CN101647942B - Quality testing method of Yindanxinnaotong soft capsules - Google Patents
Quality testing method of Yindanxinnaotong soft capsules Download PDFInfo
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- CN101647942B CN101647942B CN200910305974XA CN200910305974A CN101647942B CN 101647942 B CN101647942 B CN 101647942B CN 200910305974X A CN200910305974X A CN 200910305974XA CN 200910305974 A CN200910305974 A CN 200910305974A CN 101647942 B CN101647942 B CN 101647942B
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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, supplements the 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 of treating the soft capsule (adopted name or nomenclature of drug lunar caustic heart and brain clearing soft capsule) of cardiovascular and cerebrovascular disease.
Background technology
That lunar caustic heart and brain clearing soft capsule has is promoting blood circulation and removing blood stasis, the function of promoting qi circulation and relieving pain, relieving dyspepsia.Be used for the obstruction of qi in the chest that qi depression to blood stasis causes, disease is seen pectoralgia, and is uncomfortable in chest, breathes hard palpitaition etc., coronary disease and angina pectoris, hyperlipidemia, cerebral arteriovenous malformation, apoplexy, apoplexy sequelae.Ginkgo leaf, the red sage root, pseudo-ginseng, erigeron breviscapus 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 reappearance that pseudo-ginseng is differentiated is bad, oozing property of ester composition (tanshinone IIA) and erigeron breviscapus in the red sage root is not carried out qualitative control.The content assaying method of the red sage root is not good in addition, Total Ginkgo Flavone-Glycoides content in the ginkgo leaf 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 administrative authority product monitoring.
The object of the invention can be realized through 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 process 1000 seed lac wafers with ginkgo leaf 500g, red sage root 500g, erigeron breviscapus 300g, gynostemma pentaphylla 300g, hawthorn 400g, garlic 400g, pseudo-ginseng 200g, Chinese mugwort sheet 10g; It is characterized in that this quality determining method may further comprise the steps:
Proterties: these article (lunar caustic heart and brain clearing soft capsule) are soft capsule, and content is brown to tan paste; Gas is hot, mildly bitter flavor.
Differentiate: these article content 1g is got in (1), and add water 20ml stirring and make molten loosing, with sherwood oil (30～60 ℃) extracted twice, each 20ml; Discard petroleum ether layer, water layer is with extracted with diethyl ether 3 times, each 20ml; Merge ether solution, water-bath volatilizes, and residue adds ethyl acetate 2ml; Stir, leave standstill, get supernatant as need testing solution.Other gets the tanshinone IIA reference substance, adds ethyl acetate and processes the solution that every 1ml contains 2mg, as reference substance solution.Test according to thin-layered 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 developping agent with benzene-ethyl acetate-sherwood oil (30～60 ℃) (18: 1: 1), launches, and takes out, and dries.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the kermesinus spot of same color.
(2) get these article content 2g, add sherwood oil (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant, and residue adds methyl alcohol 20ml; Reflux 15 minutes is put coldly, filters, and the filtrating evaporate to dryness, residue adds water 20ml, and low-grade fever makes dissolving; Add water saturated normal butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with ammonia solution 25ml washing, discards ammonia solution; Use the saturated water washing of normal butyl alcohol 2 times again, each 25ml, normal butyl alcohol liquid is concentrated into dried, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets pseudo-ginseng control medicinal material 0.5g, adds about 5 of water, stirs, and adds methyl alcohol 20ml, reflux 15 minutes; Put coldly, filter, the filtrating evaporate to dryness, residue adds water 20ml, and low-grade fever makes dissolving; Add water saturated normal butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with the saturated water washing of normal butyl alcohol 2 times; Each 25ml, normal butyl alcohol liquid is concentrated into dried, and residue adds methyl alcohol 1ml makes dissolving, as control medicinal material solution.Get notoginsenoside R again, add methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With 10 ℃ of lower floor's solution with the held layering of chloroform-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing in 105 ℃; In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
(3) get these article content 1.5g, add sherwood oil (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant; Residue adds 50% ethanol 30ml, and refluxing extraction 30 minutes filters, and filtrating is waved to there not being the alcohol flavor, and residue adds the dissolving of water 20ml low-grade fever; Filter while hot, cooling, filtrating is transferred pH value to 1～2 with hydrochloric acid, uses ethyl acetate extraction again 2 times, each 15ml; Combined ethyl acetate liquid volatilizes, and residue adds methyl alcohol 1ml dissolving, as need testing solution.Other gets erigeron breviscapus control medicinal material 1g, from adding 50% ethanol 30ml, shines medicinal material solution in pairs with legal system.Get the scutellarin reference substance again, add methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 2 μ l of above-mentioned three kinds of solution, ribbon is put on same polyamide film respectively; With glacial acetic acid-ethanol (4: 1) is developping agent, launches, and takes out; Dry, spray is with 2% ferric trichloride ethanolic solution, in the test sample chromatogram; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
In the quality determining method of above-mentioned lunar caustic heart and brain clearing soft capsule, also comprise:
Inspection should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 L) relevant under the capsule item.
The assay of Sodium Danshensu is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-water-acetate (5: 160: 1) is moving phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the Sodium Danshensu peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Sodium Danshensu reference substance, adds methyl alcohol and process the solution that every 1ml contains 32 μ g, promptly gets.
The preparation of need testing solution: get the content under these article content uniformity item, grind well, get 0.8g, the accurate title, decide; Add sherwood oil (60～90 ℃), extract twice, each 10ml is centrifugal; Discard sherwood oil, residue is used hot wash, and washing lotion is put in the 50ml volumetric flask; Put coldly, add water to scale, sonicated (power: 250W; Frequency: 40KHz) 30 minutes, put to room temperature, filter, get subsequent filtrate and filter with 0.45 μ m filter membrane, promptly get.
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
Every of these article contain the red sage root with Sodium Danshensu (C
9H
10O
5Na) meter must not be less than 0.50mg.
The assay of Total Ginkgo Flavone-Glycoides is measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.4% phosphoric acid solution (50: 50) is a moving 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, mountain naphthalene element, the Isorhamnetin reference substance that takes by weighing through the phosphorus pentoxide dried overnight is an amount of; Add methyl alcohol respectively and process the mixed liquor that every 1ml contains 0.03mg, 0.03mg and 0.02mg, (or prepare the plain every 1ml of Quercetin and mountain naphthalene respectively and contain 0.1mg, the every 1ml of Isorhamnetin contains the storing solution of 0.06mg as reference substance solution; Before facing usefulness; Precision is measured each 1ml, and mixing promptly gets).
The preparation of need testing solution; The about 0.8g of content under these article of getting content uniformity item, the accurate title, decide, and adds methyl alcohol-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 methyl alcohol to scale with absorbent cotton; Shake up, the miillpore filter filtration with 0.45 μ m promptly gets.
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing; Inject liquid chromatograph, measure, calculate the content of three kinds of flavonol glycosides respectively; By formula " total flavonoids content=(quercetin content+mountain naphthalene cellulose content+Isorhamnetin content) * 2.51 " calculates, and promptly gets.
Every of these article contain the ginkgo general flavone 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 processed according to following method: get pseudo-ginseng 30g and be ground into impalpable powder, it is subsequent use that all the other are ground into meal; The Chinese mugwort sheet is ground into impalpable powder; Garlic is extracted garlic oil with steam distillation; Ginkgo leaf adds the alcohol reflux secondary, each 1.5 hours, merges extract; Reclaim ethanol, add water and left standstill 12 hours, filter; Polyamide resin column on the filtrating, water, ethanol elution are collected ethanol eluate and are concentrated into the clear cream that relative density is 1.20 (50～60 ℃) successively; Drying under reduced pressure is ground into impalpable powder.The red sage root adds the alcohol reflux secondary, and each 1.5 hours, filter, merging filtrate reclaims ethanol, and being concentrated into relative density is the clear cream of 1.20 (50～60 ℃), and drying under reduced pressure is ground into impalpable powder, and the dregs of a decoction are subsequent use.The potpourri of erigeron breviscapus, gynostemma pentaphylla, the red sage root dregs of a decoction and hawthorn and pseudo-ginseng meal, the boiling secondary each 2 hours, filters respectively; Merging filtrate after being evaporated to relative density and being the clear cream of 1.20 (50～60 ℃), adds ethanol respectively and makes and contain the alcohol amount and reach 50%, 60%, 70%, stirs; Left standstill 24 hours, and got supernatant, reclaim ethanol; Concentrate, drying is ground into impalpable powder; The impalpable powder of above-mentioned medicinal material and medicinal extract is mixed, add in the vegetable oil, fully mix and stir, process suspension, be pressed into soft capsule, promptly get with garlic oil and beeswax, sorbic acid.
Compared with prior art; The present invention has improved the TCL discrimination method to pseudo-ginseng on existing quality standard basis; Replenished that the TCL of tanshinone IIA and erigeron breviscapus differentiates in the red sage root, improved the content assaying method of the red sage root, increased assay Total Ginkgo Flavone-Glycoides.Can more effectively control the main drug ingedient 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 better guarantee be provided for medical department and patient's treatment.
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 process 1000 seed lac wafers with ginkgo leaf 500g, red sage root 500g, erigeron breviscapus 300g, gynostemma pentaphylla 300g, hawthorn 400g, garlic 400g, pseudo-ginseng 200g, Chinese mugwort sheet 10g; It is characterized in that this quality determining method may further comprise the steps:
Proterties: these article (lunar caustic heart and brain clearing soft capsule) are soft capsule, and content is brown to tan paste; Gas is hot, mildly bitter flavor.
Differentiate: these article content 1g is got in (1), and add water 20ml stirring and make molten loosing, with sherwood oil (30～60 ℃) extracted twice, each 20ml; Discard petroleum ether layer, water layer is with extracted with diethyl ether 3 times, each 20ml; Merge ether solution, water-bath volatilizes, and residue adds ethyl acetate 2ml; Stir, leave standstill, get supernatant as need testing solution.Other gets the tanshinone IIA reference substance, adds ethyl acetate and processes the solution that every 1ml contains 2mg, as reference substance solution.Test according to thin-layered 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 developping agent with benzene-ethyl acetate-sherwood oil (30～60 ℃) (18: 1: 1), launches, and takes out, and dries.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the kermesinus spot of same color.
(2) get these article content 2g, add sherwood oil (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant, and residue adds methyl alcohol 20ml; Reflux 15 minutes is put coldly, filters, and the filtrating evaporate to dryness, residue adds water 20ml, and low-grade fever makes dissolving; Add water saturated normal butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with ammonia solution 25ml washing, discards ammonia solution; Use the saturated water washing of normal butyl alcohol 2 times again, each 25ml, normal butyl alcohol liquid is concentrated into dried, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets pseudo-ginseng control medicinal material 0.5g, adds about 5 of water, stirs, and adds methyl alcohol 20ml, reflux 15 minutes; Put coldly, filter, the filtrating evaporate to dryness, residue adds water 20ml, and low-grade fever makes dissolving; Add water saturated normal butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with the saturated water washing of normal butyl alcohol 2 times; Each 25ml, normal butyl alcohol liquid is concentrated into dried, and residue adds methyl alcohol 1ml makes dissolving, as control medicinal material solution.Get notoginsenoside R again, add methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution.According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With 10 ℃ of lower floor's solution with the held layering of chloroform-methanol-water (13: 7: 2) is developping agent, launches, and takes out; Dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing in 105 ℃; In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
(3) get these article content 1.5g, add sherwood oil (30～60 ℃) 20ml, jolting is left standstill, abandoning supernatant; Residue adds 50% ethanol 30ml, and refluxing extraction 30 minutes filters, and filtrating is waved to there not being the alcohol flavor, and residue adds the dissolving of water 20ml low-grade fever; Filter while hot, cooling, filtrating is transferred pH value to 1～2 with hydrochloric acid, uses ethyl acetate extraction again 2 times, each 15ml; Combined ethyl acetate liquid volatilizes, and residue adds methyl alcohol 1ml dissolving, as need testing solution.Other gets erigeron breviscapus control medicinal material 1g, from adding 50% ethanol 30ml, shines medicinal material solution in pairs with legal system.Get the scutellarin reference substance again, add methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 2 μ l of above-mentioned three kinds of solution, ribbon is put on same polyamide film respectively; With glacial acetic acid-ethanol (4: 1) is developping agent, launches, and takes out; Dry, spray is with 2% ferric trichloride ethanolic solution, in the test sample chromatogram; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color.
Inspection should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 L) relevant under the capsule item.
The assay of Sodium Danshensu is measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-water-acetate (5: 160: 1) is moving phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the Sodium Danshensu peak should be not less than 3000.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Sodium Danshensu reference substance, adds methyl alcohol and process the solution that every 1ml contains 32 μ g, promptly gets.
The preparation of need testing solution: get the content under these article content uniformity item, grind well, get 0.8g, the accurate title, decide; Add sherwood oil (60～90 ℃), extract twice, each 10ml is centrifugal; Discard sherwood oil, residue is used hot wash, and washing lotion is put in the 50ml volumetric flask; Put coldly, add water to scale, sonicated (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 get.
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, annotate
Go into liquid chromatograph, measure, promptly get.
Every of these article contain the red sage root with Sodium Danshensu (C
9H
10O
5Na) meter must not be less than 0.50mg.
The assay of Total Ginkgo Flavone-Glycoides is measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test; Use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol-0.4% phosphoric acid solution (50: 50) is a moving 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, mountain naphthalene element, the Isorhamnetin reference substance that takes by weighing through the phosphorus pentoxide dried overnight is an amount of; Add methyl alcohol respectively and process the mixed liquor that every 1ml contains 0.03mg, 0.03mg and 0.02mg, (or prepare the plain every 1ml of Quercetin and mountain naphthalene respectively and contain 0.1mg, the every 1ml of Isorhamnetin contains the storing solution of 0.06mg as reference substance solution; Before facing usefulness; Precision is measured each 1ml, and mixing promptly gets).
The about 0.8g of content under these article content uniformity item is got in the preparation of need testing solution, and accurate the title decides; Add methyl alcohol-25% hydrochloric acid (4: 1) mixed liquor 25ml, put in the water-bath and refluxed 30 minutes, put cold; Be filtered in the 50ml volumetric flask with absorbent cotton, add methyl alcohol, shake up to scale; Miillpore filter with 0.45 μ m filters, and promptly gets.
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing; Inject liquid chromatograph, measure, calculate the content of three kinds of flavonol glycosides respectively; By formula " total flavonoids content=(quercetin content+mountain naphthalene cellulose content+Isorhamnetin content) * 2.51 " calculates, and promptly gets.
Every of these article contain the ginkgo general flavone in total flavonoids, must not be less than 2.0mg.
Described lunar caustic heart and brain clearing soft capsule is processed according to following method: get pseudo-ginseng 30g and be ground into impalpable powder, it is subsequent use that all the other are ground into meal; The Chinese mugwort sheet is ground into impalpable powder; Garlic is extracted garlic oil with steam distillation; Ginkgo leaf adds the alcohol reflux secondary, each 1.5 hours, merges extract; Reclaim ethanol, add water and left standstill 12 hours, filter; Polyamide resin column on the filtrating, water, ethanol elution are collected ethanol eluate and are concentrated into the clear cream that relative density is 1.20 (50～60 ℃) successively; Drying under reduced pressure is ground into impalpable powder.The red sage root adds the alcohol reflux secondary, and each 1.5 hours, filter, merging filtrate reclaims ethanol, and being concentrated into relative density is the clear cream of 1.20 (50～60 ℃), and drying under reduced pressure is ground into impalpable powder, and the dregs of a decoction are subsequent use.The potpourri of erigeron breviscapus, gynostemma pentaphylla, the red sage root dregs of a decoction and hawthorn and pseudo-ginseng meal, the boiling secondary each 2 hours, filters respectively; Merging filtrate after being evaporated to relative density and being the clear cream of 1.20 (50～60 ℃), adds ethanol respectively and makes and contain the alcohol amount and reach 50%, 60%, 70%, stirs; Left standstill 24 hours, and got supernatant, reclaim ethanol; Concentrate, drying is ground into impalpable powder; The impalpable powder of above-mentioned medicinal material and medicinal extract is mixed, add in the vegetable oil, fully mix and stir, process suspension, be pressed into soft capsule, promptly get with garlic oil and beeswax, sorbic acid.
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 process 1000 seed lac wafers with ginkgo leaf 500g, red sage root 500g, erigeron breviscapus 300g, gynostemma pentaphylla 300g, hawthorn 400g, garlic 400g, pseudo-ginseng 200g, Chinese mugwort sheet 10g; It is characterized in that this quality determining method may further comprise the steps:
Proterties: these article are soft capsule, and content is brown to tan paste; Gas is hot, mildly bitter flavor;
Differentiate: these article content 1g is got in (1), and add water 20ml stirring and make molten loosing, with 30～60 ℃ petroleum ether extractions twice, each 20ml; Discard petroleum ether layer, water layer is with extracted with diethyl ether 3 times, each 20ml; Merge ether solution, water-bath volatilizes, and residue adds ethyl acetate 2ml; Stir, leave standstill, get supernatant as need testing solution; Other gets the tanshinone IIA reference substance, adds ethyl acetate and processes the solution that every 1ml contains 2mg, as reference substance solution; Test according to thin-layered 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 developping agent with benzene-ethyl acetate of 18: 1: 1-30～60 ℃ sherwood oil, launches, and takes out, and dries; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the kermesinus spot of same color;
(2) get these article content 2g, add 30～60 ℃ of sherwood oil 20ml, jolting is left standstill, abandoning supernatant, and residue adds methyl alcohol 20ml; Reflux 15 minutes is put coldly, filters, and the filtrating evaporate to dryness, residue adds water 20ml, and low-grade fever makes dissolving; Add water saturated normal butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with ammonia solution 25ml washing, discards ammonia solution; Use the saturated water washing of normal butyl alcohol 2 times again, each 25ml, normal butyl alcohol liquid is concentrated into dried, and residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets pseudo-ginseng control medicinal material 0.5g, adds about 5 of water, stirs, and adds methyl alcohol 20ml, reflux 15 minutes; Put coldly, filter, the filtrating evaporate to dryness, residue adds water 20ml, and low-grade fever makes dissolving; Add water saturated normal butyl alcohol 25ml, jolting is extracted, and gets n-butanol extracting liquid, with the saturated water washing of normal butyl alcohol 2 times; Each 25ml, normal butyl alcohol liquid is concentrated into dried, and residue adds methyl alcohol 1ml makes dissolving, as control medicinal material solution; Get notoginsenoside R again, add methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution; According to the thin-layered chromatography test, draw each 2～3 μ l of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate; With 10 ℃ of lower floor's solution with the held layering of chloroform-methanol-water of 13: 7: 2 is developping agent, launches, and takes out; Dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing in 105 ℃; In the test sample chromatogram, with control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot of same color;
(3) get these article content 1.5g, add 30～60 ℃ of sherwood oil 20ml, jolting is left standstill, abandoning supernatant; Residue adds 50% ethanol 30ml, and refluxing extraction 30 minutes filters, and filtrating is waved to there not being the alcohol flavor, and residue adds the dissolving of water 20ml low-grade fever; Filter while hot, cooling, filtrating is transferred pH value to 1～2 with hydrochloric acid, uses ethyl acetate extraction again 2 times, each 15ml; Combined ethyl acetate liquid volatilizes, and residue adds methyl alcohol 1ml dissolving, as need testing solution; Other gets erigeron breviscapus control medicinal material 1g, from adding 50% ethanol 30ml, shines medicinal material solution in pairs with legal system; Get the scutellarin reference substance again, add methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution; According to the thin-layered chromatography test, draw each 2 μ l of above-mentioned three kinds of solution, ribbon is put on same polyamide film respectively; With glacial acetic acid-ethanol of 4: 1 was developping agent, launched, and took out; Dry, spray is with 2% ferric trichloride ethanolic solution, in the test sample chromatogram; With control medicinal material chromatogram and the corresponding position of reference substance chromatogram on, show the spot 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:
Inspection, inspection should meet each item regulation relevant under an appendix IL of Chinese Pharmacopoeia version in 2005 the capsule item;
The assay of Sodium Danshensu is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; Acetonitrile-water-acetate of 5: 160: 1 is moving phase; The detection wavelength is 280nm; Number of theoretical plate calculates by the Sodium Danshensu peak should be not less than 3000;
The preparation of reference substance solution: it is an amount of that precision takes by weighing the Sodium Danshensu reference substance, adds methyl alcohol and process the solution that every 1ml contains 32 μ g, promptly gets;
The preparation of need testing solution: get the content under these article content uniformity item, grind well, get 0.8g, the accurate title, decide, and adds 60～90 ℃ of sherwood oils; Extract twice, each 10ml, centrifugal, discard sherwood oil, residue is used hot wash; Washing lotion is put in the 50ml volumetric flask, puts coldly, adds water to scale, and power is 250W, and frequency is the sonicated 30 minutes of 40KHz; Put to room temperature, filter, get subsequent filtrate and filter, promptly get with 0.45 μ m filter membrane;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get;
Every of these article contain the red sage root with Sodium Danshensu (C
9H
10O
5Na) meter must not be less than 0.50mg;
The assay of Total Ginkgo Flavone-Glycoides is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: use octadecylsilane chemically bonded silica to be filling agent; 50: 50 methyl alcohol-0.4% phosphoric acid solution is a moving 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, mountain naphthalene element, the Isorhamnetin reference substance that takes by weighing through the phosphorus pentoxide dried overnight is an amount of, adds methyl alcohol respectively and processes the mixed liquor that every 1ml contains 0.03mg, 0.03mg and 0.02mg, as reference substance solution; Or prepare the plain every 1ml of Quercetin and mountain naphthalene respectively and contain 0.1mg, the every 1ml of Isorhamnetin contains the storing solution of 0.06mg, face with before, precision is measured each 1ml, mixing is as reference substance solution;
The preparation of need testing solution: get the about 0.8g of content under these article content uniformity item, the accurate title, decide, and adds 4: 1 methyl alcohol-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 methyl alcohol to scale; Shake up, the miillpore filter filtration with 0.45 μ m promptly gets;
Determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing; Inject liquid chromatograph, measure, calculate the content of three kinds of flavonol glycosides respectively; By formula " total flavonoids content=(quercetin content+mountain naphthalene cellulose content+Isorhamnetin content) * 2.51 " calculates, and promptly gets;
Every of these article contain the ginkgo general flavone 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 processed according to following method: get pseudo-ginseng 30g and be ground into impalpable powder, it is subsequent use that all the other are ground into meal; The Chinese mugwort sheet is ground into impalpable powder; Garlic is extracted garlic oil with steam distillation; Ginkgo leaf adds the alcohol reflux secondary, each 1.5 hours, merges extract; Reclaim ethanol, add water and left standstill 12 hours, filter; Polyamide resin column on the filtrating, water, ethanol elution successively, collecting ethanol eluate, to be concentrated in the time of 50～60 ℃ relative density be 1.20 clear cream; Drying under reduced pressure is ground into impalpable powder; The red sage root 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 cream, and drying under reduced pressure is ground into impalpable powder, and the dregs of a decoction are subsequent use; The potpourri of erigeron breviscapus, gynostemma pentaphylla, the red sage root dregs of a decoction and hawthorn and pseudo-ginseng meal, the boiling secondary each 2 hours, filters respectively; Merging filtrate, be evaporated in the time of 50～60 ℃ relative density and be 1.20 clear cream after, add ethanol respectively and make and contain the alcohol amount and reach 50%, 60%, 70%, stir; Left standstill 24 hours, and got supernatant, reclaim ethanol; Concentrate, drying is ground into impalpable powder; The impalpable powder of above-mentioned medicinal material and medicinal extract is mixed, in garlic oil and beeswax and sorbic acid adding vegetable oil, fully mix and stir, process suspension, be pressed into soft capsule, promptly get.
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| 刘先琼等.净丹参及酒炙丹参的薄层鉴别研究.《湖北中医学院学报》.2006,第8卷(第03期),21-22. * |
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