CN100490875C - Blackberrylily rhizome antiviral injection, preparation and venous medicine feeding blackberrylily rhizome antiviral injection thereof - Google Patents
Blackberrylily rhizome antiviral injection, preparation and venous medicine feeding blackberrylily rhizome antiviral injection thereof Download PDFInfo
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Abstract
The invention relates to Blackberrylily rhizome antiviral injection, preparation and venous medicine feeding blackberrylily rhizome antiviral injection thereof. The original medicine comprises 1-1000 portion of belamcanda rhizome by weight, 1-1000 portion of honeysuckle by weight, 1-1000 portion of Eupatorium by weight, 1-1000 portion of capilary artemisia by weight, 1-1000 portion of radix bupleuri by weight, 1-1000 portion of dandelion by weight, 1-1000 portion of isatis root by weight, 1-1000 portion of dyers woad leaf by weight. The medicine is obtained by following steps: distilling by vapor, boiling, adding adding clarifier, alcohol-settling, water-settling, centrifugation, hyperfiltration to get active component of the Blackberrylily rhizome antiviral injection, and then subpackaging, disinfecting to get finished preparation, in which the chlorogenic acid (C16H18O9) is not less than 0.5 mg/ml. The injection has the function of antivirus and killing bacteria and relieving inflammation and treating epidemic hemorrhagic fever early disease. The invention avoids the medicine liquid thickness, deposition and color changing, stabilizes the preparation, prolongs the product effective date. The injection can be applied through vein so as to prevent the adverse effects such as pain in the administration location, blood stasis and even muscle necrosis.
Description
Invention field
The present invention relates to a kind of Rhizoma Belamcandae antiviral injection, its preparation method and intravenously administrable Rhizoma Belamcandae antiviral injection belong to field of traditional Chinese.
Background technology
Rhizoma Belamcandae is called black fan, Wu Pu, ghost fan, wild tawny daylily flower, flat bamboo, golden butterfly etc., is the dry rhizome of a Rhizoma Iridis Tectori herbaceos perennial Rhizoma Belamcandae; The property hardship, cold; Main component is belamcandin, Rhizoma Iridis Tectori glycoside, tectorigenin, shekanin, Rhizoma Belamcandae alcohol etc.Rhizoma Belamcandae decocting liquid has the effect of resisting pathogenic microbes.
Flos Lonicerae, another name Flos Lonicerae, Flos Lonicerae, little egret flower, Soviet Union's flower, JINHUA, Flos Lonicerae, Flos Lonicerae, two precious flowers are dry flower or the first flower of opening of band of this plant of wooden Teng of the perennial half long green prehensile of Caprifoliaceae Radix Ophiopogonis, Flos Lonicerae, Flos Lonicerae or hair style Radix Ophiopogonis; The property sweet, cold; Contain volatile oil in spending, be mainly fragrant Camphor tree alcohol, eugenol, carvacrol, contain chlorogenic acid, isochlorogenic acid, ginkgolic acid, luteolin etc. again.Wherein chlorogenic acid, isochlorogenic acid are the main antibiotic effective ingredients of Flos Lonicerae, and Flos Lonicerae extractive solution also has the effect of antiinflammatory, raising serum IgG antibody level in addition.
Herba Eupatorii, another name Herba Chlorophyti, water perfume (or spice), great zeeland, Dou Lianglan, blue, the Rhizoma et radix valerianae of woman are the stem and leaf of feverfew Herba Chlorophyti; Herb contains volatile oil, be mainly P-cymene, neryl acetate, thymol methyl ether, leaf contains the effect that coumarin, o-coumaric acid, thymohydroquinone, stigmasterol, Palmic acid, taraxasterol, Fumaric acid, succinic acid, mannitol etc. have antibiotic and resisiting influenza virus.
Herba Artemisiae Scopariae, another name is the tender Seedling of feverfew Herba Artemisiae Scopariae or Artemisia scoparia because of dirt, horse elder generation, Herba Artemisiae Scopariae, spire Herba Artemisiae Annuae, smelly Artemisia, grandmother Artemisia; Herb contains escoparone, because of dirt Artemisia flavone, capillarisin, also have the derivant, chlorogenic acid of Quercetin, isorhamnetin and multiple capillarisin etc., have effects such as resisting pathogenic microbes, antitumor.
Radix Bupleuri, the another name Asia puecon recklessly, the Artemisia of smoking, rue, mountain dish, mushroom grass, faggot, HERBA BUPLEURI, root for umbelliferae bupleurum, Radix Bupeuri Scorzonerfolii. etc., mainly contain volatile oil in the root, valeric acid, caproic acid, enanthic acid, eugenol acetic acid Rhizoma et radix valerianae aldehydo-ester, limonene, contain saikoside, polysaccharide etc. again, wherein saikoside or Radix Bupleuri volatile oil have antiinflammatory action.The Radix Bupleuri water decoction is in external effect with resisting pathogenic microbes, and injection can suppress epidemic haemorrhagic fever virus.
Herba Taraxaci, the public dish of another name wild duck, Pu Gongcao, Herba Violae, grandmother's fourth, Herba crotalariae albidae, Pu Gongding, milk grass, Gu Guding are the herb of feverfew Herba Taraxaci, alkali ground Herba Taraxaci, different luxuriant Herba Taraxaci etc.; Herb contains inositol, agedoite amaroid, Saponin, and root contains multiple triterpene alcohol as taraxasterol, taraxerol, taraxacin and caffeic acid; Have resisting pathogenic microbes, effect such as antitumor.
Radix Isatidis is called indigo-blue, Isatis indigotica Fort (Indigofera tinctoria L, Baphicanthus cusia (nees) Brem. Polygonum tinctorium Ait) root, indigo root, is the root of cruciferae isatis, contains indigo, indirubin, indigo glycosides, sinigrin and several amino acids in the root, have resisting pathogenic microbes, anticancer, regulate effect such as immunity.
Folium Isatidis is the leaf of cruciferae isatis, contains indigo, Isatis indigotica Fort. glycosides, indirubin, the hydrolysis of Isatis indigotica Fort. glycosides in the leaf and can be changed into indigo and the furyl xylose keto acid, has resisting pathogenic microbes, antiendotoxic effect.
The 20 WS of existing Rhizoma Belamcandae antiviral injection technology visible ministry standard Chinese traditional patent formulation preparation
3-B-3952-98[method for making] described in content; Described Rhizoma Belamcandae antiviral injection is that above component obtains volatile oil component through distillation extraction, obtaining water soluble ingredient again after water is carried forms, be yellowish-brown or filemot clear liquid, antiviral and antibacterial and anti-inflammation functions are arranged, also can be used the early stage disease of treatment epidemic hemorrhagic fever with other drug.Be used for intramuscular injection.Because of being pure Chinese medicinal preparation, be prone to medicinal liquid muddiness, precipitation, metachromatism in the preservation, influence product quality, effect duration only is 2 years.
The present invention is directed to the phenomenons such as easy appearance precipitation variable color of Rhizoma Belamcandae antiviral injection in put procedure in original technology,, obtain better Rhizoma Belamcandae antiviral injection of stability through further technical finesse.
Because the existing route of administration of Rhizoma Belamcandae antiviral injection is intramuscular injection, use inconvenience clinically, patient's medicine-feeding part pain causes untoward reaction such as congestion even muscular death easily.
The Rhizoma Belamcandae antiviral injection that obtains by the bright technology of this law can be applicable to intravenously administrable, by intravenous drip or intravenous injection administration, the bioavailability height, easy to use, untoward reaction is few, comprising direct intravenous injection, infusion medium comprises glucose injection, sodium chloride injection injection etc., is different from traditional similar injection.
Summary of the invention
The object of the present invention is to provide a kind of Chinese medicine.
Another object of the present invention is to provide a kind of preparation method of Chinese medicine.
A further object of the present invention is to provide a kind of intravenously administrable Rhizoma Belamcandae antiviral injection of Rhizoma Belamcandae antiviral injection.
The present invention relates to a kind of Rhizoma Belamcandae antiviral injection, its preparation method and intravenously administrable approach thereof, belong to field of traditional Chinese.Its crude drug comprises Rhizoma Belamcandae, Flos Lonicerae, Herba Eupatorii, Herba Artemisiae Scopariae, Radix Bupleuri, Herba Taraxaci, Radix Isatidis, Folium Isatidis, wherein Rhizoma Belamcandae is 1～1000 weight portion, Flos Lonicerae is 1～1000 weight portion, Herba Eupatorii is 1～1000 weight portion, Herba Artemisiae Scopariae is 1～1000 weight portion, Radix Bupleuri is 1～1000 weight portion, Herba Taraxaci is 1～1000 weight portion, Radix Isatidis is 1～1000 weight portion, Folium Isatidis is 1～1000 weight portion, the present invention is by the crude drug vapor distillation in will writing out a prescription, decocting in water, add clarifier, precipitate with ethanol, water precipitating, centrifugal, ultrafiltration multiple technologies means obtain the effective active composition of each component of Rhizoma Belamcandae antiviral injection, through packing, sterilization obtains finished product preparation.Injection of the present invention has antiviral and antibacterial and anti-inflammation functions, also can be used the early stage disease of treatment epidemic hemorrhagic fever with other drug.Because preparation process adopted the multiple technologies means that medicinal liquid is handled, phenomenons such as the medicinal liquid muddiness that resulting preparation has been avoided occurring in the Chinese medicine injection storage process effectively, precipitation, variable color prolong keeping life.Can pass through the intravenous route administration by technology of the present invention, the bioavailability height, easy to use, untoward reaction is few, avoids using clinically inconvenience, and patient's medicine-feeding part pain causes untoward reaction such as congestion even muscular death easily.
The object of the invention can be achieved in the following manner:
Raw medicinal material and prescription: Rhizoma Belamcandae, Flos Lonicerae, Herba Eupatorii, Herba Artemisiae Scopariae, Radix Bupleuri, Herba Taraxaci, Radix Isatidis, Folium Isatidis are respectively the 1-1000 weight portion, described weight portion can be conventional units such as mg, g, kg, jin, two, money, and its preparation method comprises the steps:
(1) water of 3-6 times of weight of adding raw medicinal material weight is collected distillate with steam distillation, and distillate is carried out redistillation, and it is standby to get smart slide liquid;
(2) the water boiling that adds 4～6 times of medical material weight of the medicinal residues after will distilling decocts 2 times at least, and each 1-2 hour, filter, merge filtrate twice, filtrate concentrates,
(3) in concentrated solution, add 0.03%～0.06% clarifier of concentrated solution weight, be heated to 70～90 ℃, after leaving standstill, add 0.015%～0.03% clarifier of concentrated solution weight again, leave standstill, centrifugal, get supernatant concentration;
(4) slowly stir adding ethanol down, add ethanol precipitation, the cold preservation after-filtration, filtrate recycling ethanol, and concentrate, add ethanol again, cold preservation after-filtration, filtrate recycling ethanol and concentrated filtrate;
(5) add the water for injection of concentrated solution 1-3 times weight, the cold preservation after-filtration, filtrate is regulated PH to 5.0-7.0 with the 10-20% sodium hydroxide solution, the active carbon of adding 1% boils, and filters, add the above-mentioned smart liquid that slips in the filtrate, mix homogeneously, heating, put cold back cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection, filters, fill is sterilized, is packed in ampoule.
Collecting distillate behind the vapor distillation in the above-mentioned steps is 1/6～1/4 of medical material amount, and distillate is carried out must being about 1/8～1/6 of medical material weight by smart slide liquid behind the redistillation.
After for the first time adding clarifier, leave standstill 2 hours after, left standstill 4 hours for the second time.
Supernatant concentration to the every ml medicinal liquid that adds behind the clarifier contains crude drug amount 3～4g.
Adding for the first time ethanol makes and contains the alcohol amount and be 70-75%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, be concentrated into every ml medicinal liquid behind the filtrate recycling ethanol and contain crude drug amount 3～4g, add for the second time ethanol and make and contain the alcohol amount and be 80-85%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 6～8g.
After adding the water for injection of 1-3 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, if desired, add 1% active carbon behind the filtrate adjusting PH, boiled 30 minutes, filter paper filtering adds the above-mentioned smart liquid that slips, mix homogeneously in the filtrate, 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal, get the supernatant ultrafiltration, add water for injection, filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
By foregoing description as can be seen, the said water precipitating of the present invention is for adding water for injection in the concentrated filtrate that obtains after precipitate with ethanol reclaims ethanol.
The particle of clarifier in the above-mentioned preparation method for only removing granularity the greater in the extract that anhydrates and having precipitation trend, can keep effective polymer substance, thereby improve the clarifier of the stability of medicinal liquid, include but not limited to can be used in the prior art the various clarifiers of Chinese medicine, as commercially available 101 fruit juice clarifiers, chitin kind absorptive clarificant, the clarification of ZTC natural clarifying agent and clarifier B, clarifier A etc.
More particularly, the preparation method of Rhizoma Belamcandae antiviral injection of the present invention is: according to above-mentioned medical material formulated raw medicinal material, the purified water that adds 3-6 times of weight of medical material weight is 1/6～1/4 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/8～1/6 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 4～6 times of medical material weight decocts 2 times, and each 1-2 hour, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.03%～0.06% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.015%～0.03% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 3～4g; Slowly stir and add ethanol down, add ethanol and make and contain the alcohol amount and be 70-75%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 3～4g, add ethanol, make the alcohol amount of containing be 80-85%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 6～8g; The water for injection that adds concentrated solution 1-3 times weight, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 5.0-7.0 with the 10-20% sodium hydroxide solution, the active carbon of adding 1% boiled filter paper filtering 30 minutes, add the above-mentioned smart liquid that slips in the filtrate, mix homogeneously was 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection, filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
The resulting product specification is that 2ml/ props up, 5ml/ props up, 10ml/ props up, 20ml/ props up, and preferred 2ml/ props up, 5ml/ props up, 10ml/ props up, and every ml contains chlorogenic acid (C
16H
18O
9) for being no less than 0.5mg, preferred every ml contains chlorogenic acid (C
16H
18O
9) be 0.5～20mg.
In the preparation process, clarifier is for being purchased, and for making technology, constant product quality, clarifier B, clarifier A are provided by fixing manufacturer.Above-mentioned clarifier became the clarification technique company limited in positive day available from Tianjin, and model has two kinds, is denoted as clarifier A, clarifier B.
Injection of the present invention adopts intravenous mode when using, the bioavailability height, and easy to use, untoward reaction is few.Injection system can be: intramuscular injection, a 2ml～5ml, 3 times on the one; Intravenous drip, a 10ml～15ml once-a-day, joins in 250ml～500m15% glucose injection, 10% glucose injection or 0.9% sodium chloride injection and slowly instils, or follow the doctor's advice.
Injection of the present invention has following medicinal usage:
The respiratory tract infection of prophylactic treatment;
treats acute tonsillitis;
treats infectious disease;
treats parotitis;
treats epidemic encephalitis type B;
treats infant upper respiratory tract infection;
treats pharyngolaryngitis;
The early stage disease of treatment epidemic hemorrhagic fever.
Injection of the present invention has increased stability of formulation having under the prerequisite of good drug effect, has effectively avoided phenomenons such as degraded that traditional injection takes place in long term store, muddiness, precipitation, has prolonged the quality effect duration of Rhizoma Belamcandae antiviral drugs preparation; And be able to the intravenous route administration, the bioavailability height, easy to use, untoward reaction is few, avoids using clinically inconvenience, and patient's medicine-feeding part pain reduces and causes untoward reaction such as congestion even muscular death.
The specific embodiment
Embodiment 1
Get Rhizoma Belamcandae 500g, Flos Lonicerae 400g, Herba Eupatorii 300g, Herba Artemisiae Scopariae 200g, Radix Bupleuri 150g, Herba Taraxaci 250g, Radix Isatidis 400g, Folium Isatidis 300g, the purified water that adds 3 times of weight of medical material weight is 1/5 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/8 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 5 times of medical material weight decocts 2 times, and each 1 hour, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.06% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.03% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 4g; Slowly stir and add ethanol down, add ethanol and make that to contain the alcohol amount be 70%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 4g, add ethanol, make that to contain alcohol amount be 80%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 6g; The water for injection that adds 2.5 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 5.5 with 10% sodium hydroxide solution, adds 1% active carbon, boils 30 minutes, filter paper filtering adds the above-mentioned smart liquid that slips, mix homogeneously in the filtrate, 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection and makes every ml contain chlorogenic acid (C
16H
180
9) be 1.6mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
The resulting product specification is that 2ml/ props up, 5ml/ props up.
Embodiment 2
Get Rhizoma Belamcandae 50g, Flos Lonicerae 900g, Herba Eupatorii 100g, Herba Artemisiae Scopariae 300g, Radix Bupleuri 150g, Herba Taraxaci 250g, Radix Isatidis 100g, Folium Isatidis 200g, the purified water that adds 2 times of weight of medical material weight is 1/6 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/7 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 6 times of medical material weight decocts 2 times, and each 1 hour, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.04% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.02% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 3g; Slowly stir and add ethanol down, add ethanol and make that to contain the alcohol amount be 75%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 3g, add ethanol, make that to contain alcohol amount be 85%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 8g; The water for injection that adds 3 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 6.0 with 10% sodium hydroxide solution, adds 1% active carbon, boils 30 minutes, filter paper filtering adds the above-mentioned smart liquid that slips, mix homogeneously in the filtrate, 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection and makes every ml contain chlorogenic acid (C
16H
18O
9) be 10mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
The resulting product specification is that 2ml/ props up, 5ml/ props up.
Embodiment 3
Get Rhizoma Belamcandae 900g, Flos Lonicerae 100g, Herba Eupatorii 100g, Herba Artemisiae Scopariae 150g, Radix Bupleuri 300g, Herba Taraxaci 50g, Radix Isatidis 200g, Folium Isatidis 150g, the purified water that adds 6 times of weight of medical material weight is 1/4 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/6 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 4 times of medical material weight decocts 2 times, and each 1.5 hours, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.06% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.03% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 3.3g; Slowly stir and add ethanol down, add ethanol and make that to contain the alcohol amount be 70%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 3.3g, add ethanol, make that to contain alcohol amount be 80%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 6g; The water for injection that adds 2.5 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 6.5 with 10% sodium hydroxide solution, adds 1% active carbon, boils 30 minutes, filter paper filtering, add the above-mentioned smart liquid that slips in the filtrate, mix homogeneously adds water for injection 105 and makes every ml contain chlorogenic acid (C
16H
18O
9) be 2.4mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
The resulting product specification is that 2ml/ props up, 5ml/ props up.
Embodiment 4
Get Rhizoma Belamcandae 300g, Flos Lonicerae 300g, Herba Eupatorii 800g, Herba Artemisiae Scopariae 600g, Radix Bupleuri 50g, Herba Taraxaci 50g, Radix Isatidis 600g, Folium Isatidis 100g, the purified water that adds 5 times of weight of medical material weight is 1/4 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/7 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 8 times of medical material weight decocts 2 times, and each 1.5 hours, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.05% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.025% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 3.8g; Slowly stir and add ethanol down, add ethanol and make that to contain the alcohol amount be 75%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 3.8g, add ethanol, make that to contain alcohol amount be 85%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 6.5g; The water for injection that adds 1 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 6.7 with 10% sodium hydroxide solution, adds 1% active carbon, boils 30 minutes, filter paper filtering adds the above-mentioned smart liquid that slips, mix homogeneously in the filtrate, 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection and makes every ml contain chlorogenic acid (C
16H
18O
9) be 1.0mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
The resulting product specification is that 2ml/ props up, 5ml/ props up.
Embodiment 5
Get Rhizoma Belamcandae 200g, Flos Lonicerae 200g, Herba Eupatorii 300g, Herba Artemisiae Scopariae 200g, Radix Bupleuri 250g, Herba Taraxaci 350g, Radix Isatidis 500g, Folium Isatidis 400g, the purified water that adds 5 times of weight of medical material weight is 1/6 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/8 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 6 times of medical material weight decocts 2 times, and each 2 hours, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.06% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.03% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 4g; Slowly stir and add ethanol down, add ethanol and make that to contain the alcohol amount be 70%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 4g, add ethanol, make that to contain alcohol amount be 80%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 7g; The water for injection that adds 1.5 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 5.4 with 10% sodium hydroxide solution, adds 1% active carbon, boils 30 minutes, filter paper filtering adds the above-mentioned smart liquid that slips, mix homogeneously in the filtrate, 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection and makes every ml contain chlorogenic acid (C
16H
18O
9) be 0.8mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.The resulting product specification is that 2ml/ props up, 5ml/ props up.
Experimental example 1
This experimental example is the appearance character of injection embodiment 1 of the present invention, the inspection of pH value project, and check result is as follows:
PH value is checked: get this product, an appendix VIIG checks that pH value is 5.0-7.0, and is up to specification according to Chinese Pharmacopoeia version in 2000.
Clarity test: check according to Chinese Pharmacopoeia version standard test in 2000 rule of operation " injection " check general rule, up to specification.
Character: injection of the present invention is yellowish-brown or filemot clear liquid.
Experimental example 2
This experimental example is the toxicity test parameter:
√ heat-original determinating: in accordance with the law check (an appendix VIII of Chinese Pharmacopoeia version in 2000 A).Dosage is by the every kg injection of rabbit body weight this product 1ml, and conclusion is: this product is up to specification.
The √ undue toxicity: check according to two appendix XI of Chinese Pharmacopoeia version in 2000 C undue toxicity inspection technique, intravenously administrable, up to specification.
The √ long term toxicity is measured: indexs such as successive administration observation in three months routine blood test, liver function, kidney merit are all normal, and the main organs pathologic finding there is no unusually, toxic reaction do not occur.
Experimental example 3
This experimental example is the qualitative determination of injection embodiment 1 of the present invention.
Get this product 2ml and add strong ammonia solution accent pH value to 9～10, extract with n-butyl alcohol 2ml jolting, get 3 of n-butyl alcohol liquid, evaporate to dryness drips 1% paradime thylaminobenzaldehyde sulfuric acid solution 1ml, puts and heats 1～2 minute in the water-bath, and solution shows sepia or bronzing.
Get this product 2ml, put evaporate to dryness in the water-bath, residue dissolves with methanol 2ml, as need testing solution. do not get the chlorogenic acid reference substance, add methanol and make the solution that every 1ml contains 1mg, product solution in contrast. according to thin layer chromatography SOP test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-acetone-formic acid (3:2:1) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the reference substance chromatograph on the corresponding position, show the speckle of same color.
Get this product 10ml, extract 2 times, each 5ml with the ethyl acetate jolting, merge ethyl acetate liquid, evaporate to dryness adds methanol 1ml dissolving, as need testing solution. other gets Herba Artemisiae Scopariae control medicinal material 1.5g, adds water 30ml, refluxes 1 hour, filter, filtrate is extracted 2 times with the ethyl acetate jolting, and each 15ml merges ethyl acetate liquid, evaporate to dryness, residue dissolves with methanol 1ml, in contrast medical material solution. according to the thin layer chromatography test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with toluene-Ethyl formate-formic acid (6:4:1) is developing solvent, launches, and takes out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color; Spray dinitro phenylhydrazine ethanol test solution again, hot blast blew 5～10 minutes, put under the daylight respectively and ultra-violet lamp (365nm) under inspect.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, the speckle of apparent same color under the daylight, the fluorescence speckle of apparent same color under the ultra-violet lamp.
Protein is got this product 1ml, adds 30% sulfosalicylic acid test solution 1ml of new preparation, mixes, and places 5 minutes, muddiness must not occur.
Oxalates is got this product 2ml, adds 2～3 of 3% calcium chloride solutions, places 10 minutes, muddiness or precipitation must not occur.
Tannin is got this product 1ml, adds the normal saline 5ml that contains 1% Ovum Gallus domesticus album of new preparation, places 10 minutes, muddiness or precipitation must not occur
Potassium ion is got this product 2ml, and evaporate to dryness burns to carbonization with little heated earlier, 500～600 ℃ of blazing ashing extremely fully, adds spirit of vinegar and makes dissolving again.Put in the 25ml measuring bottle, thin up is to scale, and mixing is as need testing solution.Get two of 10ml nessler colorimetric tubes, accurate adding standard potassium ion solution 0.8ml in the first pipe, add alkaline formaldehyde solution and (get formalin, with 0.1mol/L sodium hydroxide solution adjust pH to 8.0～9.0) 12 droplets, 2 of 3% editic acid sodium solutions, 3% sodium tetraphenylborate solution 0.5ml, thin up becomes 10ml, the accurate need testing solution 1ml that adds in the second pipe with the operation in accordance with the law simultaneously of first pipe, shakes up, first, second two pipes are with putting on the black paper, from up to down have an X-rayed, turbidity that shows in the second pipe and first pipe relatively must not be denseer.
The preparation of standard potassium ion solution: it is an amount of to get potassium sulfate, and porphyrize is dried to constant weight in 110 ℃, and precision takes by weighing 2.330g, puts in the 1000ml measuring bottle, adds water and makes dissolving in right amount and be diluted to scale, shakes up, as stock solution.Before facing usefulness, precision is measured stock solution 10ml, puts in the 100ml measuring bottle, and thin up shakes up to scale, promptly gets (K that every 1ml is equivalent to 100 μ g)
Resin is got this product 5ml, adds 1 of hydrochloric acid, places 30 minutes, should not have floccule and separates out.
The inspection conformance with standard regulation of injection of the present invention to begin a project.
Experimental example 4
This experimental example is the quantitative assay of injection embodiment 1 of the present invention.
The preparation precision of reference substance solution takes by weighing chlorogenic acid reference substance 8mg, puts in the 50ml measuring bottle, adds the dissolving of water slight fever, is cooled to room temperature, thin up shakes up to scale, and precision is measured 2ml, puts in the 10ml measuring bottle, add water to scale, shake up, promptly get (every 1ml contains chlorogenic acid 32 μ g)
The preparation precision of need testing solution is got this product 1ml, add 5 of water 4ml, 5% sodium hydroxide solutions, shake up, extract 3 times, each 4ml with the ethyl acetate jolting, discard ethyl acetate liquid, add 5 of dilute hydrochloric acid, shake up, extract 5 times with the ethyl acetate jolting, each 4ml (or being extracted into ethyl acetate layer apparent blue-fluorescence under the 365nm ultra-violet lamp), merge ethyl acetate extraction liquid, evaporate to dryness, the water dissolved residue also is transferred in the 25ml measuring bottle, wash evaporating dish with water for several times, washing liquid is incorporated in the measuring bottle, puts coldly, adds water to scale, shake up, promptly.
The algoscopy precision is measured reference substance solution and each 5ml of need testing solution, puts respectively in the 10ml measuring bottle, adds 5% sodium nitrite solution 0.3ml, shake up, placed 6 minutes, add 10% aluminum nitrate solution 0.3ml, shake up, placed 6 minutes, add 5% sodium hydroxide solution 4ml, be diluted with water to scale, shake up, placed 30 minutes, according to spectrophotography, measure trap at the wavelength place of 445nm and 515nm respectively, do blank assay simultaneously.Calculate chlorogenic acid contents according to the trap difference, promptly.
By three batches of mensuration, ml contains chlorogenic acid (C as a result
16H
18O
9) all be no less than 0.5mg.
After 10 days, clarity is good, content results is stable, pH value is stable, illustrates that injection of the present invention is to light, thermally-stabilised through 4500LX illumination 10 days, 60 ℃ of heating for injection of the present invention.
Conclusion: injection of the present invention meets the injection prescription, does not have any toxic action, uses human body safety, and the preparation stability test result is good.
Comparative example 1
The Rhizoma Belamcandae antiviral injection quality standard that this comparative example explanation injection quality standard content of the present invention and common process are produced has relatively increased new project, more meets intravenous requirement, has improved quality standard.
| Project | Rhizoma Belamcandae antiviral injection quality standard of the present invention | Common process Rhizoma Belamcandae antiviral injection quality standard |
| Check | PH value: should be 5.0～7.0. | PH value: should be 5.0～7.0. |
| Protein: get this product 1ml, add 30% sulfosalicylic acid test solution 1ml of new preparation, mix, placed 5 minutes, muddiness must not occur. | ||
| Oxalates: get this product 2ml, add 2～3 of 3% calcium chloride solutions, placed 10 minutes, muddiness or precipitation must not occur. | ||
| Tannin: get this product 1ml, add the normal saline 5ml that contains 1% Ovum Gallus domesticus album of new preparation, placed 10 minutes, muddiness or precipitation must not occur. | ||
| Potassium ion: get this product 2ml, evaporate to dryness burns to carbonization with little heated earlier, 500～600 ℃ of blazing ashing extremely fully, adds spirit of vinegar and makes molten again |
| Separate.Put in the 25ml measuring bottle, thin up is to scale, and mixing is as need testing solution.Get two of 10ml nessler colorimetric tubes, accurate adding standard potassium ion solution 0.8ml in the first pipe, add alkaline formaldehyde solution and (get formalin, transfer pH value to 8.0～9.0 with the 0.1mol/L sodium hydroxide solution) 12 droplets, 2 of 3% editic acid sodium solutions, 3% sodium tetraphenylborate solution 0.5ml, thin up becomes 10ml, the accurate need testing solution 1ml that adds in the second pipe with the operation in accordance with the law simultaneously of first pipe, shakes up, first, second two pipes are with putting on the black paper, from up to down have an X-rayed, turbidity that shows in the second pipe and first pipe relatively must not be denseer. | ||
| Resin: get this product 5ml, add 1 of hydrochloric acid, placed 30 minutes, should not have floccule and separate out. | ||
| Pyrogen: get this product, check (an appendix X of Chinese Pharmacopoeia version in 2000 III A) in accordance with the law, dosage is slowly injected 1ml by the every 1Kg of rabbit body weight, should be up to specification. | ||
| The undue toxicity: get this product, check in accordance with the law and (two appendix XI of Chinese Pharmacopoeia version in 2000 C) press intravenous administration, should be up to specification. |
Comparative example 2
Result's comparison that the Rhizoma Belamcandae antiviral injection of this comparative example explanation explained hereafter of the present invention and the Rhizoma Belamcandae antiviral injection of common process production detect with the quality standard of intravenously administrable, the Rhizoma Belamcandae antiviral injection of common process production can not be used for intravenous injection.
| Project | The requirement of Rhizoma Belamcandae antiviral injection (intravenous injection) quality standard | The Rhizoma Belamcandae antiviral injection of explained hereafter of the present invention | The Rhizoma Belamcandae antiviral injection that common process is produced |
| PH value | Get this product, check that according to an appendix VII of Chinese Pharmacopoeia version in 2000 G pH value is 5.0-6.0, and is up to specification. | (5.8 up to specification) | (5.9 up to specification) |
| Protein | Get this product 1ml, add 30% sulfosalicylic acid test solution 1ml of new preparation, mix, placed 5 minutes, muddiness must not occur.An appendix IX of Chinese Pharmacopoeia version in 2000 S " injection related substance inspection technique " | Up to specification | Up to specification |
| Oxalates | Get this product 2ml, add 2～3 of 3% calcium chloride test solutions, placed 10 minutes, muddiness or precipitation must not occur.An appendix IX of Chinese Pharmacopoeia version in 2000 S " injection related substance inspection technique " | Up to specification | Against regulation |
| Tannin | Get this product 1ml, add the normal saline 5ml that contains 1% Ovum Gallus domesticus album of new preparation, placed 10 minutes, muddiness or precipitation must not occur.An appendix IX of Chinese Pharmacopoeia version in 2000 S " injection related substance inspection technique " | Up to specification | Against regulation |
| Potassium ion | Get this product 1ml, evaporate to dryness burns to carbonization with little heated earlier, 500～600 ℃ of blazing ashing extremely fully, adds spirit of vinegar and makes dissolving again.Put in the 25ml measuring bottle, thin up is to scale, and mixing is as need testing solution.Get two of 10ml nessler colorimetric tubes, accurate adding standard potassium ion solution 0.8ml in the first pipe adds alkaline formaldehyde solution (getting formalin, with 0.1mol/L sodium hydroxide solution adjust pH to 8.0～9.0) 12 | Up to specification | Against regulation |
| Drip, 2 of 3% editic acid sodium solutions, 3% sodium tetraphenylborate solution 0.5ml, thin up becomes 10ml, the accurate need testing solution 1ml that adds in the second pipe, with the operation in accordance with the law simultaneously of first pipe, shake up, first, second two pipes are from up to down had an X-rayed with putting on the black paper, turbidity that shows in the second pipe and first pipe relatively must not be denseer.The preparation of standard potassium ion solution: it is an amount of to get potassium sulfate, and porphyrize is dried to constant weight in 110 ℃, and precision takes by weighing 2.330g, puts in the 1000ml measuring bottle, adds water and makes dissolving in right amount and be diluted to scale, shakes up, as stock solution.Before facing usefulness, precision is measured stock solution 10ml, puts in the 100ml measuring bottle, and thin up shakes up to scale, promptly gets an appendix IX of (K that every ml is equivalent to 100 μ g) Chinese Pharmacopoeia version in 2000 S " injection related substance inspection technique " | |||
| Resin | Get this product 5ml, add 1 of hydrochloric acid, placed 30 minutes, should not have floccule and separate out.Appendix IXS of Chinese Pharmacopoeia version in 2000 " injection related substance inspection technique " | Up to specification | Against regulation |
| Pyrogen | Foundation: Chinese Pharmacopoeia version in 2000 appendix XIII A " pyrogen test " | Up to specification | Against regulation |
| The undue toxicity | Foundation: Chinese Pharmacopoeia version in 2000 two appendix XI C " undue toxicity's inspection technique " | Up to specification | Up to specification |
Comparative example 3
The Rhizoma Belamcandae antiviral injection clarity that the explanation of this comparative example is produced with process using clarification technique of the present invention, water precipitating cold preservation, charcoal treatment, centrifugation technique processing is better than producing with conventional compound method.
| Adopt technology of the present invention | Adopt common process | |
| Method for making | Get Rhizoma Belamcandae 500g, Flos Lonicerae 400g, Herba Eupatorii 300g, Herba Artemisiae Scopariae 200g, Radix Bupleuri 150g, Herba Taraxaci 250g, Radix Isatidis 400g, Folium Isatidis 300g, the purified water that adds 3 times of weight of medical material weight is 1/5 of a medical material amount with steam distillation collection distillate, distillate is carried out redistillation, get smart slide liquid and be about 1/8 of medical material weight, standby; The purified water boiling that medicinal residues after the distillation is added 5 times of medical material weight decocts 2 times, and each 1 hour, filter paper filtering, merge filtrate twice, filtrate concentrates, and 0.06% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.03% the clarifier A that adds concentrated solution weight again, leave standstill 4 hours after, centrifugal, supernatant inclines and, and is concentrated into every ml medicinal liquid and contains crude drug amount 4g; Slowly stir and add ethanol down, add ethanol and make that to contain the alcohol amount be 70%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, and be concentrated into every ml medicinal liquid and contain crude drug amount 4g, add ethanol, make that to contain alcohol amount be 80%, 4-8 ℃ of cold preservation 48 hours, filter paper filtering, filtrate recycling ethanol, concentrated filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 6g; The water for injection that adds 2.5 times of weight of concentrated solution, 4-8 ℃ of cold preservation 24 hours, filter paper filtering, filtrate is regulated PH to 5.5 with 10% sodium hydroxide solution, adds 1% active carbon, | Get Rhizoma Belamcandae 500g, Flos Lonicerae 400g, Herba Eupatorii 300g, Herba Artemisiae Scopariae 200g, Radix Bupleuri 150g, Herba Taraxaci 250g, Radix Isatidis 400g, Folium Isatidis 300g, more than eight the flavor, extract with vapor distillation, collect distillate 500ml, distillate is redistillation again, it is standby to get rectification liquid 300ml, and extracting solution filters, and is standby; Medicinal residues decoct with water 2 times again, each 1 hour, filter, and merge with said extracted liquid, be concentrated into about 500ml, add ethanol and make and contain alcohol and measure and reach 75%, cold preservation was placed more than 24 hours, filtered filtrate recycling ethanol, add ethanol again and reach 85% to containing the alcohol amount, cold preservation was placed more than 24 hours, filtered, (about 400ml) merges with above-mentioned rectification liquid behind the filtrate recycling ethanol, and mixing was 105 ℃ of heating 45 minutes, put coldly, place more than 24 hours in 0～4 ℃ |
| Boiled 30 minutes, filter paper filtering adds the above-mentioned smart liquid that slips in the filtrate, mix homogeneously, 105 ℃ of heating 45 minutes, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection and makes every ml contain chlorogenic acid (C 16H 18O 9) be 1.6mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.The resulting product specification is that 2ml/ props up. | Filter, add the injection water, regulate pH value to 5.0～7.0, filter to 1000ml, embedding, sterilization, promptly. | |
| Clarity | 4 have small particles in 200. | 15 have white point, white piece, 3 deposited phenomenon to occur in 200. |
Comparative example 4
Zest was little when the explanation of this comparative example was used clinically with Rhizoma Belamcandae antiviral injection of the present invention, and untoward reaction is few.
| Nomenclature of drug | Rhizoma Belamcandae antiviral injection of the present invention | Common process Rhizoma Belamcandae antiviral injection |
| Usage and dosage | Intramuscular injection, a 2ml～5ml, 3 times on the one; Intravenous drip, a 10ml～15ml once-a-day, joins in 250ml～500ml 5% glucose injection, 10 % glucose injections or 0.9% sodium chloride injection and slowly instils.Or follow the doctor's advice. | Intramuscular injection, a 2ml～5ml, 3 times on the one; |
| Clinical use | Treat 82 routine viral influenza patients | Treat 90 routine viral influenza patients |
| Beneficial effect | 90% patient cured in 4 days | 86% patient cured in 7 days |
| Untoward reaction is observed | Phenomenons such as no itch all over, uncomfortable in chest, weak, erythra, cardiopalmus. | The 3 examples phenomenon of itching is arranged |
| Zest is observed | 3 examples have the pain phenomenon | 8 examples have the pain phenomenon, and there is constriction 5 routine injection sites |
Comparative example 5
This comparative example explanation Rhizoma Belamcandae antiviral injection of the present invention and common process Rhizoma Belamcandae antiviral injection compare by the stability of acceleration in 6 months
| Rhizoma Belamcandae antiviral injection of the present invention | Common process Rhizoma Belamcandae antiviral injection | |
| Standard code | Chlorogenic acid content must not be less than the 0.5mg clarity: qualification rate is greater than 95% pH value: 5.0～7.0 | Chlorogenic acid content must not be less than the 0.5mg clarity: qualification rate is greater than 95% pH value: 5.0～7.0 |
| 0 month | Chlorogenic acid content: 1.2mg clarity: qualification rate 99% pH value: 5.8 | Chlorogenic acid content: 0.9mg clarity: qualification rate 99% pH value: 5.9 |
| 1 month | Chlorogenic acid content: 1.2mg clarity: qualification rate 99% pH value: 5.8 | Chlorogenic acid content: 0.9mg clarity: qualification rate 98% pH value: 5.8 |
| 2 months | Chlorogenic acid content: 1.2mg clarity: qualification rate 99% pH value: 5.8 | Chlorogenic acid content: 0.8mg clarity: qualification rate 97% pH value: 5.6 |
| 3 months | Chlorogenic acid content: 1.2mg clarity: qualification rate 99% pH value: 5.8 | Chlorogenic acid content: 0.7mg clarity: qualification rate 96% pH value: 5.5 |
| 6 months | Chlorogenic acid content: 1.2mg clarity: qualification rate 99% pH value: 5.8 | Chlorogenic acid content: 0.6mg clarity: qualification rate 95% pH value: 5.4 |
Show that by above data the quality stability of Rhizoma Belamcandae antiviral injection of the present invention is better than common process Rhizoma Belamcandae antiviral injection.
Claims (8)
1, a kind of Rhizoma Belamcandae antiviral injection is characterized in that, is prepared by following method:
(1) water of 3-6 times of weight of adding raw medicinal material weight is collected distillate with steam distillation, and distillate is carried out redistillation, and it is standby to get smart slide liquid;
(2) the water boiling that adds 4～6 times of medical material weight of the medicinal residues after will distilling decocts 2 times at least, and each 1-2 hour, filter, merge filtrate twice, filtrate concentrates,
(3) in concentrated solution, add 0.03%～0.06% clarifier of concentrated solution weight, be heated to 70～90 ℃, after leaving standstill, add 0.015%～0.03% clarifier of concentrated solution weight again, leave standstill, centrifugal, get supernatant concentration;
(4) slowly stir adding ethanol down, add ethanol precipitation, the cold preservation after-filtration, filtrate recycling ethanol, and concentrate, add ethanol again, cold preservation after-filtration, filtrate recycling ethanol and concentrated filtrate;
(5) add the water for injection of concentrated solution 1-3 times weight, the cold preservation after-filtration, filtrate is regulated PH to 5.0-7.0 with the 10-20% sodium hydroxide solution, filter, add the above-mentioned smart liquid that slips in the filtrate, mix homogeneously, cold back cold preservation 24 hours is put in heating, and is centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection, filters, fill is sterilized, is packed in ampoule;
Wherein raw medicinal material and prescription: Rhizoma Belamcandae, Flos Lonicerae, Herba Eupatorii, Herba Artemisiae Scopariae, Radix Bupleuri, Herba Taraxaci, Radix Isatidis, Folium Isatidis are respectively the 1-1000 weight portion.
2, injection according to claim 1 is characterized in that the every ml of described Rhizoma Belamcandae antiviral injection contains chlorogenic acid (C
16H
18O
9) be no less than 0.5mg.
3, a kind of preparation method of Rhizoma Belamcandae antiviral injection is characterized in that, comprises the steps:
(1) water of 3-6 times of weight of adding raw medicinal material weight is collected distillate with steam distillation, and distillate is carried out redistillation, and it is standby to get smart slide liquid;
(2) the water boiling that adds 4～6 times of medical material weight of the medicinal residues after will distilling decocts 2 times at least, and each 1-2 hour, filter, merge filtrate twice, filtrate concentrates,
(3) in concentrated solution, add 0.03%～0.06% clarifier of concentrated solution weight, be heated to 70～90 ℃, after leaving standstill, add 0.015%～0.03% clarifier of concentrated solution weight again, leave standstill, centrifugal, get supernatant concentration;
(4) slowly stir adding ethanol down, add ethanol precipitation, the cold preservation after-filtration, filtrate recycling ethanol, and concentrate, add ethanol again, cold preservation after-filtration, filtrate recycling ethanol and concentrated filtrate;
(5) add the water for injection of concentrated solution 1-3 times weight, the cold preservation after-filtration, filtrate is regulated PH to 5.0-7.0 with the 10-20% sodium hydroxide solution, filter, add the above-mentioned smart liquid that slips in the filtrate, mix homogeneously, cold back cold preservation 24 hours is put in heating, and is centrifugal with centrifuge, get supernatant, ultrafiltration adds water for injection, filters, fill is sterilized, is packed in ampoule.
4, preparation method according to claim 3 is characterized in that in the step (5), also be included in regulate PH after, add 1% active carbon, boil after-filtration.
5, preparation method according to claim 3, it is characterized in that collecting distillate is 1/6～1/4 of medical material amount; Collecting accurate distillate is 1/8～1/6 of medical material amount; Behind the merging filtrate, and be concentrated into every ml medicinal liquid and contain crude drug amount 1～2g; Add and medicinal liquid is concentrated into every ml medicinal liquid before the ethanol and contains crude drug amount 3～4g; Before the water precipitating, filtrate is concentrated into every ml medicinal liquid and contains crude drug amount 6～8g; Centrifugal with centrifuge behind extracting solution and the smart slide liquid mix homogeneously, revolution is 3000～4000 rev/mins; Ultrafiltration is the ultrafiltration post of molecular cut off 100,000.
6, preparation method according to claim 3 is characterized in that fill adds water for injection and contains chlorogenic acid (C to every ml before ampoule
16H
18O
9) be no less than 0.5mg.
7, preparation method according to claim 3 is characterized in that the filtering with microporous membrane of the medical filtration of fill before ampoule with 0.22 μ m.
8, preparation method according to claim 3 is characterized in that sterilizing 30 minutes under 100 ℃ of conditions after the canned end.
9, claim 1 or 2 described intravenously administrable Rhizoma Belamcandae antiviral injections.
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| CN200410008774.5 | 2004-03-18 | ||
| CNB2005100553693A CN100490875C (en) | 2004-03-18 | 2005-03-18 | Blackberrylily rhizome antiviral injection, preparation and venous medicine feeding blackberrylily rhizome antiviral injection thereof |
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| CN109549993A (en) * | 2018-12-29 | 2019-04-02 | 西安高科陕西金方药业公司 | Rectum or nebulizer administration blackberry lily anti-virus formulation and preparation and purposes |
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| Title |
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| 中华人民共和国卫生部药品标准第二十册. 国家药典委员会，265，266. 1998 |
| 中华人民共和国卫生部药品标准第二十册. 国家药典委员会，265，266. 1998 * |
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