CN102240366A - Quality detection method for preparation for vision rehabilitation - Google Patents
Quality detection method for preparation for vision rehabilitation Download PDFInfo
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- CN102240366A CN102240366A CN2011102362338A CN201110236233A CN102240366A CN 102240366 A CN102240366 A CN 102240366A CN 2011102362338 A CN2011102362338 A CN 2011102362338A CN 201110236233 A CN201110236233 A CN 201110236233A CN 102240366 A CN102240366 A CN 102240366A
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Abstract
The invention belongs to the technical field of traditional Chinese medicine, and in particular relates to a quality detection method for preparation for vision rehabilitation. The existing preparation process is comparatively complex, and part of medicines are extracted by warm immersion for the medicinal active components, so that the dissolution rate is lower, and correspondingly, the quality detection requirements are lower. The preparation for vision rehabilitation is prepared from antelope horn, puncturevine caltrop fruit, equisetum, chrysanthemum, plantain seed, self-heal, cassia seed, ginseng, cornel, dendrobium stem, wolfberry fruit, dodder, glossy privet fruit, abalone shell, coptis root, pipewort, fiveleaf akebia, prepared rehmannia root, Chinese yam, oriental waterplantain rhizome, tuckahoe, tree peony bark, rehmannia root and betel palm, and the preparation for vision rehabilitation has the main efficacies of nourishing the liver and kidney, nourishing yin, promoting production of body fluid, removing heat from the liver and improving eyesight. The invention also provides a preparation method and detection method of the preparation for vision rehabilitation, changes the warm immersion extraction method into a water decoction method, basically improves the dissolution rate of the active components and the contents of the active components in the preparation, simultaneously improves the corresponding quality detection standards, and better meets the requirements of modern medical treatment.
Description
The application belongs to and divides an application, and the applying date of original application is on November 13rd, 2009, and application number is 200910218938X, and patent name is a kind of preparation method and quality determining method thereof of Chinese medicine 'Fuming '.
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to a kind of detection method of Chinese medicine 'Fuming '.
Background technology
Its preparation method and quality determining method are improved recording on the sheet basis of recovering lost eyesight of " Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation " the 12, to improve content of effective, thereby raising curative effect, the function of said preparation cures mainly and is nourishing the liver and kidney, YIN nourishing and the production of body fluid promoting, liver heat removing and eyesight improving is used for glaucoma, just, mid-term cataract and diseases such as the photophobia photophobia that causes of the hepatic and renal YIN deficiency, blurred vision.The patent that retrieves similar ophthalmic preparation has a kind of preparation method of the eye subsides of recovering lost eyesight, and the patent No. is 200510012863; The preparation of compound mixture and the method for inspection thereof, the patent No. are 200610010950.
Summary of the invention
It is simple to the invention provides a kind of preparation method, and the preparation method of the Chinese medicine 'Fuming ' that preparation section is easy also provides a kind of quality determining method of convenient, fast and accurate Chinese medicine 'Fuming '.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of Chinese medicine 'Fuming ', its prescription is: Cornu Saigae Tataricae, Fructus Tribuli, the Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Spica Prunellae, Semen Cassiae, Radix Ginseng, Fructus Corni (processed), Herba Dendrobii, Fructus Lycii, Semen Cuscutae, Fructus Ligustri Lucidi, Concha Haliotidis, Rhizoma Coptidis, Flos Eriocauli, Caulis Akebiae, Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis, Poria, Cortex Moutan, Radix Rehmanniae, Semen Arecae, it is characterized in that: the preparation method of described preparation is: Fructus Tribuli in the prescription, the Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (processed), Radix Ginseng, Herba Dendrobii is ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, again with above-mentioned fine powder mixing, remaining Spica Prunellae, Fructus Lycii, Semen Cuscutae, Fructus Ligustri Lucidi, Concha Haliotidis, Rhizoma Coptidis, Flos Eriocauli, Caulis Akebiae, Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis, Poria, Cortex Moutan, Radix Rehmanniae and Semen Arecae are decocted with water secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15, temperature is 60 ℃ a clear paste, is prepared into concentrated pill or adds adjuvant to be prepared into tablet, granule or capsule.
A kind of quality determining method of Chinese medicine 'Fuming ' is characterized in that:
(1) gets this product, put microscopically and observe: peel fiber lignify, levels criss-cross arrangement; Plant skin palisade cells 1 row, the side is seen and is rectangle, visible light line; Contain siliceous of tiny circle in the fiber surface similar round cell, be arranged in rows;
(2) get this product 4.5g, porphyrize, add methanol 40ml, supersound process 25 minutes filters, filtrate is added on the neutral alumina post that internal diameter is 1cm, used neutral alumina weight is that 10g, fineness are the 100-200 order, collects eluent, puts to steam in the water-bath near and does, add methanol 1ml and make dissolving, as need testing solution; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw each 4 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene: ethyl acetate: methanol: isopropyl alcohol: the volume ratio of strong ammonia solution is that 6:3:2.5:1.5:1 is developing solvent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, exhibition is taken out apart from about 15cm, dries, put under the 365nm ultraviolet light and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get this product 7.5g, porphyrize adds methanol 30ml, flooded 1 hour, jolting constantly filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, reflux 30 minutes, ether extraction 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, add methanol and make the solution that every 1ml contains 1mg, product solution in contrast, test according to thin layer chromatography, draw each 5 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be 30-60 ℃ petroleum ether with the temperature: Ethyl formate: the volume ratio of formic acid is that 20:5:0.5 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) Jian assay
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile: the volume ratio of 0.05% phosphoric acid solution is 39:61, is mobile phase; The detection wavelength is 349nm, and number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
The preparation of reference substance solution gets that the Jian reference substance an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 6 g, promptly;
This product 7.5g is got in the preparation of need testing solution, and accurate the title decided porphyrize, get about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate adding volume ratio is the hydrochloric acid of 1:100: the close plug of methyl alcohol mixed liquor 50ml claims to decide weight, supersound process 30 minutes, take out, put coldly, claim to decide weight again, hydrochloric acid with volume ratio 1:100: methyl alcohol mixed liquor is supplied the weight that subtracts mistake, shakes up, and filters, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure the content of berberine hydrochloride in the calculation sample;
The used adjuvant of preparation tablet is polyvidone and magnesium stearate.
The used adjuvant of preparation granule is dextrin and stevioside.
The used adjuvant of preparation capsule is a starch.
The every 0.3g of described Chinese medicine preparation contains Rhizoma Coptidis in berberine hydrochloride, is no less than 50 g.
Beneficial effect of the present invention: the present invention mainly provides a kind of preparation method and quality determining method of Chinese medicine 'Fuming ', fundamentally improved the dissolution of effective ingredient, and content of effective, also improved simultaneously its corresponding quality inspection standard, better met the demand of modern medical service, the existing preparation method of preparation method is simple, has simplified preparation section, has invented than initial quality on the basis of this preparation method and has marked convenient, fast and accurate quality determining method.
The specific embodiment
Laboratory report
1, purpose: carry out assay relatively by Cortex Moutan, Rhizoma Coptidis, Flos Eriocauli, Semen Arecae four Chinese medicine being decocted with water, thereby determine that the preparation method that adopts Cortex Moutan, Rhizoma Coptidis, Flos Eriocauli, Semen Arecae four Chinese medicine to decoct with water is more superior with two kinds of prepared 'Fuming 's of Different Extraction Method of warm macerating.
2, experimental technique:
(1) sample preparation
'Fuming ' preparation method one
20 four Chinese medicines in the prescription, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (system), Radix Ginseng, Herba Dendrobii are ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, again with above-mentioned fine powder mixing.Ten five tastes such as all the other Fructus Lycii decoct with water secondary, each 2 hours, decocting liquid filters, filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear paste, be prepared into concentrated pill or add appropriate amount of auxiliary materials and be prepared into regular dosage forms such as tablet, granule or capsule;
'Fuming ' preparation method two
In the prescription 24 flavors, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (system), Herba Dendrobii be ground into fine powder, sieve, mixing.Cornu Saigae Tataricae, Radix Ginseng are ground into fine powder separately, again with above-mentioned fine powder mixing.Fructus Lycii etc. ten decoct with water twice simply, each two hours.Cortex Moutan, Rhizoma Coptidis, Flos Eriocauli, Semen Arecae four Chinese medicine add water temperature and soak twice, each two hours.Collecting decoction filters, and being evaporated to relative density is 1.12-1.15(60 ℃) clear paste, with above-mentioned medicated powder and extractum granulation, be prepared into concentrated pill or add appropriate amount of auxiliary materials and be prepared into regular dosage forms such as tablet, granule or capsule;
According to above-mentioned two kinds of preparation methoies, every kind of dosage form prepares 3 batches respectively, uses for assay.
(2) assay
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g dodecyl sodium sulfate) is mobile phase; The detection wavelength is 349nm.Number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
It is an amount of that the Jian reference substance is got in the preparation of reference substance solution, and accurate the title decides, and adds methanol and makes the solution that every 1ml contains 6 g, promptly;
'Fuming ' 7.5g is got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate hydrochloric acid-methanol (1:100) 50ml that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes, take out, put cold, claim to decide weight, (1:100) supplies the weight that subtracts mistake with hydrochloric acid-methanol, shakes up again, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, that is, the every 0.3g of this product contains Rhizoma Coptidis in berberine hydrochloride, must not be less than 50 g.
3, measurement result
(1) ball of recovering lost eyesight
(2) sheet of recovering lost eyesight
(3) granule of recovering lost eyesight
(4) capsule of recovering lost eyesight
4, conclusion
Contrast from the said determination result, the content that can draw berberine hydrochloride in the 'Fuming ' of employing method one preparation is significantly higher than the content of the Jian in the 'Fuming ' that adopts the method two preparation, so can determine that 'Fuming ' preparation method one is better than 'Fuming ' preparation method two, can determine that promptly the extraction process that Cortex Moutan, Rhizoma Coptidis, Flos Eriocauli, Semen Arecae four Chinese medicine decoct with water is better than the technology that its four flavors warm macerating extracts.
Embodiment 1
The ball preparation method of recovering lost eyesight:
20 four Chinese medicines in the prescription, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (system), Radix Ginseng, Herba Dendrobii are ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, and with above-mentioned fine powder mixing, ten five tastes such as all the other Fructus Lycii decoct with water secondary again, and each 2 hours, decocting liquid filtered, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear paste, be prepared into concentrated pill.
The ball detection method of recovering lost eyesight:
(1) getting this product microscopically observes: peel fiber lignify, levels criss-cross arrangement; Plant skin palisade cells 1 row, the side is seen and is rectangle, visible light line; Contain siliceous of tiny circle in the fiber surface similar round cell, be arranged in rows;
(2) get this product 4.5g, porphyrize adds methanol 40ml, supersound process 25 minutes, filter, filtrate is added on the neutral alumina post (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath and do, add methanol 1ml and make dissolving, as need testing solution near.Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin layer chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively in same be that (6:3:2.5:1.5:1) is developing solvent with toluene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, exhibition is taken out apart from about 15cm, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get this product 7.5g, porphyrize adds methanol 30ml, flooded 1 hour, jolting constantly filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, reflux 30 minutes, ether extraction 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (20:5:0.5) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) assay of Jian
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g dodecyl sodium sulfate) is mobile phase; The detection wavelength is 349nm.Number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
The preparation of reference substance solution gets that the Jian reference substance an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 6 g, promptly;
This product 7.5g is got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate hydrochloric acid-methanol (1:100) 50ml that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes, take out, put cold, claim to decide weight, (1:100) supplies the weight that subtracts mistake with hydrochloric acid-methanol, shakes up again, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and the result is as follows:
Embodiment 2
The piece preparation method of recovering lost eyesight:
20 four Chinese medicines in the prescription, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (system), Radix Ginseng, Herba Dendrobii are ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, again with above-mentioned fine powder mixing.Ten five tastes such as all the other Fructus Lycii, decoct with water secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear paste, mixing fine powder and 15g polyvidone mix homogeneously, concentrate the clear paste spray granulation with gained, granule and magnesium stearate 1.5g always mix, and make tablet.
The chip detection method of recovering lost eyesight:
(1) getting this product microscopically observes: peel fiber lignify, levels criss-cross arrangement; Plant skin palisade cells 1 row, the side is seen and is rectangle, visible light line; Contain siliceous of tiny circle in the fiber surface similar round cell, be arranged in rows;
(2) get this product 4.5g, porphyrize adds methanol 40ml, supersound process 25 minutes, filter, filtrate is added on the neutral alumina post (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath and do, add methanol 1ml and make dissolving, as need testing solution near.Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin layer chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively in same be that (6:3:2.5:1.5:1) is developing solvent with toluene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, exhibition is taken out apart from about 15cm, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get this product 7.5g, porphyrize adds methanol 30ml, flooded 1 hour, jolting constantly filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, reflux 30 minutes, ether extraction 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (20:5:0.5) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) assay of Jian
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g dodecyl sodium sulfate) is mobile phase; The detection wavelength is 349nm.Number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
The preparation of reference substance solution gets that the Jian reference substance an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 6 g, promptly;
This product 7.5g is got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate hydrochloric acid-methanol (1:100) 50ml that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes, take out, put cold, claim to decide weight, (1:100) supplies the weight that subtracts mistake with hydrochloric acid-methanol, shakes up again, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and the result is as follows:
Embodiment 3
The preparation method of granules of recovering lost eyesight:
20 four Chinese medicines in the prescription, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (system), Radix Ginseng, Herba Dendrobii are ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, again with above-mentioned fine powder mixing.Ten five tastes such as all the other Fructus Lycii decoct with water secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear paste, mixing fine powder and 300g dextrin and 5g stevioside mix homogeneously concentrate the clear paste spray granulation with gained, make granule.
The particle detection of recovering lost eyesight method:
(1) getting this product microscopically observes: peel fiber lignify, levels criss-cross arrangement; Plant skin palisade cells 1 row, the side is seen and is rectangle, visible light line; Contain siliceous of tiny circle in the fiber surface similar round cell, be arranged in rows;
(2) get this product 4.5g, porphyrize adds methanol 40ml, supersound process 25 minutes, filter, filtrate is added on the neutral alumina post (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath and do, add methanol 1ml and make dissolving, as need testing solution near.Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin layer chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively in same be that (6:3:2.5:1.5:1) is developing solvent with toluene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, exhibition is taken out apart from about 15cm, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get this product 7.5g, porphyrize adds methanol 30ml, flooded 1 hour, jolting constantly filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, reflux 30 minutes, ether extraction 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (20:5:0.5) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) assay of Jian
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g dodecyl sodium sulfate) is mobile phase; The detection wavelength is 349nm.Number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
The preparation of reference substance solution gets that the Jian reference substance an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 6 g, promptly;
This product 7.5g is got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate hydrochloric acid-methanol (1:100) 50ml that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes, take out, put cold, claim to decide weight, (1:100) supplies the weight that subtracts mistake with hydrochloric acid-methanol, shakes up again, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and the result is as follows:
Embodiment 4
The capsule preparation method thereof of recovering lost eyesight:
20 four Chinese medicines in the prescription, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Semen Cassiae, Fructus Corni (system), Radix Ginseng, Herba Dendrobii are ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, again with above-mentioned fine powder mixing.Ten five tastes such as all the other Fructus Lycii decoct with water secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear paste, mixing fine powder and 1.5g starch mix homogeneously concentrate the clear paste spray granulation with gained, make capsule.
The capsule detection method of recovering lost eyesight:
(1) getting this product microscopically observes: peel fiber lignify, levels criss-cross arrangement; Plant skin palisade cells 1 row, the side is seen and is rectangle, visible light line; Contain siliceous of tiny circle in the fiber surface similar round cell, be arranged in rows;
(2) get this product 4.5g, porphyrize adds methanol 40ml, supersound process 25 minutes, filter, filtrate is added on the neutral alumina post (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath and do, add methanol 1ml and make dissolving, as need testing solution near.Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin layer chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively in same be that (6:3:2.5:1.5:1) is developing solvent with toluene-ethyl acetate-methanol-isopropyl alcohol-strong ammonia solution on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, exhibition is taken out apart from about 15cm, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get this product 7.5g, porphyrize adds methanol 30ml, flooded 1 hour, jolting constantly filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, reflux 30 minutes, ether extraction 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the chrysophanol reference substance, adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with petroleum ether (30-60 ℃)-Ethyl formate-formic acid (20:5:0.5) is developing solvent, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) assay of Jian
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g dodecyl sodium sulfate) is mobile phase; The detection wavelength is 349nm.Number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
The preparation of reference substance solution gets that the Jian reference substance an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 6 g, promptly;
This product 7.5g is got in the preparation of need testing solution, and accurate the title decides, and porphyrize is got about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate hydrochloric acid-methanol (1:100) 50ml that adds, close plug claims to decide weight, supersound process (power 250W, frequency 40kHz) 30 minutes, take out, put cold, claim to decide weight, (1:100) supplies the weight that subtracts mistake with hydrochloric acid-methanol, shakes up again, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and the result is as follows:
Claims (2)
1. the quality determining method of a Chinese medicine 'Fuming ', described Chinese medicine 'Fuming ' prescription is: Cornu Saigae Tataricae, Fructus Tribuli, Herba Equiseti Hiemalis, Flos Chrysanthemi, Semen Plantaginis, Spica Prunellae, Semen Cassiae, Radix Ginseng, Fructus Corni (processed), Herba Dendrobii, Fructus Lycii, Semen Cuscutae, Fructus Ligustri Lucidi, Concha Haliotidis, Rhizoma Coptidis, Flos Eriocauli, Caulis Akebiae, Radix Rehmanniae Preparata, Rhizoma Dioscoreae, Rhizoma Alismatis, Poria, Cortex Moutan, Radix Rehmanniae, Semen Arecae
It is characterized in that: operating procedure is as follows:
(1) gets this product, put microscopically and observe: peel fiber lignify, levels criss-cross arrangement; Plant skin palisade cells 1 row, the side is seen and is rectangle, visible light line; Contain siliceous of tiny circle in the fiber surface similar round cell, be arranged in rows;
(2) get this product 4.5g, porphyrize, add methanol 40ml, supersound process 25 minutes filters, filtrate is added on the neutral alumina post that internal diameter is 1cm, used neutral alumina weight is that 10g, fineness are the 100-200 order, collects eluent, puts to steam in the water-bath near and does, add methanol 1ml and make dissolving, as need testing solution; Other gets the berberine hydrochloride reference substance, adds methanol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution; Test according to thin layer chromatography, draw each 4 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with toluene: ethyl acetate: methanol: isopropyl alcohol: the volume ratio of strong ammonia solution is that 6:3:2.5:1.5:1 is developing solvent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, exhibition is taken out apart from about 15cm, dries, put under the 365nm ultraviolet light and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(3) get this product 7.5g, porphyrize adds methanol 30ml, flooded 1 hour, jolting constantly filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, reflux 30 minutes, ether extraction 2 times are used in cooling immediately, each 20ml merges ether solution, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the chrysophanol reference substance, add methanol and make the solution that every 1ml contains 1mg, product solution in contrast, test according to thin layer chromatography, draw each 5 l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be 30-60 ℃ petroleum ether with the temperature: Ethyl formate: the volume ratio of formic acid is that 20:5:0.5 is developing solvent, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) Jian assay
Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile: the volume ratio of 0.05% phosphoric acid solution is 39:61, is mobile phase; The detection wavelength is 349nm, and number of theoretical plate calculates and should be not less than 2000 by the Jian peak;
The preparation of reference substance solution gets that the Jian reference substance an amount of, accurately claims surely, adds methanol and makes the solution that every 1ml contains 6 g, promptly;
This product 7.5g is got in the preparation of need testing solution, and accurate the title decided porphyrize, get about 2g, the accurate title, decide, and puts in the tool plug conical flask, accurate adding volume ratio is the hydrochloric acid of 1:100: the close plug of methyl alcohol mixed liquor 50ml claims to decide weight, supersound process 30 minutes, take out, put coldly, claim to decide weight again, hydrochloric acid with volume ratio 1:100: methyl alcohol mixed liquor is supplied the weight that subtracts mistake, shakes up, and filters, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each 10 l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure the content of berberine hydrochloride in the calculation sample.
2. the detection method of a kind of Chinese medicine 'Fuming ' according to claim 1 is characterized in that: the every 0.3g of described Chinese medicine preparation contains Rhizoma Coptidis in berberine hydrochloride, is no less than 50 g.
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| CN104365945A (en) * | 2014-11-27 | 2015-02-25 | 桂林瑞丰环保微生物应用研究所 | Health food with functions of refreshing mind and improving eyesight |
| CN106370749A (en) * | 2016-08-29 | 2017-02-01 | 鲁南厚普制药有限公司 | Quality detection method of ginseng basis-consolidating oral solution |
| CN113917041A (en) * | 2021-11-01 | 2022-01-11 | 湖南新汇制药股份有限公司 | Quality detection method for standard decoction of moutan bark |
| CN115684429A (en) * | 2022-11-17 | 2023-02-03 | 湖南易能生物医药有限公司 | Quality control method and application of traditional Chinese medicine composition containing rehmannia |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103207148A (en) * | 2013-04-17 | 2013-07-17 | 西安碑林药业股份有限公司 | Quality detection method for Chinese herbal preparation for treating glaucoma and early-middle period cataract |
| CN104365945A (en) * | 2014-11-27 | 2015-02-25 | 桂林瑞丰环保微生物应用研究所 | Health food with functions of refreshing mind and improving eyesight |
| CN106370749A (en) * | 2016-08-29 | 2017-02-01 | 鲁南厚普制药有限公司 | Quality detection method of ginseng basis-consolidating oral solution |
| CN113917041A (en) * | 2021-11-01 | 2022-01-11 | 湖南新汇制药股份有限公司 | Quality detection method for standard decoction of moutan bark |
| CN113917041B (en) * | 2021-11-01 | 2024-03-15 | 湖南新汇制药股份有限公司 | Quality detection method for cortex moutan standard decoction |
| CN115684429A (en) * | 2022-11-17 | 2023-02-03 | 湖南易能生物医药有限公司 | Quality control method and application of traditional Chinese medicine composition containing rehmannia |
| CN115684429B (en) * | 2022-11-17 | 2023-07-04 | 湖南易能生物医药有限公司 | Quality control method and application of traditional Chinese medicine composition containing rehmannia |
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