CN1830465A - Clary injection and its preparation method - Google Patents
Clary injection and its preparation method Download PDFInfo
- Publication number
- CN1830465A CN1830465A CN 200510051488 CN200510051488A CN1830465A CN 1830465 A CN1830465 A CN 1830465A CN 200510051488 CN200510051488 CN 200510051488 CN 200510051488 A CN200510051488 A CN 200510051488A CN 1830465 A CN1830465 A CN 1830465A
- Authority
- CN
- China
- Prior art keywords
- water
- hours
- concentrated
- injection
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Medicinal Preparation (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
A Chinese medicine 'Xiangdan injection' for treating angina pectoris and myocardial infarction is prepared from red sage root and dalbergia wood through preparing the aromatic liquid by distilling dalbergia wood, preparing liquid extract of red sage root through depositing in alcohol and water, centrifugal separation and ultrafiltration, mixing them together, stirring, loading in containers and sterilizing.
Description
Invention field
The present invention relates to a kind of XIANGDAN ZHUSHEYE and preparation method thereof, belong to field of traditional Chinese.
Background technology
Radix Salviae Miltiorrhizae is the root of Labiatae salvia Radix Salviae Miltiorrhizae.Bitter in the mouth, cold nature.Blood circulation promoting and blood stasis dispelling, nourishing blood to tranquillize the mind, removing heat from blood eliminating carbuncle are arranged and arrange the function of dense granulation promoting, be divided into fat-soluble composition and water-soluble components two classes in the Main Ingredients and Appearance, fat-soluble composition is mainly: TANSHINONES, cryptotanshinone, tanshinol, Radix Salviae Miltiorrhizae quinone etc.Be mainly in the water-soluble components: danshensu, saivianic acid A, second, the third, protocatechualdehyde etc.Salvia-soluble composition obviously coronary artery dilator significantly increases coronary artery blood flow, promotes collateral circulation; Myocardial ischemia and myocardial infarction there is protective effect; Experiment shows that Radix Salviae Miltiorrhizae can make microcirculatory blood flow obviously increase; Effects such as Radix Salviae Miltiorrhizae also has resisting blood coagulation, increases myocardium anti-anoxia ability, antibiotic, calmness.
Lignum Dalbergiae Odoriferae is the root heartwood of leguminous plant Lignum Dalbergiae Odoriferae wingceltis and sissoo.Acrid in the mouth, warm in nature.Contain 2 '-O-methyl isoliquiritin unit, Radix Glycyrrhizae aglycon, isoliquiritin unit etc., Lignum Dalbergiae Odoriferae can significantly promote the recovery of the experimental microcirculation disturbance blood flow of small intestinal mesentery, and arteriole after shrinking recovery and the recovery of local microcirculation, arteriolar contraction is stronger due to its antiadrenergic drug.Lignum Dalbergiae Odoriferae also has the blood fat reducing effect, and some composition also has the effect of remarkable anticoagulant in the Lignum Dalbergiae Odoriferae.
XIANGDAN ZHUSHEYE is a pure Chinese medicinal preparation, is prone to medicinal liquid muddiness, precipitation, metachromatism in the preservation, influences product quality, and effect duration only is 2 years.
The present invention is directed to the phenomenons such as easy appearance precipitation variable color of XIANGDAN ZHUSHEYE in put procedure in original technology,, obtain better XIANGDAN ZHUSHEYE of stability through further technical finesse.
Summary of the invention
The object of the invention is to provide a kind of Chinese medicine.
The object of the invention is to provide a kind of preparation method of Chinese medicine.
The present invention relates to a kind of XIANGDAN ZHUSHEYE its preparation method, belong to field of traditional Chinese.Contain Radix Salviae Miltiorrhizae, Lignum Dalbergiae Odoriferae medical material, wherein Radix Salviae Miltiorrhizae is that 1～1000 weight portion, Lignum Dalbergiae Odoriferae are 1～1000 weight portion, the present invention handles respectively by the medical material in will writing out a prescription, the Lignum Dalbergiae Odoriferae vapor distillation, get Aromatic water, clarifier, precipitate with ethanol, water precipitating are carried, added to Radix Salviae Miltiorrhizae water, centrifugal, ultrafiltration multiple technologies means obtain Radix Salviae Miltiorrhizae extract, then with Aromatic water and Radix Salviae Miltiorrhizae extract mix homogeneously, obtain the XIANGDAN ZHUSHEYE active ingredient, through packing, sterilization, obtain finished product preparation, every ml contains protocatechualdehyde for being no less than 0.17mg.Injection of the present invention has blood vessel dilating, promotes the effect of coronary artery blood flow.Be used for angina pectoris, also can be used for myocardial infarction etc.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 make preparation stabilization, extension of validity.
Describe in detail
Goal of the invention of the present invention can be achieved in the following manner:
It is characterized in that the medical material Lignum Dalbergiae Odoriferae is collected Aromatic water with steam distillation, with the Radix Salviae Miltiorrhizae decocting in water, add clarifier, precipitate with ethanol, water precipitating, centrifugal, ultrafiltration comprises following process: the Lignum Dalbergiae Odoriferae of getting the 1-1000 weight portion, the purified water that adds 3-6 times of weight of medical material weight is 1/3～1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divide the layer that deoils, use filter paper filtering, get the Lignum Dalbergiae Odoriferae Aromatic water, standby; The purified water of 5～8 times of red rooted salvias is decocted 3 times, 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, adds 0.01%～0.5% active carbon, boils 30 minutes, filter paper filtering, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add an amount of water for injection, filter, fill was sterilized 15～30 minutes for 100～121 ℃ in ampoule.
The resulting product specification is that 2ml/ props up, 4ml/ props up, 5ml/ props up, 10ml/ props up, 15ml/ props up, 20ml/ props up, and preferred 2ml/ props up, 10ml/ props up, 20ml/ props up, and every ml contains protocatechualdehyde for being no less than 0.17mg, and it is 0.17～15mg that preferred every ml contains protocatechualdehyde; Intramuscular injection, a 2ml, 1～2 time on the one.Intravenous drip, a 10～20ml uses with 5～10% glucose injections, 250～500ml dilution back, or follows the doctor's advice.
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 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 pharmaceutical preparation.
The specific embodiment
Embodiment 1
Get Lignum Dalbergiae Odoriferae 1000g, the purified water that adds 3 times of weight of medical material weight is 1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divides the layer that deoils, and filter paper filtering gets the Lignum Dalbergiae Odoriferae Aromatic water, and is standby; The purified water that the 1000g red rooted salvia is added 8,6,6 times of medical material weight decocts 3 times, and 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter merging filtrate, 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 0.5% active carbon, boils 30 minutes, filter, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add water for injection and make every ml contain protocatechualdehyde to be 1.5mg, to filter, fill was sterilized 30 minutes for 100 ℃ in ampoule.
Embodiment 2
Get Lignum Dalbergiae Odoriferae 500g, the purified water that adds 5 times of weight of medical material weight is 1/3 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divides the layer that deoils, and filter paper filtering gets the Lignum Dalbergiae Odoriferae Aromatic water, and is standby; The purified water that the 800g red rooted salvia is added 8,5,5 times of medical material weight decocts 3 times, and 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter merging filtrate, 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 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 6.0 with 10% sodium hydroxide solution, adds 0.05% active carbon, boils 30 minutes, filter, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add water for injection and make every ml contain protocatechualdehyde to be 0.5mg, to filter, fill was sterilized 30 minutes for 108 ℃ in ampoule.
Embodiment 3
Get Lignum Dalbergiae Odoriferae 300g, the purified water that adds 4 times of weight of medical material weight is 1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divides the layer that deoils, and filter paper filtering gets the Lignum Dalbergiae Odoriferae Aromatic water, and is standby; The purified water that the 500g red rooted salvia is added 8,6,6 times of medical material weight decocts 3 times, and 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter merging filtrate, 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 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 6.0 with 10% sodium hydroxide solution, adds 0.1% active carbon, boils 30 minutes, filter, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add water for injection and make every ml contain protocatechualdehyde to be 0.8mg, to filter, fill was sterilized 15 minutes for 121 ℃ in ampoule.
Embodiment 4
Get Lignum Dalbergiae Odoriferae 1000g, the purified water that adds 3 times of weight of medical material weight is 1/3 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divides the layer that deoils, and filter paper filtering gets the Lignum Dalbergiae Odoriferae Aromatic water, and is standby; The purified water that the 700g red rooted salvia is added 6,6,6 times of medical material weight decocts 3 times, and 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter merging filtrate, 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 7.0 with 10% sodium hydroxide solution, adds 0.06% active carbon, boils 30 minutes, filter, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add water for injection and make every ml contain protocatechualdehyde to be 0.87mg, to filter, fill was sterilized 25 minutes for 110 ℃ in ampoule.
Embodiment 5
Get Lignum Dalbergiae Odoriferae 800g, the purified water that adds 5 times of weight of medical material weight is 1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divides the layer that deoils, and filter paper filtering gets the Lignum Dalbergiae Odoriferae Aromatic water, and is standby; The purified water that the 1000g red rooted salvia is added 8,5,6 times of medical material weight decocts 3 times, and 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter merging filtrate, filtrate concentrates, and 0.08% of adding concentrated solution weight clarifier B is heated to 70～90 ℃ in concentrated solution, after leaving standstill 2 hours, 0.04% 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 6.5 with 10% sodium hydroxide solution, adds 0.2% active carbon, boils 30 minutes, filter, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add water for injection and make every ml contain protocatechualdehyde to be 0.20mg, to filter, fill was sterilized 20 minutes for 115 ℃ in ampoule.
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: get this product, check that according to an appendix VII of Chinese Pharmacopoeia version in 2000 G pH value is 5.0-7.0, and is up to specification.
Clarity: 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 brown 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 0.5ml, 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, up to specification.
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 number droplet, put on the filter paper bar, after doing, be suspended on (not according to touching liquid level) in the hartshorn bottle, take out after 20 minutes, put ultra-violet lamp (365nm) under and observe, apparent light blue fluorescence.
Get this product 2ml, put in the separatory funnel, add petroleum ether (30～60 ℃) 10ml, jolting is extracted, and divides and gets petroleum ether layer, volatilizes, and residue adds 1～2 of 5% vanillin sulfuric acid solution, promptly shows brownish red, places back gradual change aubergine.
Get this product 4ml, put in the evaporating dish, evaporate to dryness in the water-bath, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.Other gets the protocatechualdehyde reference substance, adds dehydrated alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2000 B), draw each 2～5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate-formic acid (8: 5: 0.8) is developing solvent, launch, take out, dry, spray is with the mixed liquor of 2% liquor ferri trichloridi and 1% potassium ferricyanide solution (1: 1).In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Experimental example 4
This experimental example is the mensuration of injection embodiment 1 related item of the present invention.
Trap: get this product 1ml, thin up becomes 500ml, measures according to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2000 A), at the wavelength place of 281 ± 3nm absorption maximum is arranged, and it is up to specification that basic trap should be not less than 0.30. this product.
Haemolysis and agglutination test: get the rabbit cardiac blood, be equipped with in the container of bead, jolting number minute, removing fibronectin makes and becomes to take off fine blood, add normal saline, shake up, centrifugal, supernatant inclines, sedimentary erythrocyte reuse normal saline washing 3～4 times, apparent red to centrifugal back supernatant, press the gained erythrocyte volume, be diluted to 2% suspension with normal saline. get test sample 0.0,0.3,0.3ml put respectively in three test tubes, add normal saline 2.5 respectively, 2.2,2.2ml and above-mentioned red blood cell suspension 2.5ml, shake up, put rapidly in the calorstat, keep 36.5 ℃ ± 0.5 ℃ temperature, observed 3 hours, haemolysis and blood coagulation phenomenon must not be arranged. if cohesion is arranged, through jolting, condensation product should be able to homodisperse.
Residue on ignition: must not cross 1.0% (an appendix IX of Chinese Pharmacopoeia version in 2000 J).This product is up to specification.
Protein: get this product 1ml, add 1～3 of tannic acid test solution, muddiness must not occur.This product is up to specification.
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.This product is up to specification.
Heavy metal: get the residue of leaving under the residue on ignition item, check in accordance with the law and (2000 editions appendix IXE of Chinese Pharmacopoeia) must not cross 10/1000000ths.This product is up to specification.
Arsenic salt: get this product 2ml, check in accordance with the law and (2000 editions one appendix IX F of Chinese Pharmacopoeia) must not cross 5/1000000ths.This product is 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.This product is up to specification.
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 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 ml is equivalent to 100 μ g).
This product potassium ion is checked up to specification.
Resin: get this product 5ml, add chloroform 10ml jolting and extract, divide and get chloroform solution, put evaporate to dryness in the water-bath, residue adds acetic acid 2ml makes dissolving, puts in the tool plug test tube, adds water 3ml, and mixing was placed 30 minutes, should not have floccule and separated out.This product is up to specification.
Total solid: precision is measured this product 10ml, puts in the evaporating dish of constant weight, and behind evaporate to dryness in the water-bath, 105 ℃ of dryings 3 hours, cooling was 30 minutes in the dislocation exsiccator, claimed to decide weight rapidly.Leave over residue and must not be less than 0.5%.This product is up to specification.
Experimental example 5
This experimental example is the quantitative assay of injection embodiment 1 of the present invention.
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; With methanol-1% glacial acetic acid solution (8: 92) is mobile phase; The detection wavelength is 280nm.Number of theoretical plate is pressed the protocatechualdehyde peak and is calculated, and should be not less than 3000.
The preparation of reference substance solution: precision takes by weighing the protocatechualdehyde 10mg that is dried to constant weight in silica gel drier, puts in the 50ml measuring bottle, adds methanol to scale, shake up, precision is measured 5ml, puts in the 50ml measuring bottle, add methanol to scale, shake up, promptly get (containing protocatechualdehyde 0.02mg among every 1ml).
The preparation of need testing solution: precision is measured this product 5.00ml, puts in the 100ml measuring bottle, adds water to scale, shakes up, as need testing solution.
Algoscopy: precision is measured reference substance solution and each 20 μ l of need testing solution respectively, injects chromatograph of liquid, measures, promptly.
The every 1ml of this product contains former youngster's aldehyde must not be less than 0.17mg.
By three batches of mensuration, 1ml contains protocatechualdehyde and all is no less than 0.17mg as a result.
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 XIANGDAN ZHUSHEYE quality that the explanation of this comparative example is produced with PROCESS FOR TREATMENT of the present invention is better than producing with conventional compound method.(wherein indicate the unspecified project in the conventional formulation quality standard that is of # before the project, but, will carry out the inspection of these these projects) by the version pharmacopeia in 2005 that are about to issue execution
Table 2
| Project | One adopts this technology | Two common process |
| Method for making | Get Lignum Dalbergiae Odoriferae 1000g, the purified water that adds 3 times of weight of medical material weight is 1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divide the layer that deoils, filter paper | Get Lignum Dalbergiae Odoriferae 1000g, the purified water that adds 3 times of weight of medical material amount is 1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours |
| Filter, get the Lignum Dalbergiae Odoriferae Aromatic water, standby; The 1000g red rooted salvia is added medical material weight 8,6,6 times purified water decocts 3 times, 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter, merging filtrate, filtrate concentrates, 0.06% of adding concentrated solution weight clarifier B in concentrated solution, be heated to 70～90 ℃, after leaving standstill 2 hours, 0.03% the clarifier A that adds concentrated solution weight again, after leaving standstill 4 hours, 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 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, the active carbon that adds 0.5 %, boiled 30 minutes, filter, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, adding water for injection, to make every ml contain protocatechualdehyde be 1.5mg, filter, fill was sterilized 30 minutes for 100 ℃ in ampoule. | Divide the layer that deoils, filter paper filtering, get the Lignum Dalbergiae Odoriferae Aromatic water, the 1000g red rooted salvia adds medical material weight 8,6,6 times purified water decocts 3 times, 2 hours for the first time, 1.5 hours for the second time, 1.5 hours for the third time, filter, merging filtrate, filtrate are concentrated into every ml medicinal liquid and contain crude drug amount 4g; Slowly stir and add ethanol down, add ethanol and make that to contain alcohol amount be 75%, 4-8 ℃ of cold preservation 40 hours, filter, 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 85 %, 4-8 ℃ of cold preservation 40 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 16 hours, filter paper filtering, filtrate is regulated PH to 6.5～6.8 with 10% sodium hydroxide solution, boiled 1 hour, the active carbon of adding 1%, boiled 15 minutes, filter, filtrate is regulated PH to 6.8 with 10% sodium hydroxide solution, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, adding water for injection, to make every ml contain protocatechualdehyde be 1.5mg, filter, fill was sterilized 30 minutes for 100 ℃ in ampoule. | |
| Clarity (qualification rate is greater than 95%) | Get 200 of this product, check by " clarity test detailed rules and regulations and criterion ": 20040101 batches: only 4 have chips of glass, qualification rate 98%. | Get 200 of this product, check by " clarity test detailed rules and regulations and criterion ": 20040104 batches: wherein 1 has chips of glass, 9 have the small particles more than 3 |
| 20040102 batches: only 3 have chips of glass, qualification rate 98.5%.20040103 batches: only 3 have chips of glass, qualification rate 98.5%.When getting rid of fill because of the chips of glass factor of the disruptive generation of ampoule, after this PROCESS FOR TREATMENT, the clarity qualification rate reaches 100% substantially. | Qualification rate 95%.20040105 batches: wherein 2 have chips of glass, and 8 have the small particles more than 3, qualification rate 95%.20040106 batches: wherein 4 have chips of glass, and 6 have the small particles more than 3, qualification rate 95%.When getting rid of fill because of the chips of glass factor of the disruptive generation of ampoule, after this PROCESS FOR TREATMENT, the clarity qualification rate is between 95～97 %. | |
| Residue on ignition (must not cross 1.0%) | 0.3% | 0.8% |
| # heavy metal (should be up to specification) | Up to specification | Up to specification |
| # protein | Up to specification | Up to specification |
| The # tannin | Up to specification | Against regulation |
| The # potassium ion | Up to specification | Against regulation |
| # arsenic salt | Up to specification | Up to specification |
| The # resin | Up to specification | Up to specification |
| The # total solid | Leave over residue 2.5%. | Leave over residue 1.5%. |
Comparative example 2
Zest was little when the explanation of this comparative example was used clinically with XIANGDAN ZHUSHEYE of the present invention, and untoward reaction is few.
Table 3
| Technology XIANGDAN ZHUSHEYE of the present invention | The XIANGDAN ZHUSHEYE of common process | |
| Usage and dosage | Intramuscular injection, a 2ml, 1～2 time on the one.Intravenous drip, a 10～20ml uses with 5～10% glucose injections, 250～500ml dilution back, or follows the doctor's advice. | |
| Clinical use | Treat 43 routine patient with angina pectoris | Treat 48 patient with angina pectoris |
| Untoward reaction is observed | Do not have | Do not have |
| Zest is observed | No pain phenomenon | 11 examples have the pain phenomenon, 8 routine injection site rednesses |
Comparative example 3
Treat patient with angina pectoris and common process group clinically relatively:
2 groups of therapeutic outcome comparative examples of table 4 (%)
| Group | The example number | Effectively | Invalid |
| Technology group common process group of the present invention | 43 48 | 40(93) 42(87) | 3(7) 6(13) |
Claims (10)
1. XIANGDAN ZHUSHEYE, get Aromatic water by the medical material Lignum Dalbergiae Odoriferae vapor distillation in will writing out a prescription, medical material Radix Salviae Miltiorrhizae decocting in water, add clarifier, precipitate with ethanol, water precipitating, centrifugal, ultrafiltration multiple technologies means obtain Radix Salviae Miltiorrhizae extract, with Lignum Dalbergiae Odoriferae Aromatic water and Radix Salviae Miltiorrhizae extract mix homogeneously, obtain the effective active components of Radix Salviae Miltiorrhizae Injection, through packing, sterilization, obtain finished product preparation.
2. injection according to claim 1 is characterized in that described Lignum Dalbergiae Odoriferae, Radix Salviae Miltiorrhizae are respectively the 1-1000 weight portion.
3. the preparation method of an XIANGDAN ZHUSHEYE, it is characterized in that the medical material Lignum Dalbergiae Odoriferae vapor distillation in the prescription is got Aromatic water, medical material Radix Salviae Miltiorrhizae decocting in water, add clarifier, precipitate with ethanol, water precipitating, centrifugal, ultrafiltration multiple technologies means obtain Radix Salviae Miltiorrhizae extract, with Lignum Dalbergiae Odoriferae Aromatic water and Radix Salviae Miltiorrhizae extract mix homogeneously, obtain the effective active components of Radix Salviae Miltiorrhizae Injection, through packing, sterilization, obtain finished product preparation.
4. injection according to claim 1 is characterized in that the every ml of described XIANGDAN ZHUSHEYE contains protocatechualdehyde for being no less than 0.17mg.
5. preparation method according to claim 2, it is characterized in that the medical material Lignum Dalbergiae Odoriferae is collected Aromatic water with steam distillation, with the Radix Salviae Miltiorrhizae decocting in water, add clarifier, precipitate with ethanol, water precipitating, centrifugal, ultrafiltration comprises following process: the Lignum Dalbergiae Odoriferae of getting the 1-1000 weight portion, the purified water that adds 3-6 times of weight of medical material weight is 1/3～1/2 of a medical material amount with steam distillation collection distillate, with distillate cold preservation 24 hours, divide the layer that deoils, use filter paper filtering, get the Lignum Dalbergiae Odoriferae Aromatic water, standby; The purified water of 5～8 times of red rooted salvias is decocted 3 times, 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, adds 0.01%～0.5% active carbon, boils 30 minutes, filter paper filtering, put cold, 4-8 ℃ of cold preservation 24 hours, centrifugal with centrifuge, get supernatant, ultrafiltration, add Lignum Dalbergiae Odoriferae Aromatic water and 5 ‰ tween 80s, add an amount of water for injection, filter, fill was sterilized 15～30 minutes for 100～121 ℃ in ampoule.
6. according to claim 3 or 4 described preparation methoies, it is characterized in that collecting distillate is 1/3～1/2 of medical material amount.
7. according to claim 3 or 4 described preparation methoies, it is characterized in that water precipitating before, filtrate is concentrated into every ml medicinal liquid and contains crude drug amount 6～8g.
8. according to claim 3 or 4 described preparation methoies, it is characterized in that using centrifuge centrifugal behind extracting solution and the smart slide liquid mix homogeneously, revolution is 3000～4000 rev/mins.
9. according to claim 3 or 4 described preparation methoies, it is characterized in that ultrafiltration is the ultrafiltration post of molecular cut off 100,000.
10. according to claim 3 or 4 described preparation methoies, it is characterized in that fill adds water for injection and contains protocatechualdehyde to every ml and be no less than 0.17mg before ampoule.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510051488 CN1830465A (en) | 2005-03-08 | 2005-03-08 | Clary injection and its preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510051488 CN1830465A (en) | 2005-03-08 | 2005-03-08 | Clary injection and its preparation method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1830465A true CN1830465A (en) | 2006-09-13 |
Family
ID=36993065
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200510051488 Pending CN1830465A (en) | 2005-03-08 | 2005-03-08 | Clary injection and its preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1830465A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102845797A (en) * | 2012-08-30 | 2013-01-02 | 重庆市集银中药材有限责任公司 | Preparation and application of aromatic water from stems and leaves of honeysuckle flower |
| CN103239505A (en) * | 2013-05-22 | 2013-08-14 | 四川升和药业股份有限公司 | Salvia miltiorrhiza medicine injection preparation containing polyethylene glycol-12-hydroxystearic acid and preparation method of salvia miltiorrhiza medicine injection preparation |
| CN103285135A (en) * | 2013-06-20 | 2013-09-11 | 成都乾坤动物药业有限公司 | Preparation technology for increasing clarity of poplar flower injection |
| CN111728049A (en) * | 2020-06-26 | 2020-10-02 | 湖南黑美人茶业股份有限公司 | Method for preparing fructus aurantii extract for preparing dark tea |
-
2005
- 2005-03-08 CN CN 200510051488 patent/CN1830465A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102845797A (en) * | 2012-08-30 | 2013-01-02 | 重庆市集银中药材有限责任公司 | Preparation and application of aromatic water from stems and leaves of honeysuckle flower |
| CN103239505A (en) * | 2013-05-22 | 2013-08-14 | 四川升和药业股份有限公司 | Salvia miltiorrhiza medicine injection preparation containing polyethylene glycol-12-hydroxystearic acid and preparation method of salvia miltiorrhiza medicine injection preparation |
| CN103239505B (en) * | 2013-05-22 | 2014-03-12 | 四川升和药业股份有限公司 | Salvia miltiorrhiza medicine injection preparation containing polyethylene glycol-12-hydroxystearic acid and preparation method of salvia miltiorrhiza medicine injection preparation |
| CN103285135A (en) * | 2013-06-20 | 2013-09-11 | 成都乾坤动物药业有限公司 | Preparation technology for increasing clarity of poplar flower injection |
| CN111728049A (en) * | 2020-06-26 | 2020-10-02 | 湖南黑美人茶业股份有限公司 | Method for preparing fructus aurantii extract for preparing dark tea |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102488863A (en) | Chinese herbal medicine compound with anticancer effect, preparation method and detection method thereof | |
| CN1872106A (en) | Application of wild basil circle leaves in treating disease of virulence cold | |
| CN100418512C (en) | 'Shengmai' infusion and its preparation process | |
| CN1931369A (en) | Medicine composition containing cyclodextrin/polyene taxol and its prepn process | |
| CN1830465A (en) | Clary injection and its preparation method | |
| CN101040906A (en) | Injection for treating cardiovascular or cerebrovascular disease and the preparing method and the quality control method | |
| CN1270769C (en) | Cinobufotalin lyophilized powder for injection and its preparation method | |
| CN1709417A (en) | Ainsliaea fragrans champ extract and its preparing method | |
| CN1297279C (en) | Medicinal composition containing danshensu, total ara-saponin and camphol and its preparation and use | |
| CN1775233B (en) | Red-rooted-salvia-root chuanxiong-rhizome azine injecta, its preparation method and use | |
| CN100490876C (en) | Sarcadra injection, its making method and venous injection | |
| Oforibika et al. | Study of the renal function of Wistar albino rat treated with three different herbal bitters (Confam, G. Winco and 1960 Roots) | |
| CN102846704A (en) | A Leonurus japonicus injection, its preparation method, and method for detecting total alkaloids | |
| CN1158295C (en) | Process for preparing tetra-hexose ganglioside monosialate | |
| CN1322872C (en) | Fracture union-promoting medicine and its preparation | |
| CN101081250A (en) | Potygonum multiflorum thunb extract medicament for treating anemia and the preparing method thereof | |
| WO2019113861A1 (en) | Ginkgo biloba extract medicinal raw material and preparation method therefor | |
| CN100490875C (en) | Blackberrylily rhizome antiviral injection, preparation and venous medicine feeding blackberrylily rhizome antiviral injection thereof | |
| CN1830461A (en) | Safflower injection and its preparation method | |
| CN1264506C (en) | Pharmaceutical combination containing red sage root element and preparation method thereof | |
| CN1751691A (en) | Small volume intravenous injection of gastrodine and its prepn. method | |
| CN1785212A (en) | Novel cinobufogenin freeze-drying powder injection, its prepn. method and quality control method | |
| CN101045103A (en) | Traditional Chinese medicine for treating arthrolithiasis of fowl, its preparating method and use | |
| CN1872101A (en) | Distillage of Ardisia chinensis Benth of possessing function of antivirus, distilling method and application | |
| CN1817356A (en) | Production of vermilion injection for treating cardiovascular disease |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C57 | Notification of unclear or unknown address | ||
| DD01 | Delivery of document by public notice |
Addressee: Xu Wenjie Document name: Notification of the application for patent for invention to go through the substantive examination procedure |
|
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20060913 |