CN101422456A - Medicine combination drop-pills and preparation method and quality detection method thereof - Google Patents
Medicine combination drop-pills and preparation method and quality detection method thereof Download PDFInfo
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- CN101422456A CN101422456A CNA2007101767843A CN200710176784A CN101422456A CN 101422456 A CN101422456 A CN 101422456A CN A2007101767843 A CNA2007101767843 A CN A2007101767843A CN 200710176784 A CN200710176784 A CN 200710176784A CN 101422456 A CN101422456 A CN 101422456A
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- bilobalide
- medicament composition
- dropping pills
- ginkalide
- composition dropping
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Abstract
The invention discloses a ginkgolides dripping pill and a preparation method and a quality detection method thereof. During the preparation process, the ginkgolides and various substrates are evenly mixed and heated according to proportion, stirred and suspended and finally prepared into the dripping pill in a gradient way; one or a plurality of distinguishing or content detecting methods are adopted to carry out quality detection. The preparation formulation of the dripping pill selected by the ginkgolides dripping pill is the typical preparation formulation of the oral administration in the modern traditional Chinese medicines, and is characterized by high medicament stability, hard hydration and oxidation, quick effect, high bioavailability as well as convenient use and carrying. The ginkgolides is a medicament which is hardly dissolved in water, is dispersed into the substrates and prepared into the dripping pill; moreover, the solubility, the stripping speed and the bioavailability thereof are improved.
Description
Technical field
The present invention relates to a kind of medicament composition dropping pills and preparation method thereof and quality determining method, particularly a kind of bilobalide drop pill and preparation method thereof and quality determining method.
Background technology
Modern study finds that Folium Ginkgo can be regulated the tension force and the elasticity of blood vessel, and the protection blood vessel is avoided infringement; Folium Ginkgo can also lower hematoblastic bonding force, and then the circulation, the protection erythrocyte that influence blood avoid destroying, and allows erythrocyte scatter uniformly in blood vessel, and this measure helps the conveying and the supply of oxygen in the erythrocyte.Along with the development of Folium Ginkgo research, now prove: the active component of Folium Ginkgo mainly is flavone and lactone compound.Bilobalide is that a class of only finding in Folium Ginkgo has the Chinese medicine ingredients of special construction and remarkable pharmacologically active, does not find as yet so far to be present in other any plants.The bilobalide constituents is definite with its pharmacology, drug action, can stop the platelet aggregation that platelet activating factor (PAF) causes fully and has caused the extensive concern of Chinese scholars.PAF is a kind of important inflammatory mediator, also is one of medium of multiple disease incidence, and pathological study shows that PAF plays an important role in the processes such as shock that allergy, ulcer, asthma, thrombosis, inflammation, organ-graft refection, endotoxin cause.
Both at home and abroad the Folium Ginkgo series products has been carried out many researchs and clinical use is arranged at present, 2005 editions division of traditional Chinese drugs of Chinese Pharmacopoeia have also recorded kinds such as Folium Ginkgo, Semen Ginkgo extrac and Folium Ginkgo, but pure bilobalide launch is not arranged at present as yet.
Summary of the invention
One object of the present invention is to disclose a kind of medicament composition dropping pills; Another object of the present invention is to disclose a kind of bilobalide drop pill; The 3rd purpose of the present invention is to disclose the preparation technology of this medicament composition dropping pills; The 4th purpose of the present invention is to disclose the quality determining method of this medicament composition dropping pills.
The present invention seeks to be achieved through the following technical solutions:
Medicament composition dropping pills of the present invention is made up of the raw material of following weight ratio:
Bilobalide: substrate=1: 0.5-12; Described substrate is that any or two kinds of conventional ratios of Macrogol 4000, polyethylene glycol 6000, stearic acid, glyceryl monostearate or gelatin combine; In above-mentioned substrate, can also add a kind of surfactant constituents in the tween-80, lecithin, carbomer of 0.5%-2.5%; Ginkalide B content in the described bilobalide is not less than 50%, and ginkalide A, B, K total content are not less than 90%.
Aforementioned pharmaceutical compositions drop pill raw material preferred weight ratio of the present invention is:
Bilobalide: substrate=1:1-8.
Aforementioned pharmaceutical compositions drop pill raw material preferred weight ratio of the present invention is:
Bilobalide: substrate=1:2.5.
Aforementioned pharmaceutical compositions drop pill raw material preferred weight ratio of the present invention is:
Bilobalide: substrate=1:1.5.
Aforementioned pharmaceutical compositions drop pill raw material preferred weight ratio of the present invention is:
Bilobalide: substrate=1:5 or 1:6.
The preparation method of medicament composition dropping pills of the present invention is: gets bilobalide 10 weight portions, bilobalide pulverized the 100-200 eye mesh screen, get the bilobalide fine powder, and standby; Get 5-120 weight portion Macrogol 4000, polyethylene glycol 6000, stearic acid, glyceryl monostearate or any substrate of gelatin or the two kinds of substrate compositions formed of ratio routinely, be heated to fusion, under 40-95 ℃ of keeping warm mode, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 18-2 ℃ dimethicone 100, liquid paraffin or the vegetable oil through water dropper, molding promptly.
The preparation method of medicament composition dropping pills of the present invention is preferably: gets bilobalide 10 weight portions, bilobalide pulverized the 100-200 eye mesh screen, get the bilobalide fine powder, and standby; Get 10-80 weight portion Macrogol 4000, polyethylene glycol 6000, stearic acid, glyceryl monostearate or any substrate of gelatin or the two kinds of substrate compositions formed of ratio routinely, be heated to fusion, under 60-85 ℃ of keeping warm mode, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 15-2 ℃ dimethicone 100, liquid paraffin or the vegetable oil through water dropper, molding promptly.
The preparation method of medicament composition dropping pills of the present invention is preferably: gets bilobalide 10 weight portions, bilobalide pulverized 120 eye mesh screens, get the bilobalide fine powder, and standby; Get 25 weight portion polyethylene glycol 6000s, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 10-2 ℃ the dimethicone 100 through water dropper, molding promptly.
The preparation method of medicament composition dropping pills of the present invention is preferably: gets bilobalide 10 weight portions, bilobalide pulverized 150 eye mesh screens, get the bilobalide fine powder, and standby; Get 15 weight portion Macrogol 4000s, be heated to fusion, under 85 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 14-2 ℃ the liquid paraffin through water dropper, molding promptly.
The preparation method of medicament composition dropping pills of the present invention is preferably: gets bilobalide 10 weight portions, bilobalide pulverized 110 eye mesh screens, get the bilobalide fine powder, and standby; Get 60 weight portion stearic acid, be heated to fusion, under 70 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 16-2 ℃ the vegetable oil through water dropper, molding promptly.
Gradient cooling in the above-mentioned preparation method is meant the coolant temperature Gradient distribution, keeps the temperature of condensing tube upper coolant to be controlled at 10-18 ℃, and the temperature of condensing tube bottom liquid coolant is controlled at 2 ℃.
Day taking dose or the using dosage of medicament composition dropping pills of the present invention determine, every day taking dose in ginkalide A, B total amount, be 210～345mg.It is identical to contain suitable raw medicinal herbs amount in day taking dose of different preparations or the using dosage.Method of quality control of the present invention is that unit detects preparation with daily dosage promptly.
The quality determining method of medicament composition dropping pills of the present invention comprises that following discriminating or content side decide one or more in the method:
Differentiate: get medicament composition dropping pills 20 balls of the present invention, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography, with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:18-36:60-85 is mobile phase, detect wavelength 210～230nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time;
Assay: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia); The test of chromatographic condition and system suitability as filler, is a mobile phase with normal propyl alcohol-oxolane-water of 1:18-36:60-85 with octadecylsilane chemically bonded silica, and the detection wavelength is 210～230nm; Get medicament composition dropping pills 20 balls of the present invention, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Normal propyl alcohol-oxolane of the preferred 1:27:72 of mobile phase-water in above-mentioned discriminating or the content assaying method.Normal propyl alcohol-oxolane of the preferred 1:32:65 of mobile phase-water in above-mentioned discriminating or the content assaying method.
Normal propyl alcohol-oxolane of the preferred 1:21:80 of mobile phase-water in above-mentioned discriminating or the content assaying method.
Detect the preferred 220nm of wavelength in above-mentioned discriminating or the content assaying method.
The selected drops of medicament composition dropping pills of the present invention is the representative dosage form of modern Chinese medicine oral administration, have the medicine stability height, be difficult for hydrolysis oxidation, rapid-action, bioavailability is high, use and convenient carrying, bilobalide is a poorly water soluble drugs, be scattered in the substrate, make drop pill, improved its dissolubility, dissolution rate and bioavailability.
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
The quality control standard of experimental example medicament composition dropping pills raw material of the present invention bilobalide
1.1 character: should be white crystalline powder; Odorless, bitter in the mouth.
1.2 differentiate: the high performance liquid chromatography inspection should detect ginkalide A, ginkalide B, ginkalide C, bilobalide K chromatographic peak.
1.3 check item:
Loss on drying is got embodiment 1 described drug regimen raw material 1g of the present invention, is dried to constant weight at 105 ℃, and subtracting weight loss must not surpass 6.0%.
Residue on ignition must not be crossed 0.1% (700～800 ℃ of blazing temperature).
Heavy metal is got embodiment 1 described drug regimen raw material 1g of the present invention, and according to the operation of residue on ignition inspection technique, 500～600 ℃ of blazing temperature are checked in accordance with the law, contain heavy metal and must not cross 10/1000000ths.Arsenic salt is got embodiment 1 described drug regimen raw material 1g of the present invention, according to the operation of residue on ignition inspection technique, and 500～600 ℃ of blazing temperature, residue adds hydrochloric acid 5ml, and water 23ml checks in accordance with the law, contains arsenic salt and must not cross 2/1000000ths.
Ginkgoic acid C
13:0Check according to high performance liquid chromatography (2005 editions appendix VID of Chinese Pharmacopoeia).Drug regimen raw material argentiferous Fructus Pruni acid C of the present invention
13:0Must not cross 2/1000000ths.
1.4 assay is according to high effective liquid chromatography for measuring.Drug regimen raw material bilobalide-containing A (C of the present invention
20H
24O
9), ginkalide B (C
20H
24O
10), bilobalide K (C
20H
22O
10) total amount must not be less than 90.0%, ginkalide B content must not be lower than 50.0%.
1.5 the methodological study of assay
1.5.1 precision is investigated
Accurate reference substance (the ginkalide A: 328 μ g/ml of drawing; Ginkalide B: solution 10 μ l 364 μ g/ml), repeat sample introduction 6 times, record the peak area integrated value, calculate RSD.The results are shown in following table:
The test of table 1 precision
1.5.2 stability test
(lot number: 041201) about 1g prepares need testing solution by need testing solution preparation method under the assay item, the accurate need testing solution 10 μ l that draw to get this product, injected chromatograph of liquid respectively on the the 0th, 1,2,4,8,12,24 hour, sample introduction is 7 times altogether, records the peak area integrated value, calculates RSD.The result shows that ginkalide A, B test liquid are basicly stable in 24 hours.The results are shown in following table:
Table 2 stability test
1.5.3 replica test
Get this product (lot number: 041201) about 1g, the porphyrize mixing, get five parts, every part of about 30mg prepares need testing solution by need testing solution preparation method under the assay item, the accurate need testing solution 10 μ l that draw, measure, calculate content, the result shows that this method is measured ginkalide A, B content repeatability is good, the ginkalide A average content is 10.14%, RSD=0.83%; The ginkalide B average content is 15.09%, RSD=2.21%.The results are shown in following table:
Table 3 replica test
1.5.4 average recovery test
Get known content this product (lot number: 041201, ginkalide A content: 10.14%; Ginkalide B content: 15.09%), porphyrize is got five parts, and accurate the title decides, accurate respectively reference substance solution (the ginkalide A 2.211mg/ml that adds; Ginkalide B 26.64mg/ml) 1ml prepares need testing solution by the need testing solution preparation method of ginkalide A, B under the assay item, carries out assay, and calculate recovery rate.The result shows that the response rate meets the requirements, and shows that this method response rate is good, the results are shown in following table:
The test of table 4 ginkalide A average recovery
The test of table 5 ginkalide B average recovery
Conclusion: show that through above methodological study result this method precision, repeatability, application of sample reclaim all better, can measure the content of ginkalide A in the finished product, B accurately and fast.
Following embodiment all can realize the effect of above-mentioned experimental example.
The specific embodiment
Embodiment 1: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; Get the 2.5kg polyethylene glycol 6000, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 10-2 ℃ dimethicone 100, the gradient cooling, molding, 100,000 drop pill (35mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 35mg, one time 10 ball, 3 times on the one.
Embodiment 2: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 150 eye mesh screens, get the bilobalide fine powder, standby; Get the 1.5kg Macrogol 4000, be heated to fusion, under 85 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt machinery that spice is splashed into gradient cooling in 14-2 ℃ the liquid paraffin through water dropper, molding, 100,000 drop pill (25mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 25mg, one time 10 ball, 3 times on the one.
Embodiment 3: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 110 eye mesh screens, get the bilobalide fine powder, standby; Get the 6kg stearic acid, be heated to fusion, under 70 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 16-2 ℃ vegetable oil, the gradient cooling, molding, 100,000 drop pill (70mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 70mg, one time 10 ball, 3 times on the one.
Embodiment 4: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; The mixture 2.5kg of taking polyethylene glycol 6000: Macrogol 4000=1:1 is heated to fusion, adds the bilobalide fine powder under 80 ℃ of keeping warm modes, stirs and makes suspendible; Adopt machinery with spice in water dropper splashes into 18-2 ℃ dimethicone 100, the gradient cooling, molding, 100,000 drop pill (35mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 35mg, one time 10 ball, 3 times on the one.
Embodiment 5: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; Get 10% gelatin 2.5kg, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 15-2 ℃ dimethicone 100, the gradient cooling, molding, 100,000 drop pill (35mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 35mg, one time 10 ball, 3 times on the one.
Embodiment 6: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; Get stearic acid 2.5kg, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 16-2 ℃ dimethicone 100, the gradient cooling, molding, 100,000 drop pill (35mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 35mg, one time 10 ball, 3 times on the one.
Embodiment 7: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; Get glyceryl monostearate 5kg, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 14-2 ℃ dimethicone 100, the gradient cooling, molding, 100,000 drop pill (60mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 60mg, one time 10 ball, 3 times on the one.
Embodiment 8: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; Get the 2.5kg polyethylene glycol 6000, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, and add 37.5g tween-80, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 10-2 ℃ dimethicone 100, the gradient cooling, molding, 100,000 drop pill (35mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 35mg, one time 10 ball, 3 times on the one.
Embodiment 9: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 150 eye mesh screens, get the bilobalide fine powder, standby; Get the 1.5kg Macrogol 4000, be heated to fusion, under 85 ℃ of keeping warm modes, add the bilobalide fine powder, and add 15g lecithin, stir and make suspendible; Adopt machinery that spice is splashed into gradient cooling in 14-2 ℃ the liquid paraffin through water dropper, molding, 100,000 drop pill (25mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 25mg, one time 10 ball, 3 times on the one.
Embodiment 10: medicament composition dropping pills of the present invention
Get bilobalide 1kg, bilobalide was pulverized 110 eye mesh screens, get the bilobalide fine powder, standby; Get the 6kg stearic acid, be heated to fusion, under 70 ℃ of keeping warm modes, add the bilobalide fine powder, and add the 120g carbomer, stir and make suspendible; Adopt machinery with spice in water dropper splashes into 16-2 ℃ vegetable oil, the gradient cooling, molding, 100,000 drop pill (70mg/ ball); The every ball bilobalide-containing of medicament composition dropping pills of the present invention is with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg, wherein ginkalide A (C
20H
24O
9) should be 2.0～4.0mg, ginkalide B (C
20H
24O
10) should be 5.0～7.5mg; Oral, every ball 70mg, one time 10 ball, 3 times on the one.
Embodiment 11: the method for quality control of medicament composition dropping pills of the present invention
Differentiate: get medicament composition dropping pills of the present invention 20 balls of embodiment 1 preparation, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography (2005 editions one appendix VI D of Chinese Pharmacopoeia), with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:27:72 is mobile phase, detect wavelength 220nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time.
Embodiment 12: the method for quality control of medicament composition dropping pills of the present invention
Differentiate: get medicament composition dropping pills of the present invention 20 balls of embodiment 2 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography (2005 editions appendix VID of Chinese Pharmacopoeia), with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:32:65 is mobile phase, detect wavelength 230nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time.
Embodiment 13: the method for quality control of medicament composition dropping pills of the present invention
Differentiate: get medicament composition dropping pills of the present invention 20 balls of embodiment 3 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography (2005 editions appendix VID of Chinese Pharmacopoeia), with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:21:80 is mobile phase, detect wavelength 210nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time.
Embodiment 14: the method for quality control of medicament composition dropping pills of the present invention
Assay: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia D); Chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica as filler, normal propyl alcohol-oxolane-water with 1:27:72 is mobile phase, and the detection wavelength is 220nm, gets medicament composition dropping pills of the present invention 20 balls of embodiment 4 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, be settled to scale, get need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Embodiment 15: the method for quality control of medicament composition dropping pills of the present invention
Assay: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia); Chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica as filler, normal propyl alcohol-oxolane-water with 1:32:65 is mobile phase, and the detection wavelength is 220nm, gets medicament composition dropping pills of the present invention 20 balls of embodiment 5 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, be settled to scale, get need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Embodiment 16: the method for quality control of medicament composition dropping pills of the present invention
Assay: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia); Chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica as filler, normal propyl alcohol-oxolane-water with 1:21:80 is mobile phase, and the detection wavelength is 230nm, gets medicament composition dropping pills of the present invention 20 balls of embodiment 6 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, be settled to scale, get need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Embodiment 17: the method for quality control of medicament composition dropping pills of the present invention
Differentiate: get medicament composition dropping pills of the present invention 20 balls of embodiment 7 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography (2005 editions one appendix VI D of Chinese Pharmacopoeia), with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:27:72 is mobile phase, detect wavelength 220nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time;
Assay: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia); Chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica as filler, normal propyl alcohol-oxolane-water with 1:27:72 is mobile phase, and the detection wavelength is 220nm, gets medicament composition dropping pills of the present invention 20 balls of embodiment 7 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, be settled to scale, get need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Embodiment 18: the method for quality control of medicament composition dropping pills of the present invention
Differentiate: get medicament composition dropping pills of the present invention 20 balls of embodiment 8 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography (2005 editions appendix VID of Chinese Pharmacopoeia), with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:32:65 is mobile phase, detect wavelength 210nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time;
Assay: measure according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia D); Chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica as filler, normal propyl alcohol-oxolane-water with 1:32:65 is mobile phase, and the detection wavelength is 210nm, gets medicament composition dropping pills of the present invention 20 balls of embodiment 8 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, be settled to scale, get need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Embodiment 19: the method for quality control of medicament composition dropping pills of the present invention
Differentiate: get medicament composition dropping pills of the present invention 20 balls of embodiment 9 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to high performance liquid chromatography (2005 editions appendix VID of Chinese Pharmacopoeia), with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:21:80 is mobile phase, detect wavelength 230nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time;
Assay: measure according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia); Chromatographic condition and system suitability test, with octadecylsilane chemically bonded silica as filler, normal propyl alcohol-oxolane-water with 1:21:80 is mobile phase, and the detection wavelength is 230nm, gets medicament composition dropping pills of the present invention 20 balls of embodiment 9 preparations, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, be settled to scale, get need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with ginkalide A (C
20H
24O
9), ginkalide B (C
20H
24O
10) the total amount meter, should be 7.0～11.5mg.
Claims (16)
1, a kind of medicament composition dropping pills is characterized in that this medicament composition dropping pills is made up of the raw material of following weight ratio:
Bilobalide: substrate=1:0.5-12; Described substrate is meant that any or two kinds of conventional ratios of Macrogol 4000, polyethylene glycol 6000, stearic acid, glyceryl monostearate or gelatin combine; Ginkalide B content in the described bilobalide is not less than 50%, and ginkalide A, B, K total content are not less than 90%.
2, medicament composition dropping pills as claimed in claim 1 is characterized in that in wherein said substrate adding a kind of surfactant constituents in the tween-80, lecithin, carbomer of 0.5%-2.5%.
3, medicament composition dropping pills as claimed in claim 1 or 2 is characterized in that this medicament composition dropping pills is made up of the raw material of following weight ratio:
Bilobalide: substrate=1:1-8.
4, medicament composition dropping pills as claimed in claim 1 or 2 is characterized in that this medicament composition dropping pills is made up of the raw material of following weight ratio:
Bilobalide: substrate=1:2.5.
5, medicament composition dropping pills as claimed in claim 1 or 2 is characterized in that this medicament composition dropping pills is made up of the raw material of following weight ratio:
Bilobalide: substrate=1:1.5.
6, medicament composition dropping pills as claimed in claim 1 or 2 is characterized in that this medicament composition dropping pills is made up of the raw material of following weight ratio:
Bilobalide: substrate=1:5 or 1:6.
7, a kind of preparation method of medicament composition dropping pills is characterized in that this method is:
Get bilobalide 10 weight portions, bilobalide was pulverized the 100-200 eye mesh screen, get the bilobalide fine powder, standby; Get 5-120 weight portion Macrogol 4000, polyethylene glycol 6000, stearic acid, glyceryl monostearate or any substrate of gelatin or the two kinds of substrate compositions formed of ratio routinely, be heated to fusion, under 40-90 ℃ of keeping warm mode, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 18-2 ℃ dimethicone 100, liquid paraffin or the vegetable oil through water dropper, molding promptly.
8, the preparation method of medicament composition dropping pills as claimed in claim 7 is characterized in that this method is:
Get bilobalide 10 weight portions, bilobalide was pulverized the 100-200 eye mesh screen, get the bilobalide fine powder, standby; Get 10-80 weight portion Macrogol 4000, polyethylene glycol 6000, stearic acid, glyceryl monostearate or any substrate of gelatin or the two kinds of substrate compositions formed of ratio routinely, be heated to fusion, under 60-80 ℃ of keeping warm mode, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 15-2 ℃ dimethicone 100, liquid paraffin or the vegetable oil through water dropper, molding promptly.
9, the preparation method of medicament composition dropping pills as claimed in claim 7 is characterized in that this method is:
Get bilobalide 10 weight portions, bilobalide was pulverized 120 eye mesh screens, get the bilobalide fine powder, standby; Get 25 weight portion polyethylene glycol 6000s, be heated to fusion, under 80 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 10-2 ℃ the dimethicone 100 through water dropper, molding promptly.
10, the preparation method of medicament composition dropping pills as claimed in claim 7 is characterized in that this method is:
Get bilobalide 10 weight portions, bilobalide was pulverized 150 eye mesh screens, get the bilobalide fine powder, standby; Get 15 weight portion Macrogol 4000s, be heated to fusion, under 85 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 14-2 ℃ the liquid paraffin through water dropper, molding promptly.
11, the preparation method of medicament composition dropping pills as claimed in claim 7 is characterized in that this method is:
Get bilobalide 10 weight portions, bilobalide was pulverized 110 eye mesh screens, get the bilobalide fine powder, standby; Get 60 weight portion stearic acid, be heated to fusion, under 70 ℃ of keeping warm modes, add the bilobalide fine powder, stir and make suspendible; Adopt craft or machinery that spice is splashed into gradient cooling in 16-2 ℃ the vegetable oil through water dropper, molding promptly.
12, a kind of quality determining method of medicament composition dropping pills is characterized in that this method comprises in fixed one or more of following discriminating or content side:
Differentiate: get this medicament composition dropping pills 20 balls, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B, ginkalide C, bilobalide K reference substance, add dissolve with methanol respectively and make the solution that every 1ml contains 0.3mg, 0.5mg, 0.5mg, 0.1mg, in contrast product solution; Test according to 2005 editions one appendix VI D of Chinese Pharmacopoeia high performance liquid chromatography, with octadecylsilane chemically bonded silica is filler, normal propyl alcohol-oxolane-water with 1:18-36:60-85 is mobile phase, detect wavelength 210～230nm, draw reference substance solution and need testing solution respectively, inject chromatograph of liquid, should present the chromatographic peak identical in the test sample chromatograph with the reference substance retention time;
Assay: according to an appendix VID of Chinese Pharmacopoeia high effective liquid chromatography for measuring; The test of chromatographic condition and system suitability as filler, is a mobile phase with normal propyl alcohol-oxolane-water of 1:18-36:60-85 with octadecylsilane chemically bonded silica, and the detection wavelength is 210～230nm; Get medicament composition dropping pills 20 balls of the present invention, porphyrize, precision takes by weighing the drop pill fine powder that is equivalent to ginkgo lactone material 8.57mg, puts in the 10ml measuring bottle, adds dissolve with methanol, is settled to scale, gets need testing solution; Get ginkalide A, ginkalide B reference substance respectively, the accurate title, decide, and adds methanol and make the solution that every 1ml contains 0.3mg, 0.45mg, gets reference substance solution; Accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, measure, promptly; Medicament composition dropping pills day of the present invention taking dose 1/30 bilobalide-containing with C
20H
24O
9Ginkalide A, C
20H
24O
10The total amount meter of ginkalide B should be 7.0～11.5mg.
13, the quality determining method of medicament composition dropping pills as claimed in claim 12 is characterized in that the mobile phase described in this method is normal propyl alcohol-oxolane-water of 1:27:72.
14, the quality determining method of medicament composition dropping pills as claimed in claim 12 is characterized in that the mobile phase described in this method is normal propyl alcohol-oxolane-water of 1:32:65.
15, the quality determining method of medicament composition dropping pills as claimed in claim 12 is characterized in that the mobile phase described in this method is normal propyl alcohol-oxolane-water of 1:21:80.
16, the quality determining method of medicament composition dropping pills as claimed in claim 12 is characterized in that the detection wavelength described in this method is 220nm.
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| CN2007101767843A CN101422456B (en) | 2007-11-02 | 2007-11-02 | Preparation method and quality detection method for medicine composition drop-pills |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924197A (en) * | 2015-12-30 | 2017-07-07 | 成都百裕制药股份有限公司 | A kind of Ginkgolides drop pills and preparation method thereof |
| CN107753445A (en) * | 2016-08-18 | 2018-03-06 | 江苏康缘药业股份有限公司 | A kind of bilobalide K dripping pill and preparation method thereof |
| CN108125988A (en) * | 2017-12-31 | 2018-06-08 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | Ginkolide B is in the application that microglia inflammatory reaction is inhibited to mitigate Alzheimer disease symptoms |
| WO2020073844A1 (en) | 2018-10-08 | 2020-04-16 | 成都百裕制药股份有限公司 | Dropping pill comprising ginkgo terpene lactones as active components and preparation method therefor |
| CN113133976A (en) * | 2020-01-19 | 2021-07-20 | 成都百裕制药股份有限公司 | A dripping pill containing ginkgolide as effective component |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1249067C (en) * | 2003-08-30 | 2006-04-05 | 曹明成 | Extracting process for bilobalide A, B, C and its preparation |
| CN100490801C (en) * | 2005-12-16 | 2009-05-27 | 陈卫东 | Ginkgolide B dropping pill and its preparing method |
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2007
- 2007-11-02 CN CN2007101767843A patent/CN101422456B/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106924197A (en) * | 2015-12-30 | 2017-07-07 | 成都百裕制药股份有限公司 | A kind of Ginkgolides drop pills and preparation method thereof |
| CN106924197B (en) * | 2015-12-30 | 2020-05-08 | 成都百裕制药股份有限公司 | A bilobalide dripping pill and its preparation method |
| CN107753445A (en) * | 2016-08-18 | 2018-03-06 | 江苏康缘药业股份有限公司 | A kind of bilobalide K dripping pill and preparation method thereof |
| CN108125988A (en) * | 2017-12-31 | 2018-06-08 | 温州医科大学附属第二医院、温州医科大学附属育英儿童医院 | Ginkolide B is in the application that microglia inflammatory reaction is inhibited to mitigate Alzheimer disease symptoms |
| WO2020073844A1 (en) | 2018-10-08 | 2020-04-16 | 成都百裕制药股份有限公司 | Dropping pill comprising ginkgo terpene lactones as active components and preparation method therefor |
| CN113133976A (en) * | 2020-01-19 | 2021-07-20 | 成都百裕制药股份有限公司 | A dripping pill containing ginkgolide as effective component |
| CN113133976B (en) * | 2020-01-19 | 2022-03-04 | 成都百裕制药股份有限公司 | A dripping pill containing ginkgolide as effective component |
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|---|---|
| CN101422456B (en) | 2011-05-04 |
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