CN101647942A - Quality testing method of Yindanxinnaotong soft capsules - Google Patents
Quality testing method of Yindanxinnaotong soft capsules Download PDFInfo
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Abstract
The invention discloses a quality testing method of Yindanxinnaotong soft capsules. The method improves the TCL identification of pseudo-ginseng on the basis of the prior quality standard, supplementsthe identification of tanshinone IIA and erigeron breviscapus in Salvia miltiorrhiza, improves the content determination of Salvia miltiorrhiza and adds the content determination of gingko general flavone. The method can effectively control the main medicinal components of the Yindanxinnaotong soft capsules and greatly enhances the quality testing level of the Yindanxinnaotong soft capsules. Themethod is good for the manufacturers and the supervisory and management department to monitor the product quality, and can provide better guarantees for the treatment of the medical-care department and the patients.
Description
Technical field
The invention belongs to the pharmaceutical technology field, relate to a kind of quality determining method of soft capsule, particularly a kind of quality determining method for the treatment of the soft capsule (adopted name or nomenclature of drug lunar caustic heart and brain clearing soft capsule) of cardiovascular and cerebrovascular disease.
Background technology
Lunar caustic heart and brain clearing soft capsule has the function of blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain, relieving dyspepsia.Be used for the thoracic obstruction that qi depression to blood stasis causes, disease is seen chest pain, and is uncomfortable in chest, breathes hard cardiopalmus etc., angina pectoris, hyperlipemia, cerebral arteriosclerosis, apoplexy, apoplexy sequela.Folium Ginkgo, Radix Salviae Miltiorrhizae, Radix Notoginseng, Herba Erigerontis are respectively the characteristic index compositions of lunar caustic heart and brain clearing soft capsule.In existing lunar caustic heart and brain clearing soft capsule quality standard, the TLC repeatability that Radix Notoginseng is differentiated is bad, oozing property of ester composition (tanshinone) and Herba Erigerontis in the Radix Salviae Miltiorrhizae is not carried out qualitative control.The content assaying method of Radix Salviae Miltiorrhizae is not good in addition, Ginkgo total flavones content in the Folium Ginkgo is not control effectively.Above problem is unfavorable for that manufacturer and superintendent office are to controllable quality.For the quality that further guarantees this product and more help supervision, management to this product quality, thus be necessary the quality determining method of this medicine is improved, thus further guarantee the quality and the curative effect of this product.
Summary of the invention
The objective of the invention is: the quality determining method that a kind of lunar caustic heart and brain clearing soft capsule is provided.The present invention is on initial quality control basis, increased the method that can effectively detect to the main pharmaceutical compositions of lunar caustic heart and brain clearing soft capsule, remedied the deficiency of proper mass control procedure, improved the quality monitoring level of product, also helped administration section product monitoring.
Purpose of the present invention can realize by following technical proposal: the quality determining method of lunar caustic heart and brain clearing soft capsule, calculate according to weight, lunar caustic heart and brain clearing soft capsule is to make 1000 seed lac wafers with Folium Ginkgo 500g, Radix Salviae Miltiorrhizae 500g, Herba Erigerontis 300g, Herb Gynostemmae Pentaphylli 300g, Fructus Crataegi 400g, Bulbus Allii 400g, Radix Notoginseng 200g, Blumeae preparatum Tabellae 10g; It is characterized in that this quality determining method may further comprise the steps:
Character: this product (lunar caustic heart and brain clearing soft capsule) is a soft capsule, and content is brown to tan paste; The gas suffering, mildly bitter flavor.
Differentiate: (1) gets this product content 1g, adds water 20ml stirring and makes molten loosing, with petroleum ether (30～60 ℃) extracting twice, each 20ml, discard petroleum ether layer, water layer extracted with diethyl ether 3 times, each 20ml, merge ether solution, water-bath volatilizes, and residue adds ethyl acetate 2ml, stirs, leave standstill, get supernatant as need testing solution.Other gets the tanshinone reference substance, adds ethyl acetate and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B).Drawing each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate petroleum ether (30～60 ℃) (18: 1: 1), launches, and takes out, and dries.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the kermesinus speckle of same color.
(2) get this product content 2g, add petroleum ether (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant, residue add methanol 20ml, and reflux 15 minutes is put cold, filter, filtrate evaporate to dryness, residue add water 20ml, and slight fever makes dissolving, add water saturated n-butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with ammonia solution 25ml washing, discard ammonia solution, the saturated water washing of reuse n-butyl alcohol 2 times, each 25ml, n-butyl alcohol liquid is concentrated into dried, and residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Notoginseng control medicinal material 0.5g, adds about 5 of water, stirs evenly, add methanol 20ml, reflux 15 minutes is put cold, filter, filtrate evaporate to dryness, residue add water 20ml, slight fever makes dissolving, adds water saturated n-butyl alcohol 25ml, and jolting is extracted, get n-butanol extracting liquid, use the saturated water washing of n-butyl alcohol 2 times, each 25ml, n-butyl alcohol liquid is concentrated into dried, and residue adds methanol 1ml makes dissolving, in contrast medical material solution.Get arasaponin R1 again, add methanol and make 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 2005 B), draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, placing stratified lower floor solution below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing in 105 ℃, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get this product content 1.5g, add petroleum ether (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant, residue add 50% ethanol 30ml, reflux, extract, 30 minutes, filter, filtrate is waved to there not being the alcohol flavor, and residue adds the dissolving of water 20ml slight fever, filter while hot, cooling, filtrate is transferred pH value to 1～2 with hydrochloric acid, reuse ethyl acetate extraction 2 times, each 15ml, combined ethyl acetate liquid, volatilize, residue adds methanol 1ml dissolving, as need testing solution.Other gets Herba Erigerontis control medicinal material 1g, from adding 50% ethanol 30ml, shines medical material solution in pairs with legal system.Get the scutellarin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 2 μ l of above-mentioned three kinds of solution, ribbon is put on same polyamide film respectively, is developing solvent with glacial acetic acid-ethanol (4: 1), launches, take out, dry, spray is with 2% ferric chloride alcoholic solution, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
In the quality determining method of above-mentioned lunar caustic heart and brain clearing soft capsule, also comprise:
Check, should meet every regulation relevant under the capsule item (an appendix I of Chinese Pharmacopoeia version in 2005 L).
The assay of danshensu sodium is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water-acetic acid (5: 160: 1) is mobile phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the danshensu sodium peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the danshensu sodium reference substance, adds methanol and make the solution that every 1ml contains 32 μ g, promptly.
The preparation of need testing solution: get the content under this product content uniformity item, grind well, get 0.8g, the accurate title, decide, and adds petroleum ether (60～90 ℃), extracts twice, each 10ml, centrifugal, discard petroleum ether, the residue hot wash, washing liquid is put in the 50ml volumetric flask, put coldly, add water to scale, supersound process (power: 250W; Frequency: 40KHz) 30 minutes, put to room temperature, filter, get subsequent filtrate and filter, promptly with 0.45 μ m filter membrane.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Salviae Miltiorrhizae with danshensu sodium (C
9H
10O
5Na) meter must not be less than 0.50mg.
The assay of Ginkgo total flavones is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Methanol-0.4% phosphoric acid solution (50: 50) is a mobile phase; The detection wavelength is 360nm.Number of theoretical plate calculates by the Quercetin peak should be not less than 2500.
The preparation of reference substance solution: accurate respectively Quercetin, kaempferol, the isorhamnetin reference substance that takes by weighing through the phosphorus pentoxide dried overnight is an amount of, add methanol respectively and make the mixed liquor that every 1ml contains 0.03mg, 0.03mg and 0.02mg, product solution (or is prepared Quercetin respectively and the every 1ml of kaempferol contains 0.1mg in contrast, the every 1ml of isorhamnetin contains the storing solution of 0.06mg, before facing usefulness, precision is measured each 1ml, mixing, promptly).
The preparation of need testing solution; Get the about 0.8g of content under this product content uniformity item, the accurate title, decide, and adds methanol-25% hydrochloric acid (4: 1) mixed liquor 25ml, puts in the water-bath and refluxed 30 minutes, put coldly, be filtered in the 50ml volumetric flask, add methanol to scale with absorbent cotton, shake up, with the microporous filter membrane filtration of 0.45 μ m, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate the content of three kinds of flavonol glycosides respectively, by formula " total flavonoids content=(quercetin content+kaempferol content+isorhamnetin content) * 2.51 " calculates, promptly.
Every of this product contains the Semen Ginkgo total flavones in total flavonoids, must not be less than 2.0mg.
In the quality determining method of aforementioned lunar caustic heart and brain clearing soft capsule, described lunar caustic heart and brain clearing soft capsule is made according to following method: get Radix Notoginseng 30g and be ground into impalpable powder, it is standby that all the other are ground into coarse powder; Blumeae preparatum Tabellae is ground into impalpable powder; Bulbus Allii is extracted Oleum Bulbus Allii with steam distillation; Folium Ginkgo adds the alcohol reflux secondary, each 1.5 hours, merge extractive liquid, reclaims ethanol, adds water and leaves standstill 12 hours, filter, polyamide resin column on the filtrate, water, ethanol elution are collected ethanol elution and are concentrated into the clear paste that relative density is 1.20 (50～60 ℃) successively, drying under reduced pressure is ground into impalpable powder.Radix Salviae Miltiorrhizae adds the alcohol reflux secondary, and each 1.5 hours, filter, merging filtrate reclaims ethanol, and being concentrated into relative density is the clear paste of 1.20 (50～60 ℃), and drying under reduced pressure is ground into impalpable powder, and medicinal residues are standby.The mixture of Herba Erigerontis, Herb Gynostemmae Pentaphylli, Radix Salviae Miltiorrhizae decoction dregs and Fructus Crataegi and Radix Notoginseng coarse powder decocts with water secondary respectively, each 2 hours, filter, merging filtrate is after being evaporated to relative density and being the clear paste of 1.20 (50～60 ℃), adding ethanol respectively makes and contains alcohol amount and reach 50%, 60%, 70%, stir evenly, left standstill 24 hours, get supernatant, reclaim ethanol, concentrate, drying is ground into impalpable powder; With the impalpable powder mix homogeneously of above-mentioned medical material and extractum, add in the vegetable oil with Oleum Bulbus Allii and Cera Flava, sorbic acid, fully mix and stir, make suspension, be pressed into soft capsule, promptly.
Compared with prior art, the present invention has improved the TCL discrimination method to Radix Notoginseng on existing quality standard basis, replenished that the TCL of tanshinone and Herba Erigerontis differentiates in the Radix Salviae Miltiorrhizae, improved the content assaying method of Radix Salviae Miltiorrhizae, increased assay Ginkgo total flavones.Can carry out more effective control to the main ingredient of lunar caustic heart and brain clearing soft capsule, make the quality monitoring level of lunar caustic heart and brain clearing soft capsule be greatly improved.Application of the present invention, both more help manufacturer and supervisory and management department to the monitoring of product quality, also can provide better guarantee for medical department and patient's treatment.
The specific embodiment
The quality determining method of lunar caustic heart and brain clearing soft capsule, calculate according to weight, lunar caustic heart and brain clearing soft capsule is to make 1000 seed lac wafers with Folium Ginkgo 500g, Radix Salviae Miltiorrhizae 500g, Herba Erigerontis 300g, Herb Gynostemmae Pentaphylli 300g, Fructus Crataegi 400g, Bulbus Allii 400g, Radix Notoginseng 200g, Blumeae preparatum Tabellae 10g; It is characterized in that this quality determining method may further comprise the steps:
Character: this product (lunar caustic heart and brain clearing soft capsule) is a soft capsule, and content is brown to tan paste; The gas suffering, mildly bitter flavor.
Differentiate: (1) gets this product content 1g, adds water 20ml stirring and makes molten loosing, with petroleum ether (30～60 ℃) extracting twice, each 20ml, discard petroleum ether layer, water layer extracted with diethyl ether 3 times, each 20ml, merge ether solution, water-bath volatilizes, and residue adds ethyl acetate 2ml, stirs, leave standstill, get supernatant as need testing solution.Other gets the tanshinone reference substance, adds ethyl acetate and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005).Drawing each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate-petroleum ether (30～60 ℃) (18: 1: 1), launches, and takes out, and dries.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the kermesinus speckle of same color.
(2) get this product content 2g, add petroleum ether (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant, residue add methanol 20ml, and reflux 15 minutes is put cold, filter, filtrate evaporate to dryness, residue add water 20ml, and slight fever makes dissolving, add water saturated n-butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with ammonia solution 25ml washing, discard ammonia solution, the saturated water washing of reuse n-butyl alcohol 2 times, each 25ml, n-butyl alcohol liquid is concentrated into dried, and residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Notoginseng control medicinal material 0.5g, adds about 5 of water, stirs evenly, add methanol 20ml, reflux 15 minutes is put cold, filter, filtrate evaporate to dryness, residue add water 20ml, slight fever makes dissolving, adds water saturated n-butyl alcohol 25ml, and jolting is extracted, get n-butanol extracting liquid, use the saturated water washing of n-butyl alcohol 2 times, each 25ml, n-butyl alcohol liquid is concentrated into dried, and residue adds methanol 1ml makes dissolving, in contrast medical material solution.Get arasaponin R1 again, add methanol and make 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 2005 B), draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, placing stratified lower floor solution below 10 ℃ with chloroform-methanol-water (13: 7: 2) is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing in 105 ℃, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get this product content 1.5g, add petroleum ether (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant, residue add 50% ethanol 30ml, reflux, extract, 30 minutes, filter, filtrate is waved to there not being the alcohol flavor, and residue adds the dissolving of water 20ml slight fever, filter while hot, cooling, filtrate is transferred pH value to 1～2 with hydrochloric acid, reuse ethyl acetate extraction 2 times, each 15ml, combined ethyl acetate liquid, volatilize, residue adds methanol 1ml dissolving, as need testing solution.Other gets Herba Erigerontis control medicinal material 1g, from adding 50% ethanol 30ml, shines medical material solution in pairs with legal system.Get the scutellarin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 2 μ l of above-mentioned three kinds of solution, ribbon is put on same polyamide film respectively, is developing solvent with glacial acetic acid ethanol (4: 1), launches, take out, dry, spray is with 2% ferric chloride alcoholic solution, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
Check, should meet every regulation relevant under the capsule item (an appendix I of Chinese Pharmacopoeia version in 2005 L).
The assay of danshensu sodium is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water-acetic acid (5: 160: 1) is mobile phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the danshensu sodium peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the danshensu sodium reference substance, adds methanol and make the solution that every 1ml contains 32 μ g, promptly.
The preparation of need testing solution: get the content under this product content uniformity item, grind well, get 0.8g, the accurate title, decide, and adds petroleum ether (60～90 ℃), extracts twice, each 10ml, centrifugal, discard petroleum ether, the residue hot wash, washing liquid is put in the 50ml volumetric flask, put coldly, add water to scale, supersound process (power: 250W; Frequency: 40KHz) 30 minutes put to room temperature, filter, and get subsequent filtrate and filter with 0.45 μ m filter membrane, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, annotate
Go into chromatograph of liquid, measure, promptly.
Every of this product contains Radix Salviae Miltiorrhizae with danshensu sodium (C
9H
10O
5Na) meter must not be less than 0.50mg.
The assay of Ginkgo total flavones is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D)
Chromatographic condition and system suitability test; With octadecylsilane chemically bonded silica is filler; Methanol-0.4% phosphoric acid solution (50: 50) is a mobile phase; The detection wavelength is 360nm.Number of theoretical plate calculates by the Quercetin peak should be not less than 2500.
The preparation of reference substance solution: accurate respectively Quercetin, kaempferol, the isorhamnetin reference substance that takes by weighing through the phosphorus pentoxide dried overnight is an amount of, add methanol respectively and make the mixed liquor that every 1ml contains 0.03mg, 0.03mg and 0.02mg, product solution (or is prepared Quercetin respectively and the every 1ml of kaempferol contains 0.1mg in contrast, the every 1ml of isorhamnetin contains the storing solution of 0.06mg, before facing usefulness, precision is measured each 1ml, mixing, promptly).
The preparation of need testing solution; get the about 0.8g of content under this product content uniformity item; the accurate title decides, and adds methanol-25% hydrochloric acid (4: 1) mixed liquor 25ml, puts in the water-bath and refluxes 30 minutes; put cold; be filtered in the 50ml volumetric flask with absorbent cotton, add methanol to scale, shake up; the microporous filter membrane with 0.45 μ m filters, promptly.
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate the content of three kinds of flavonol glycosides respectively, by formula " total flavonoids content=(quercetin content+kaempferol content+isorhamnetin content) * 2.51 " calculates, promptly.
Every of this product contains the Semen Ginkgo total flavones in total flavonoids, must not be less than 2.0mg.
Described lunar caustic heart and brain clearing soft capsule is made according to following method: get Radix Notoginseng 30g and be ground into impalpable powder, it is standby that all the other are ground into coarse powder; Blumeae preparatum Tabellae is ground into impalpable powder; Bulbus Allii is extracted Oleum Bulbus Allii with steam distillation; Folium Ginkgo adds the alcohol reflux secondary, each 1.5 hours, merge extractive liquid, reclaims ethanol, adds water and leaves standstill 12 hours, filter, polyamide resin column on the filtrate, water, ethanol elution are collected ethanol elution and are concentrated into the clear paste that relative density is 1.20 (50～60 ℃) successively, drying under reduced pressure is ground into impalpable powder.Radix Salviae Miltiorrhizae adds the alcohol reflux secondary, and each 1.5 hours, filter, merging filtrate reclaims ethanol, and being concentrated into relative density is the clear paste of 1.20 (50～60 ℃), and drying under reduced pressure is ground into impalpable powder, and medicinal residues are standby.The mixture of Herba Erigerontis, Herb Gynostemmae Pentaphylli, Radix Salviae Miltiorrhizae decoction dregs and Fructus Crataegi and Radix Notoginseng coarse powder decocts with water secondary respectively, each 2 hours, filter, merging filtrate is after being evaporated to relative density and being the clear paste of 1.20 (50～60 ℃), adding ethanol respectively makes and contains alcohol amount and reach 50%, 60%, 70%, stir evenly, left standstill 24 hours, get supernatant, reclaim ethanol, concentrate, drying is ground into impalpable powder; With the impalpable powder mix homogeneously of above-mentioned medical material and extractum, add in the vegetable oil with Oleum Bulbus Allii and Cera Flava, sorbic acid, fully mix and stir, make suspension, be pressed into soft capsule, promptly.
Claims (3)
1. the quality determining method of lunar caustic heart and brain clearing soft capsule, calculate according to weight, lunar caustic heart and brain clearing soft capsule is to make 1000 seed lac wafers with Folium Ginkgo 500g, Radix Salviae Miltiorrhizae 500g, Herba Erigerontis 300g, Herb Gynostemmae Pentaphylli 300g, Fructus Crataegi 400g, Bulbus Allii 400g, Radix Notoginseng 200g, Blumeae preparatum Tabellae 10g; It is characterized in that this quality determining method may further comprise the steps:
Character: this product is a soft capsule, and content is brown to tan paste; The gas suffering, mildly bitter flavor;
Differentiate: (1) gets this product content 1g, adds water 20ml and stirs and make molten loosing, with twice of 30～60 ℃ petroleum ether extraction, each 20ml, discard petroleum ether layer, water layer extracted with diethyl ether 3 times, each 20ml, merge ether solution, water-bath volatilizes, and residue adds ethyl acetate 2ml, stirs, leave standstill, get supernatant as need testing solution; Other gets the tanshinone reference substance, adds ethyl acetate and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin layer chromatography; Drawing each 5～10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is developing solvent with benzene-ethyl acetate of 18: 1: 1-30～60 ℃ petroleum ether, launches, and takes out, and dries; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the kermesinus speckle of same color;
(2) get this product content 2g, add 30～60 ℃ of petroleum ether 20ml, jolting is left standstill, abandoning supernatant, residue add methanol 20ml, and reflux 15 minutes is put cold, filter, filtrate evaporate to dryness, residue add water 20ml, and slight fever makes dissolving, add water saturated n-butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with ammonia solution 25ml washing, discard ammonia solution, the saturated water washing of reuse n-butyl alcohol 2 times, each 25ml, n-butyl alcohol liquid is concentrated into dried, and residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Radix Notoginseng control medicinal material 0.5g, adds about 5 of water, stirs evenly, add methanol 20ml, reflux 15 minutes is put cold, filter, filtrate evaporate to dryness, residue add water 20ml, slight fever makes dissolving, adds water saturated n-butyl alcohol 25ml, and jolting is extracted, get n-butanol extracting liquid, use the saturated water washing of n-butyl alcohol 2 times, each 25ml, n-butyl alcohol liquid is concentrated into dried, and residue adds methanol 1ml makes dissolving, in contrast medical material solution; Get arasaponin R1 again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, placing stratified lower floor solution below 10 ℃ with chloroform-methanol-water of 13: 7: 2 is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to speckle colour developing in 105 ℃, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this product content 1.5g, add 30～60 ℃ of petroleum ether 20ml, jolting is left standstill, abandoning supernatant, residue add 50% ethanol 30ml, reflux, extract, 30 minutes, filter, filtrate is waved to there not being the alcohol flavor, and residue adds the dissolving of water 20ml slight fever, filter while hot, cooling, filtrate is transferred pH value to 1～2 with hydrochloric acid, reuse ethyl acetate extraction 2 times, each 15ml, combined ethyl acetate liquid, volatilize, residue adds methanol 1ml dissolving, as need testing solution; Other gets Herba Erigerontis control medicinal material 1g, from adding 50% ethanol 30ml, shines medical material solution in pairs with legal system; Get the scutellarin reference substance again, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of above-mentioned three kinds of solution, ribbon is put on same polyamide film respectively, is developing solvent with glacial acetic acid-ethanol of 4: 1, launches, take out, dry, spray is with 2% ferric chloride alcoholic solution, in the test sample chromatograph, with control medicinal material chromatograph and the corresponding position of reference substance chromatograph on, show the speckle of same color.
2. the quality determining method of lunar caustic heart and brain clearing soft capsule according to claim 1 is characterized in that, this quality determining method also comprises:
Check, should meet every regulation relevant under the capsule item;
The assay of danshensu sodium is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; Acetonitrile-water-acetic acid of 5: 160: 1 is mobile phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the danshensu sodium peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the danshensu sodium reference substance, adds methanol and make the solution that every 1ml contains 32 μ g, promptly;
The preparation of need testing solution: get the content under this product content uniformity item, grind well, get 0.8g, the accurate title, decide, add 60～90 ℃ of petroleum ether, extract twice, each 10ml, centrifugal, discard petroleum ether, the residue hot wash, washing liquid is put in the 50ml volumetric flask, puts coldly, adds water to scale, power is 250W, and frequency is the supersound process 30 minutes of 40KHz, puts to room temperature, filter, get subsequent filtrate and filter, promptly with 0.45 μ m filter membrane;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly;
Every of this product contains Radix Salviae Miltiorrhizae in danshensu sodium (C9H1005Na), must not be less than 0.50mg;
The assay of Ginkgo total flavones is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with octadecylsilane chemically bonded silica is filler; 50: 50 methanol-0.4% phosphoric acid solution is a mobile phase; The detection wavelength is 360nm; Number of theoretical plate calculates by the Quercetin peak should be not less than 2500;
The preparation of reference substance solution: accurate respectively Quercetin, kaempferol, the isorhamnetin reference substance that takes by weighing through the phosphorus pentoxide dried overnight is an amount of, adds methanol respectively and makes the mixed liquor that every 1ml contains 0.03mg, 0.03mg and 0.02mg, in contrast product solution; Or prepare Quercetin respectively and the every 1ml of kaempferol contains 0.1mg, the every 1ml of isorhamnetin contains the storing solution of 0.06mg, face with before, precision is measured each 1ml, mixing, product solution in contrast;
The preparation of need testing solution: get the about 0.8g of content under this product content uniformity item, the accurate title, decide, add 4: 1 methanol 25% hydrochloric acid mixed solution 25ml, put in the water-bath and to reflux 30 minutes, put coldly, be filtered in the 50ml volumetric flask with absorbent cotton, add methanol to scale, shake up, with the microporous filter membrane filtration of 0.45 μ m, promptly;
Algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, calculate the content of three kinds of flavonol glycosides respectively, by formula " total flavonoids content=(quercetin content+kaempferol content+isorhamnetin content) * 2.51 " calculates, promptly;
Every of this product contains the Semen Ginkgo total flavones in total flavonoids, must not be less than 2.0mg.
3. the quality determining method of lunar caustic heart and brain clearing soft capsule according to claim 1 and 2 is characterized in that, described lunar caustic heart and brain clearing soft capsule is made according to following method: get Radix Notoginseng 30g and be ground into impalpable powder, it is standby that all the other are ground into coarse powder; Blumeae preparatum Tabellae is ground into impalpable powder; Bulbus Allii is extracted Oleum Bulbus Allii with steam distillation; Folium Ginkgo adds the alcohol reflux secondary, each 1.5 hours, merge extractive liquid, reclaims ethanol, adds water and leaves standstill 12 hours, filter, polyamide resin column on the filtrate, water, ethanol elution successively, collecting ethanol elution, to be concentrated in the time of 50～60 ℃ relative density be 1.20 clear paste, drying under reduced pressure is ground into impalpable powder; Radix Salviae Miltiorrhizae adds the alcohol reflux secondary, and each 1.5 hours, filter, merging filtrate reclaims ethanol, is concentrated in the time of 50～60 ℃ relative density and is 1.20 clear paste, and drying under reduced pressure is ground into impalpable powder, and medicinal residues are standby; The mixture of Herba Erigerontis, Herb Gynostemmae Pentaphylli, Radix Salviae Miltiorrhizae decoction dregs and Fructus Crataegi and Radix Notoginseng coarse powder decocts with water secondary respectively, each 2 hours, filter, merging filtrate, be evaporated in the time of 50～60 ℃ relative density and be 1.20 clear paste after, adding ethanol respectively makes and contains alcohol amount and reach 50%, 60%, 70%, stir evenly, left standstill 24 hours, get supernatant, reclaim ethanol, concentrate, drying is ground into impalpable powder; With the impalpable powder mix homogeneously of above-mentioned medical material and extractum, in Oleum Bulbus Allii and Cera Flava and sorbic acid adding vegetable oil, fully mix and stir, make suspension, be pressed into soft capsule, promptly.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103454374A (en) * | 2013-08-29 | 2013-12-18 | 贵州维康药业有限公司 | Quality control method of bone rehabilitation medicine |
| CN103735603A (en) * | 2014-02-11 | 2014-04-23 | 武汉市元大生物科技有限公司 | Compound lipid-decreasing soft capsule and preparation method thereof |
| CN109521114A (en) * | 2018-11-30 | 2019-03-26 | 贵州百灵企业集团制药股份有限公司 | The detection method of main effects ingredient in Capsule YD |
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2009
- 2009-08-24 CN CN200910305974XA patent/CN101647942B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103454374A (en) * | 2013-08-29 | 2013-12-18 | 贵州维康药业有限公司 | Quality control method of bone rehabilitation medicine |
| CN103735603A (en) * | 2014-02-11 | 2014-04-23 | 武汉市元大生物科技有限公司 | Compound lipid-decreasing soft capsule and preparation method thereof |
| CN103735603B (en) * | 2014-02-11 | 2016-08-31 | 武汉市元大生物科技有限公司 | A kind of compound antihyperglycemic soft capsule and preparation method thereof |
| CN109521114A (en) * | 2018-11-30 | 2019-03-26 | 贵州百灵企业集团制药股份有限公司 | The detection method of main effects ingredient in Capsule YD |
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