CN101007074B - Preparing method of Ginseng and Aconite preparation for injection - Google Patents
Preparing method of Ginseng and Aconite preparation for injection Download PDFInfo
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- CN101007074B CN101007074B CN 200610013122 CN200610013122A CN101007074B CN 101007074 B CN101007074 B CN 101007074B CN 200610013122 CN200610013122 CN 200610013122 CN 200610013122 A CN200610013122 A CN 200610013122A CN 101007074 B CN101007074 B CN 101007074B
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Abstract
The invention provides a process for preparing ginseng and monkshood preparation suitable for injection, which is capable of producing with less impurity substance and poisonous substance.
Description
Technical field
The present invention relates to the preparation method technical field of medicine, particularly the preparation method of traditional medicine Injectio.
Background technology
Shenfu decoction derives from " the roman class is wanted ", and main component is Radix Ginseng, gun additioner.By theory of Chinese medical science, its main function is a supplementing QI to revive YANG, cures mainly vigour and loses greatly, the yang-energy sudden collapse.Modern medicine think shenfu decoction can enhancing body resistance, rising blood pressure, improve the body circulation, also have effects such as antiinflammatory, anti-endotoxin effect and antianaphylaxis simultaneously, be applicable to the shock treatment clinically.
Radix Ginseng has the branch of Radix Ginseng and Radix Ginseng Rubra because of the processing method difference, the composition difference that the two is contained, and Radix Ginseng contains ginsenoside Ro, Rb
1, Rb
2, Rc, Rd, Re, Rf, Rg
1, Rg
2Deng; In addition Radix Ginseng Rubra also contains distinctive ginsenoside Rg3, Rh1 and Rh2 and panaxatriol (Panaxatriol).According to the data bibliographical information, Radix Ginseng Rubra is all strong than Radix Ginseng in pharmacological actions such as defying age, antitumor, enhancing animal activity ability, increase heart contraction amplitudes, so this preparation adopts Radix Ginseng Rubra to offer medicine as raw material.
The ginseng polysaccharide has immunization widely, can activating macrophage, panimmunity cells such as T lymphocyte, IAK cell, and promote cytokine to generate, complement activation; Also have effects such as antitumor, antiviral, infection, antiulcer, antioxidation, anti-aging, blood sugar lowering blood fat, useful to this preparation recuperating depleted YANG and rescuing the patient from collapse effect, and have no side effect, should use as active ingredient.
Radix Ginseng Rubra be the cultivation product of Radix Ginseng Panax ginseng C.A.Mey. through steaming the dry root that processes, sweet, the little hardship of nature and flavor, temperature are returned lung, the heart, spleen channel, have good strongly invigorating primordial QI, multiple arteries and veins takes off the function of nourishing qi to stop admittedly.Be used for weak body and prostration, cold extremities faint pulse, QI failing to control blood, metrostaxis; Heart failure, cardiogenic shock etc.
Radix Aconiti Lateralis Preparata is the daughter root processed goods of ranunculaceae plant Aconitum carmichjaelii Debx. Aconitum carmichaeli Debx., nature and flavor suffering, sweet, big heat; Poisonous, GUIXIN, kidney, spleen channel have recuperating depleted YANG and rescuing the patient from collapse, mend the effect that fire is supporing yang, pursue wind-cold damp pathogen.Be used for the YANG-depletion collapse, the cold extremities faint pulse, sexual impotence, cold womb, trusted subordinate's cold type of pain, deficiency and coldness is vomited and diarrhoea, YIN-cold edema, yang deficiency diseases caused by exogenous pathogenic factor, arthralgia due to cold-dampnes.
Domestic literature is to the existing report of Ginseng and Aconite preparation for injection and preparation method thereof, as Chinese patent application 200410002164.4 (publication number CN 1557361, on December 29th, open day), a kind of Shenfu freeze driet powder injection is disclosed, form by Radix Ginseng Rubra, Radix Aconiti Lateralis Preparata effective ingredient and water for injection dissolubility pharmaceutic adjuvant, be characterized in keeping the polysaccharide in the Radix Ginseng, this application also discloses a kind of Shenfu freeze driet powder injection preparation method, and this method comprises: (1) Radix Ginseng Rubra obtains ginsenoside extract through steps such as alcohol extraction, filtration, non-polar solven extractions; (2) with the filtering residue of step (1) through steps such as decocting, precipitate with ethanol, ultrafiltration, obtain polysaccharide solution; (3) RADIX ACONITI LATERALIS PREPARATA obtains the Radix Aconiti Lateralis Preparata extracting solution through steps such as decocting, precipitate with ethanol; (4) merge the said extracted thing, add the adjuvant lyophilization.Zoopery shows that the resulting Shenfu freeze driet powder injection of this method has Antishock function, yet the toxicant aconitine content in the preparation is higher, has limited its application clinically.
Summary of the invention
The invention provides that a kind of to prepare impurity few, toxic chemical content is low, is suitable for the preparation method of the preparation of injection.
The present invention is achieved through the following technical solutions:
A kind of preparation method of Ginseng and Aconite preparation for injection is characterized in that medical material Radix Ginseng and Radix Aconiti Lateralis Preparata weight ratio that it is used are 1: 2, may further comprise the steps:
A. get the Radix Ginseng Rubra coarse powder, the alcohol heating reflux that adds the 70-85% that 7-9 doubly measures extracts 4-6 time, the 1.5-2.5h that at every turn refluxes, filtration, merging filtrate, concentrating under reduced pressure, concentrate adds water, heating for dissolving, cooling, put 0-12 ℃ and place 8-12h, filter, get filtrate, cross pretreated D
101, AB-8 or HPD-100 type macroporous resin, the ethanol elution of water, 30-80% successively, collect ethanol elution, decompression recycling ethanol is not to there being the alcohol flavor, and concentrate adds the ethanol that 15-25 doubly measures 80-90%, heating in water bath, filter, decompression filtrate recycling ethanol, the concentrate vacuum drying promptly gets Radix Ginseng Rubra extract.
B. get the Radix Ginseng Rubra medicinal residues, adding 12-18 times of water gaging decocts 2-4 time, each 2-3h filters merging filtrate, be concentrated into the medical material amount, add ethanol and make and contain alcohol amount and reach 75-85%, leave standstill 12-24h, filter, get filter cake, add the water heating for dissolving and make solution contain the about 1-3% of polysaccharide, centrifugal, filtrate is concentrated into the 1/5-1/3 volume, adding ethanol makes and contains pure 75-85%, leave standstill 12-24h, filter, get filter cake, add the water heating for dissolving and make solution contain the about 1-3% of polysaccharide, centrifugal, the supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate are concentrated into the 1/5-1/3 volume, add ethanol and make and contain pure 75-85%, leave standstill 12-24h, filter, the filter cake heating for dissolving also makes solution contain polysaccharide to be 5-15%, to add the 25-35% tannic acid aqueous solution and produce to no longer including precipitation, centrifugal, supernatant concentration is 5-15% to containing polysaccharide, adds ethanol and makes and contain pure 75-85%, leaves standstill 12-24h, filter, filter cake adds the pure water heating for dissolving and makes solution contain the about 5-15% of polysaccharide, and is centrifugal, and supernatant adds ethanol to be made and contain pure 75-85%, leave standstill 12-24h, filter, filter cake adds the water heating for dissolving and makes solution contain the about 5-15% of polysaccharide, and is centrifugal, supernatant adds ethanol to be made and contains pure 75-85%, leave standstill 12-24h, filter, filter cake 90-98% washing with alcohol 2-4 time, lyophilization gets the Radix Ginseng Rubra total polysaccharides.
C. get Radix Aconiti Lateralis Preparata, add 20-30 and doubly measure pure water heating decoction 2-4 time, each 4-6h, filter, merging filtrate is concentrated into the medical material amount, add ethanol to containing the alcohol amount, leave standstill 12-24h, sucking filtration for 55-65%, filtrate adds ethanol again to containing the alcohol amount for 75-85%, leaves standstill 12-24h, sucking filtration, filtrate adds ethanol again to containing the alcohol amount for 75-85%, leaves standstill 12-24h, sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract.
D. get above-mentioned Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract, make injection, lyophilized injectable powder or sterilized powder.
Preparation method of the present invention, steps d wherein, extract can be according to conventional method, adds as required or does not add pharmaceutically acceptable carrier, makes injection, lyophilized injectable powder or sterilized powder, preferred lyophilized injectable powder.Extract is prepared into above-mentioned preparation, be to realize easily for those skilled in the art, need not performing creative labour.
Optimized technical scheme of the present invention may further comprise the steps:
A. get the Radix Ginseng Rubra coarse powder, add the 70% medicinal alcohol heating and refluxing extraction 5 times of 8 times of amounts, the 2h that at every turn refluxes filters, merging filtrate, and concentrating under reduced pressure, concentrate adds water, heating for dissolving, cooling is put 10 ℃ and is placed 8-12h, filters, and gets filtrate, crosses pretreated D
101Macroporous resin, water, 60% ethanol elution are collected 60% ethanol elution successively, and decompression recycling ethanol is to there not being the alcohol flavor, concentrate adds 20 times of amount 85% ethanol, and heating in water bath filters, decompression filtrate recycling ethanol, concentrate are put 80 ℃ of vacuum dryings, promptly get Radix Ginseng Rubra extract.
B. get the Radix Ginseng Rubra medicinal residues, add 15 times of water gagings and decoct each 2h 3 times, 2h, 2h, filter, merging filtrate is concentrated into the medical material amount, add 95% ethanol, make to contain alcohol amount and reach 80%, leave standstill 12-24h, filter, get filter cake, add the water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal 4000rpm, 10min, filtrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, get filter cake, add the water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal 4000rpm, 10min, supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, the filter cake heating for dissolving also makes solution contain polysaccharide about 10%, adding 30% tannic acid aqueous solution produces to no longer including precipitation, centrifugal 4000rpm, 10min, supernatant concentration is to containing polysaccharide about 10%, add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal 4000rpm, 10min, supernatant add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, filter cake adds the water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal 4000rpm, 10min, supernatant add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, filter cake is with 95% washing with alcohol 3 times, lyophilization gets the Radix Ginseng Rubra total polysaccharides.
C. get Radix Aconiti Lateralis Preparata, add 20 times of water gaging heating and decoct each 4h 3 times, filter, merging filtrate is concentrated into the medical material amount, adding 95% ethanol is 60% to containing the alcohol amount, leaves standstill 14h, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, leaves standstill 14h, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, leaves standstill 14h, sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract.
D. get recipe quantity Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract, add proper amount of water for injection and make abundant dissolving, add, add activated carbon adsorption 10-20min, filtration, packing, lyophilization with behind an amount of freeze-dried excipient.
The described freeze-dried excipient of steps d of the present invention can be any excipient commonly used, includes but not limited to mannitol, lactose, sucrose, glucose, HP-etc., and these excipient can use separately, also can unite use; Preferred HP-.
Technical scheme of the present invention is a large amount of test of inventor's process, comprises what orthogonal test obtained.
Technical scheme of the present invention has the following advantages:
Do not use other organic solvents beyond the ethanol, the simplification to protection, technology and the equipment of personnel, environment on producing is very helpful; The average yield of step a Radix Ginseng Rubra extract of the present invention is about 4.6%, and the Radix Ginseng total saponins average content is about 70.0%, and the Radix Ginseng total saponins yield on average is about 3.0%; Step b medicinal residues of the present invention are through 5 water-soluble precipitate with ethanol, ultrafiltration and add tannic acid except that albumen, guaranteed the purity of polysaccharide, and wherein ultrafiltration is got molecular weight more than 3000, the macromole below 100,000, and wherein, near the polyoses contents the molecular weight 10,000 account for 99%; Among the present invention, Radix Aconiti Lateralis Preparata is through the processing of step c, and extract yield can not detect aconitine more than 1.95% in the product, has guaranteed security of products.
Adopt optimized technical scheme of the present invention, three batches of lab scale sample extraction of Radix Ginseng Rubra result of study sees Table 1
Three batches of Radix Ginseng Rubra lab scales of table 1 trial-manufacture of sample quality investigation result
Adopt optimized technical scheme of the present invention, three batches of lab scale extracts of Radix Aconiti Lateralis Preparata are investigated and be the results are shown in Table 2
Three batches of lab scale extracts of table 2 Radix Aconiti Lateralis Preparata are investigated the result
The Ginseng and Aconite preparation for injection of the present invention's preparation through a large amount of in vitro testses and zoopery checking, under high dose and low dosage situation, does not all have haemolysis and causes hemagglutinative effect; The shock of white mice being scalded the mice due to property shock, dog hemorrhagic shock and the endotoxin all has significant therapeutic effect.
Among the present invention, Radix Ginseng total saponins content adopts spectrophotography to detect, Radix Ginseng total polysaccharides content adopts HPLC/ differential refraction detection method, and polysaccharide molecular weight distributes and adopts high effective liquid chromatography for measuring, aconitine assay employing high performance liquid chromatography (2000 " first one of Chinese pharmacopoeia).
The specific embodiment
Below in conjunction with embodiment the present invention is elaborated, embodiment should not regard the restriction of many present invention protection domain as.
The preparation of embodiment one Shenfu freeze driet powder injection
Prescription
Radix Ginseng Rubra 300g
Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata) 600g
Pharmaceutic adjuvant is an amount of
Make 1000 bottles of injection lyophilized powders
More than two flavors, get the Radix Ginseng Rubra coarse powder, add 70% medicinal alcohol heating and refluxing extraction 5 times (each 8 times of amounts, backflow 2h), filter, merging filtrate, concentrating under reduced pressure, concentrate add the injection water, heating for dissolving, cooling, put 10 ℃ and place 8-12h, filter, get filtrate, cross pretreated D
101Macroporous resin is used pure water, 60% medicinal alcohol eluting successively, collects 60% ethanol elution, and decompression recycling ethanol is to there not being the alcohol flavor, concentrate adds 20 times of amount 85% ethanol, and heating in water bath filters, decompression filtrate recycling ethanol, concentrate are put 80 ℃ of vacuum dryings, promptly get Radix Ginseng Rubra extract.
Get the Radix Ginseng Rubra medicinal residues, add 15 times of amount pure water and decoct each 2h 3 times, 2h, 2h, filter, merging filtrate is concentrated into the medical material amount, adds 95% ethanol, make and contain alcohol amount and reach 80%, standing over night (about 14 hours) filters, and gets filter cake (total polysaccharides), add the pure water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal (4000rpm, 10min), filtrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, standing over night (about 14 hours) is filtered, and gets filter cake, add the pure water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal (4000rpm, 10min), the supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate is concentrated into 1/4 volume, add 95% alcohol make contain alcohol 80%, standing over night (about 14 hours) is filtered, and the filter cake heating for dissolving also makes solution contain polysaccharide about 10%, add 30% tannic acid aqueous solution and produce (this moment, system contained tannic acid 2%) to no longer including precipitation, centrifugal (4000rpm, 10min), supernatant concentration is to containing polysaccharide about 10%, add 95% ethanol make contain alcohol 80%, standing over night (about 14 hours) is filtered, and filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal (4000rpm, 10min), supernatant add 95% ethanol make contain alcohol 80%, standing over night (about 14 hours), filter, filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal (4000rpm, 10min), supernatant add 95% alcohol make contain alcohol 80%, standing over night is filtered, and filter cake is with 95% washing with alcohol 3 times, lyophilization gets the Radix Ginseng Rubra total polysaccharides.
Get Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata), add the heating of 20 times of amount pure water and decoct each 4h 3 times, filter, merging filtrate is concentrated into the medical material amount, adding 95% alcohol is 60% to containing the alcohol amount, standing over night (about 14 hours), sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% alcohol again, standing over night (about 14 hours), sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night (about 14 hours), sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract.
Get recipe quantity Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract, add 900ml water for injection and make dissolving, medicinal liquid leaves standstill 14h (about 14 hours) in 4 ℃, 0.45 μ m microporous filter membrane filters, filtrate adds with the dissolved HP-of 900ml water for injection again, is heated to 80 ℃, constant temperature, the active carbon that adds 0.2% (w/v) stirs evenly, absorption 15min stirs 2-3 time filtering decarbonization during this period, with remaining 200ml water for injection washing nozzle, cleaning mixture and filtrate are merged, and under aseptic condition, the medicinal liquid warp is with 0.8 μ m, 0.45 μ m, after 0.22 the combined strainer that the filter of μ m microporous filter membrane is formed filters, fill, lyophilization compresses Jiao Gai, takes out, roll lid, promptly.
The preparation of embodiment two Shenfu freeze driet powder injections
Prescription
Radix Ginseng Rubra 300g
Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata) 600g
Pharmaceutic adjuvant is an amount of
Make 1000 bottles of injection lyophilized powders
More than two the flavor, get the Radix Ginseng Rubra coarse powder, add 80% medicinal alcohol heating and refluxing extraction 4 times (each 9 times of amounts, backflow 2.5h), filter merging filtrate, concentrating under reduced pressure, concentrate add injection water, heating for dissolving, cooling, put 4 ℃ and place 8-12h, filter, get filtrate, cross pretreated AB-8 macroporous resin, use pure water, 35% medicinal alcohol eluting successively, collect 35% ethanol elution, decompression recycling ethanol is to there not being the alcohol flavor, concentrate adds 25 times of amount 80% ethanol, heating in water bath filters decompression filtrate recycling ethanol, concentrate is put 80 ℃ of vacuum dryings, promptly gets Radix Ginseng Rubra extract.
Get the Radix Ginseng Rubra medicinal residues, add 12 times of amount pure water and decoct each 3h 4 times, 2h, 2h and 2h, filter, merging filtrate is concentrated into the medical material amount, adds 95% ethanol, make and contain alcohol amount and reach 75%, standing over night filters, and gets filter cake (total polysaccharides), add the pure water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal (4000rpm, 10min), filtrate is concentrated into 1/3 volume, add 95% ethanol make contain alcohol 75%, standing over night is filtered, and gets filter cake, add the pure water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal (4000rpm, 10min), the supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate is concentrated into 1/5 volume, add 95% ethanol make contain alcohol 75%, standing over night is filtered, and the filter cake heating for dissolving also makes solution contain polysaccharide about 10%, add 30% tannic acid aqueous solution and produce (this moment, system contained tannic acid 2%) to no longer including precipitation, centrifugal (4000rpm, 10min), supernatant concentration is to containing polysaccharide about 10%, add 95% ethanol make contain alcohol 80%, standing over night is filtered, and filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal (4000rpm, 10min), supernatant add 95% ethanol make contain alcohol 80%, standing over night, filter, filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal (4000rpm, 10min), supernatant add 95% ethanol make contain alcohol 80%, standing over night is filtered, and filter cake is with 95% washing with alcohol 4 times, lyophilization gets the Radix Ginseng Rubra total polysaccharides.
Get Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata), add the heating of 25 times of amount pure water and decoct 3 times, respectively 4h, 5h and 6h, filter, merging filtrate is concentrated into the medical material amount, adding 95% ethanol is 55% to containing the alcohol amount, standing over night, sucking filtration, it is 75% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night, sucking filtration, it is 75% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night, sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract.
Get recipe quantity Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract, add 900ml water for injection and make dissolving, medicinal liquid leaves standstill 14h (or spending the night) in 4 ℃, 0.45 μ m microporous filter membrane filters, filtrate adds with the dissolved HP-of 900ml water for injection again, is heated to 80 ℃, constant temperature, the active carbon that adds 0.2% (w/v) stirs evenly, absorption 15min stirs 2-3 time filtering decarbonization during this period, with remaining 200ml water for injection washing nozzle, cleaning mixture and filtrate are merged, and under aseptic condition, the medicinal liquid warp is with 0.8 μ m, 0.45 μ m, after 0.22 the combined strainer that the filter of μ m microporous filter membrane is formed filters, fill, lyophilization compresses Jiao Gai, takes out, roll lid, promptly.
The preparation of the attached sterilized powder of embodiment three ginsengs
Prescription
Radix Ginseng Rubra 300g
Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata) 600g
Pharmaceutic adjuvant is an amount of
Make 1000 bottles of injection lyophilized powders
More than two the flavor, get the Radix Ginseng Rubra coarse powder, add 85% medicinal alcohol heating and refluxing extraction 6 times (each 8 times of amounts, backflow 2h), filter merging filtrate, concentrating under reduced pressure, concentrate add injection water, heating for dissolving, cooling, put 4 ℃ and place 8-12h, filter, get filtrate, cross pretreated HPD-100 macroporous resin, use pure water, 75% medicinal alcohol eluting successively, collect 75% ethanol elution, decompression recycling ethanol is to there not being the alcohol flavor, concentrate adds 15 times of amount 90% ethanol, heating in water bath filters decompression filtrate recycling ethanol, concentrate is put 80 ℃ of vacuum dryings, promptly gets Radix Ginseng Rubra extract.
Get the Radix Ginseng Rubra medicinal residues, add 12 times of amount pure water and decoct 4 times, be respectively 2h, 3h, 2h and 3h, filter, merging filtrate is concentrated into the medical material amount, adds 95% ethanol, make and contain alcohol amount and reach 85%, standing over night filters, and gets filter cake (total polysaccharides), add the pure water heating for dissolving and make solution contain polysaccharide about 1%, centrifugal (5000rpm, 10min), filtrate is concentrated into 1/3 volume, add 95% ethanol make contain alcohol 85%, standing over night is filtered, and gets filter cake, add the pure water heating for dissolving and make solution contain polysaccharide about 1%, centrifugal (5000rpm, 10min), the supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate is concentrated into 1/3 volume, add 95% ethanol make contain alcohol 85%, standing over night is filtered, and the filter cake heating for dissolving also makes solution contain polysaccharide about 10%, add 30% tannic acid aqueous solution and produce (this moment, system contained tannic acid 2%) to no longer including precipitation, centrifugal (5000rpm, 10min), supernatant concentration is to containing polysaccharide about 10%, add 95% ethanol make contain alcohol 80%, standing over night is filtered, and filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal (5000rpm, 10min), supernatant add 95% ethanol make contain alcohol 85%, standing over night, filter, filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 15%, centrifugal (5000rpm, 10min), supernatant add 95% ethanol make contain alcohol 85%, standing over night is filtered, and filter cake is with 90% washing with alcohol 3 times, lyophilization gets the Radix Ginseng Rubra total polysaccharides.
Get Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata), add the heating of 25 times of amount pure water and decoct each 5h 2 times, filter, merging filtrate is concentrated into the medical material amount, adding 95% ethanol is 65% to containing the alcohol amount, standing over night, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night, sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract.
Get recipe quantity Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract, add 2000ml water for injection and make dissolving, medicinal liquid leaves standstill 14h in 4 ℃, under aseptic condition, after the combined strainer of medicinal liquid through forming with 0.8 μ m, 0.45 μ m, the filter of 0.22 μ m microporous filter membrane filtered, spray drying promptly.
The preparation of embodiment four SHENFU ZHUSHEYE
Prescription
Radix Ginseng Rubra 1000g
Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata) 2000g
Pharmaceutic adjuvant is an amount of
Make 1000 bottles of injection lyophilized powders
More than two flavors, get the Radix Ginseng Rubra coarse powder, add 80% medicinal alcohol heating and refluxing extraction 6 times (each 7 times of amounts, backflow 1.5h), filter, merging filtrate, concentrating under reduced pressure, concentrate add the injection water, heating for dissolving, cooling, put 4 ℃ and place 8-12h, filter, get filtrate, cross pretreated D
101Macroporous resin is used pure water, 60% medicinal alcohol eluting successively, collects 60% ethanol elution, and decompression recycling ethanol is to there not being the alcohol flavor, concentrate adds 15 times of amount 90% ethanol, and heating in water bath filters, decompression filtrate recycling ethanol, concentrate are put 80 ℃ of vacuum dryings, promptly get Radix Ginseng Rubra extract.
Get the Radix Ginseng Rubra medicinal residues, add 15 times of amount pure water and decoct 4 times, be respectively 2h, 2h, 3h and 3h, filter, merging filtrate is concentrated into the medical material amount, adds 95% ethanol, make and contain alcohol amount and reach 80%, standing over night filters, and gets filter cake (total polysaccharides), add the pure water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal (4000rpm, 10min), filtrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, standing over night is filtered, and gets filter cake, add the pure water heating for dissolving and make solution contain polysaccharide about 2%, centrifugal (4000rpm, 10min), the supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, standing over night is filtered, and the filter cake heating for dissolving also makes solution contain polysaccharide about 10%, add 30% tannic acid aqueous solution and produce (this moment, system contained tannic acid 2%) to no longer including precipitation, centrifugal (4000rpm, 10min), supernatant concentration is to containing polysaccharide about 10%, add 95% ethanol make contain alcohol 80%, standing over night is filtered, and filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 10%, centrifugal (4000rpm, 10min), supernatant add 95% ethanol make contain alcohol 80%, standing over night, filter, filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide about 15%, centrifugal (4000rpm, 10min), supernatant add 95% ethanol make contain alcohol 80%, standing over night is filtered, and filter cake is with 90% washing with alcohol 3 times, lyophilization gets the Radix Ginseng Rubra total polysaccharides.
Get Radix Aconiti Lateralis Preparata (Radix Aconiti Lateralis Preparata), add the heating of 30 times of amount pure water and decoct each 5h 2 times, filter, merging filtrate is concentrated into the medical material amount, adding 95% ethanol is 55% to containing the alcohol amount, standing over night, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, standing over night, sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract.
Get recipe quantity Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract, add 8000ml water for injection and make dissolving, medicinal liquid leaves standstill 14h in 4 ℃, 0.45 μ m microporous filter membrane filters, filtrate adds 0.2% soil temperature-20, under aseptic condition, after the combined strainer of medicinal liquid through forming with 0.8 μ m, 0.45 μ m, the filter of 0.22 μ m microporous filter membrane filters, the water for injection flushing filtrate of reuse 2000ml merges liquid, and packing promptly.
Claims (2)
1. the preparation method of a Ginseng and Aconite preparation for injection is characterized in that medical material Radix Ginseng Rubra and Radix Aconiti Lateralis Preparata weight ratio that it is used are 1: 2, may further comprise the steps:
A. get the Radix Ginseng Rubra coarse powder, add the 70% medicinal alcohol heating and refluxing extraction 5 times of 8 times of amounts, the 2h that at every turn refluxes filters, merging filtrate, and concentrating under reduced pressure, concentrate adds water, heating for dissolving, cooling is put 10 ℃ and is placed 8-12h, filters, and gets filtrate, crosses pretreated D
101Macroporous resin, water, 60% ethanol elution are collected 60% ethanol elution successively, and decompression recycling ethanol is to there not being the alcohol flavor, concentrate adds 20 times of amount 85% ethanol, and heating in water bath filters, decompression filtrate recycling ethanol, concentrate are put 80 ℃ of vacuum dryings, promptly get Radix Ginseng Rubra extract;
B. get the Radix Ginseng Rubra medicinal residues, add 15 times of water gagings and decoct each 2h 3 times, 2h, 2h, filter, merging filtrate is concentrated into the medical material amount, add 95% ethanol, make to contain alcohol amount and reach 80%, leave standstill 12-24h, filter, get filter cake, add the water heating for dissolving and make solution contain polysaccharide 2%, centrifugal 4000rpm, 10min, filtrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, get filter cake, add the water heating for dissolving and make solution contain polysaccharide 2%, centrifugal 4000rpm, 10min, supernatant ultrafiltration, the intercepting molecular weight is 3,000-100,000 filtrate, ultrafiltrate is concentrated into 1/4 volume, add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, the filter cake heating for dissolving also makes solution contain polysaccharide 10%, adding 30% tannic acid aqueous solution produces to no longer including precipitation, centrifugal 4000rpm, 10min, supernatant concentration is to containing polysaccharide 10%, add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, filter cake adds the pure water heating for dissolving and makes solution contain polysaccharide 10%, centrifugal 4000rpm, 10min, supernatant add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, filter cake adds the water heating for dissolving and makes solution contain polysaccharide 10%, centrifugal 4000rpm, 10min, supernatant add 95% ethanol make contain alcohol 80%, leave standstill 12-24h, filter, filter cake is with 95% washing with alcohol 3 times, lyophilization gets the Radix Ginseng Rubra total polysaccharides;
C. get Radix Aconiti Lateralis Preparata, add 20 times of water gaging heating and decoct each 4h 3 times, filter, merging filtrate is concentrated into the medical material amount, adding 95% ethanol is 60% to containing the alcohol amount, leaves standstill 14h, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, leaves standstill 14h, sucking filtration, it is 80% to containing the alcohol amount that filtrate adds 95% ethanol again, leaves standstill 14h, sucking filtration, filtrate decompression reclaims solvent, and vacuum drying promptly gets Radix Aconiti Lateralis Preparata extract:
D. get above-mentioned Radix Ginseng Rubra total polysaccharides, Radix Ginseng Rubra extract and Radix Aconiti Lateralis Preparata extract and make lyophilized injectable powder, be specially: add proper amount of water for injection and make abundant dissolving, add an amount of freeze-dried excipient after, add activated carbon adsorption 10-20min, filtration, packing, lyophilization.
2. the method for claim 1, wherein the used freeze-dried excipient of steps d is a HP-.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1493340A (en) * | 2003-08-29 | 2004-05-05 | 雅安三九药业有限公司 | Ginseng and aconite preparation for treating qi vacuity and yang desertion and its preparation method |
| CN1500518A (en) * | 2002-11-13 | 2004-06-02 | 雅安三九药业有限公司 | Freeze drying powder containing red ginseng and accessory piece for injection |
| CN1557361A (en) * | 2004-01-16 | 2004-12-29 | 张正生 | Freeze dried genseng and prepared aconite root powder injecta and its preparation |
| CN1689593A (en) * | 2004-04-29 | 2005-11-02 | 哈药集团中药二厂 | Method for preparing ginseng and aconite powdered injection |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1500518A (en) * | 2002-11-13 | 2004-06-02 | 雅安三九药业有限公司 | Freeze drying powder containing red ginseng and accessory piece for injection |
| CN1493340A (en) * | 2003-08-29 | 2004-05-05 | 雅安三九药业有限公司 | Ginseng and aconite preparation for treating qi vacuity and yang desertion and its preparation method |
| CN1557361A (en) * | 2004-01-16 | 2004-12-29 | 张正生 | Freeze dried genseng and prepared aconite root powder injecta and its preparation |
| CN1689593A (en) * | 2004-04-29 | 2005-11-02 | 哈药集团中药二厂 | Method for preparing ginseng and aconite powdered injection |
Non-Patent Citations (2)
| Title |
|---|
| 吴荣祖.附子减毒与增效—中药附子传统加工工艺创新研究.《药品评价》.2005,第2卷(第5期), * |
| 胡亚芹等.超滤膜技术在多糖提取方面的应用.《生物技术通讯》.2005,第16卷(第2期), * |
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