes three times of product effective ingredient in the product that the present invention makes for the pharmacopeia manufacture method.
Table 7 the present invention and officinal manufacture method can be compared by following table
| Project | The invention technology | Known technology |
| Prescription | Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g | Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g |
| Radix Salviae Miltiorrhizae | Reuse water extract-alcohol precipitation after the supercritical extraction | 50% ethanol extraction behind 95% ethanol extraction, the reuse decocting boils. |
| Ethanol extraction | Do not extract, fine powder is used as medicine |
| Project | The invention technology | Known technology |
| Borneolum Syntheticum | Fine powder is used as medicine | Fine powder is used as medicine |
| Characteristics | Fat-soluble extracting section is complete, and TANSHINONES is not decomposed, and water extract-alcohol precipitation has improved salvianolic acid class content; The Radix Notoginseng alcohol extraction has improved the content of arasaponin. | TANSHINONES can be decomposed, and salvianolic acid content is low; Arasaponin content is low. |
Advantage of the present invention is to fill a part extraction to effective ingredient in the medical material, improves effective ingredient concentration in the medicine, improves curative effect, reduces taking dose.
The specific embodiment
Embodiment one:
[prescription] Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g
The present invention gets red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 25Mpa, 40 ℃ of extraction temperature, resolve pressure 6Mpa, 45 ℃ of resolution temperatures, carbon dioxide flow are 10L/h, entrainer ethanol flow 2mL/min, extraction time 3h, extract are evaporated to the extractum that relative density is 1.40 (55～60 ℃); Radix Salviae Miltiorrhizae slag after the supercritical extraction with water extraction twice, is added the water of 10 times of amounts the first time, and 70 ℃ were refluxed 2 hours, filtered; The water that adds for the second time 10 times of amounts, 70 ℃ were refluxed 2 hours, filter, merging filtrate and to be evaporated to relative density be 1.20 (55～60 ℃) concentrated solution, adding ethanol to amount of alcohol is 60%, left standstill 12～24 hours, and got supernatant, being concentrated into relative density is the extractum of 1.30～1.40 (55～60 ℃).The pseudo-ginseng section, alcohol extraction twice adds 6 times of 80% alcohol reflux 2h for the first time, filters, and adds 6 times of 60% alcohol reflux 2h for the second time, and merge extractive liquid, also is evaporated to the clear paste that relative density is 1.20 (55～60 ℃), and spray drying gets the yellowish-brown powder.Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, and mixing is pressed into 1000, the bag film-coat.
Embodiment two
[prescription] Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g
The present invention gets red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 15Mpa, 30 ℃ of extraction temperature, resolve pressure 1Mpa, 35 ℃ of resolution temperatures, carbon dioxide flow are 5L/h, entrainer ethanol flow 1mL/min, extraction time 2h, extract are evaporated to the extractum that relative density is 1.20 (55 ℃); Radix Salviae Miltiorrhizae slag after the supercritical extraction with water extraction twice, is added the water of 6 times of amounts the first time, and 55 ℃ were refluxed 1 hour, filtered; The water that adds for the second time 5 times of amounts, 55 ℃ were refluxed 1 hour, filtered, merging filtrate and to be evaporated to relative density be 1.10 (55 ℃) concentrated solution, adding ethanol to amount of alcohol is 50%, leaves standstill 12 hours, get supernatant, being concentrated into relative density is the extractum of 1.30 (55 ℃).The pseudo-ginseng section, alcohol extraction twice adds 5 times of 65% alcohol reflux 1h for the first time, filters, and adds 5 times of 50% alcohol reflux 1h for the second time, and merge extractive liquid, also is evaporated to the clear paste that relative density is 1.10 (55 ℃), and spray drying gets the yellowish-brown powder.Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, and mixing is pressed into 1000, the bag film-coat.
Embodiment three
[prescription] Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g
The present invention gets red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 45Mpa, 60 ℃ of extraction temperature, resolve pressure 10Mpa, 60 ℃ of resolution temperatures, carbon dioxide flow are 15L/h, entrainer ethanol flow 5mL/min, extraction time 5h, extract are evaporated to the extractum that relative density is 1.40 (60 ℃); Radix Salviae Miltiorrhizae slag after the supercritical extraction with water extraction twice, is added the water of 15 times of amounts the first time, and 100 ℃ were refluxed 3 hours, filtered; The water that adds for the second time 15 times of amounts, 100 ℃ were refluxed 3 hours, filtered, merging filtrate and to be evaporated to relative density be 1.30 (60 ℃) concentrated solution, adding ethanol to amount of alcohol is 70%, leaves standstill 24 hours, get supernatant, being concentrated into relative density is the extractum of 1.40 (60 ℃).The pseudo-ginseng section, alcohol extraction twice adds 10 times of 95% alcohol reflux 3h for the first time, filters, and adds 8 times of 70% alcohol reflux 3h for the second time, and merge extractive liquid, also is evaporated to the clear paste that relative density is 1.30 (60 ℃), and spray drying gets the yellowish-brown powder.Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, and mixing is pressed into 1000, the bag film-coat.
Claims (2)
1. the manufacture method of a FUFANG DANSHEN PIAN is characterized in that:
Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g
1. extract the active effective ingredient of Radix Salviae Miltiorrhizae
A) get red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 15Mpa, 30 ℃ of extraction temperature, resolve pressure 1Mpa, 35 ℃ of resolution temperatures, carbon dioxide flow are 5L/h, entrainer ethanol flow 1mL/min, extraction time 2h, it is 1.20 extractum that extract is evaporated to relative density at 55 ℃;
B) with the water extraction twice of the Radix Salviae Miltiorrhizae slag after the supercritical extraction, add the water of 6 times of amounts for the first time, 55 ℃ were refluxed 1 hour, filtered; The water that adds for the second time 5 times of amounts, 55 ℃ were refluxed 1 hour, filtered, merging filtrate and to be evaporated to relative density at 55 ℃ be 1.10 concentrated solution, adding ethanol to amount of alcohol is 50%, leaves standstill 12 hours, get supernatant, being concentrated into relative density at 55 ℃ is 1.30 extractum;
2. extract the active effective ingredient of Radix Notoginseng
Pseudo-ginseng section, alcohol extraction twice adds 5 times of 65% alcohol reflux 1h for the first time, filters, and adds 5 times of 50% alcohol reflux 1h for the second time, merge extractive liquid, and to be evaporated to relative density at 55 ℃ be 1.10 clear paste, spray drying gets the yellowish-brown powder;
3. produce FUFANG DANSHEN PIAN
Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, and mixing is pressed into 1000, the bag film-coat.
2. the manufacture method of a FUFANG DANSHEN PIAN is characterized in that:
Radix Salviae Miltiorrhizae 1350g, Radix Notoginseng 423g, Borneolum Syntheticum 24g
1. extract the active effective ingredient of Radix Salviae Miltiorrhizae
A) get red rooted salvia, be ground into coarse powder, in the supercritical extraction reactor of packing into, extracting pressure 25Mpa, 40 ℃ of extraction temperature, resolve pressure 6Mpa, 45 ℃ of resolution temperatures, carbon dioxide flow are 10L/h, entrainer ethanol flow 2mL/min, extraction time 3h, it is 1.40 extractum that extract is evaporated to relative density at 55～60 ℃;
B) with the water extraction twice of the Radix Salviae Miltiorrhizae slag after the supercritical extraction, add the water of 10 times of amounts for the first time, 70 ℃ were refluxed 2 hours, filtered; The water that adds for the second time 10 times of amounts, 70 ℃ were refluxed 2 hours, filter, merging filtrate and to be evaporated to relative density at 55～60 ℃ be 1.20 concentrated solution, adding ethanol to amount of alcohol is 60%, left standstill 12～24 hours, and got supernatant, being concentrated into relative density at 55～60 ℃ is 1.30～1.40 extractum;
2. extract the active effective ingredient of Radix Notoginseng
Pseudo-ginseng section, alcohol extraction twice adds 6 times of 80% alcohol reflux 2h for the first time, filters, and adds 6 times of 60% alcohol reflux 2h for the second time, merge extractive liquid, and to be evaporated to relative density at 55～60 ℃ be 1.20 clear paste, spray drying gets the yellowish-brown powder;
3. produce FUFANG DANSHEN PIAN
Radix Notoginseng is extracted powder and appropriate amount of starch, and with last two kinds of Radix Salviae Miltiorrhizae extractum mixings, drying is made granule, adds the Borneolum Syntheticum fine powder, and mixing is pressed into 1000, the bag film-coat.
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| CN102240322A (en) * | 2011-07-01 | 2011-11-16 | 天圣制药集团股份有限公司 | Compound red sage root tablet and preparing process thereof |
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| CN103054946B (en) * | 2013-02-01 | 2014-10-29 | 山东华信制药集团股份有限公司 | Countercurrent extraction process and preparation process for compound salvia miltiorrhiza tablets |
| CN103494878A (en) * | 2013-10-08 | 2014-01-08 | 南京正亮医药科技有限公司 | Preparation method and application of compound danshen tablets |
| CN105582051A (en) * | 2016-03-02 | 2016-05-18 | 南京正亮医药科技有限公司 | Preparation method and application of compound salvia miltiorrhiza tablet |
| CN106490607B (en) * | 2016-09-30 | 2019-11-29 | 湖北省轻工业科学研究设计院 | A kind of cordyceps sinensis gracilis polysaccharide piece and preparation method thereof |
| CN108096319B (en) * | 2018-01-22 | 2020-12-18 | 一力制药股份有限公司 | Compound salvia miltiorrhiza film coated tablet and preparation process thereof |
| CN113350264A (en) * | 2021-06-18 | 2021-09-07 | 周宇 | Compound red sage root oral preparation and its preparing process |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424096A (en) * | 2002-12-31 | 2003-06-18 | 北京采瑞医药有限公司 | Composite red sage root micro-capsules for cardio-cerebral diseases and its preparing method |
| CN1733069A (en) * | 2005-08-19 | 2006-02-15 | 袁洪 | Oral cavity spray containing two effective parts of compound red sage root formula and its preparation process |
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2006
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1424096A (en) * | 2002-12-31 | 2003-06-18 | 北京采瑞医药有限公司 | Composite red sage root micro-capsules for cardio-cerebral diseases and its preparing method |
| CN1733069A (en) * | 2005-08-19 | 2006-02-15 | 袁洪 | Oral cavity spray containing two effective parts of compound red sage root formula and its preparation process |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102240322A (en) * | 2011-07-01 | 2011-11-16 | 天圣制药集团股份有限公司 | Compound red sage root tablet and preparing process thereof |
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| CN1895353A (en) | 2007-01-17 |
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