CN102240366B - Quality detection method for preparation for vision rehabilitation - Google Patents
Quality detection method for preparation for vision rehabilitation Download PDFInfo
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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 preparation for vision rehabilitation.
Technical field
The invention belongs to technical field of traditional Chinese medicines, be specifically related to a kind of detection method of preparation for vision rehabilitation.
Background technology
Its preparation method and quality determining method are improved recording on the Fuming Tablet basis of " Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation " the 12, to improve the content of effective constituent, thereby raising curative effect, the function of said preparation cures mainly as nourishing liver and kidney, nourishing Yin and promoting production of body fluid, clear liver and improve vision, be used for glaucoma, just, mid-term cataract and the diseases such as the photophobia photophobia that causes of the deficiency of liver-yin and kidney-yin, blurred vision.It is 200510012863 that the patent that retrieves similar ophthalmic preparation has a kind of preparation method of the eye sticker of recovering lost eyesight, the patent No.; Preparation of compound mixture and the method for inspection thereof, the patent No. are 200610010950.
Summary of the invention
The invention provides a kind of preparation method simple, the preparation method of the preparation for vision rehabilitation that preparation section is easy also provides a kind of quality determining method of convenient, fast and accurate preparation for vision rehabilitation.
For achieving the above object, the technical solution used in the present invention is: a kind of preparation method of preparation for vision rehabilitation, its prescription is: antelope's horn, puncture vine, the scouring rush, chrysanthemum, plantain seed, selfheal, cassia seed, ginseng, Fructus Corni (processed), the stem of noble dendrobium, the fruit of Chinese wolfberry, the seed of Chinese dodder, the fruit of glossy privet, the shell of seaear, the coptis, pipewort, akebi, prepared rhizome of rehmannia, Chinese yam, rhizoma alismatis, Poria cocos, moutan bark, glutinous rehmannia, betel nut, it is characterized in that: the preparation method of described preparation is: puncture vine in the prescription, the scouring rush, chrysanthemum, plantain seed, cassia seed, Fructus Corni (processed), ginseng, the stem of noble dendrobium is ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, again with above-mentioned fine powder mixing, with remaining selfheal, the fruit of Chinese wolfberry, the seed of Chinese dodder, the fruit of glossy privet, the shell of seaear, the coptis, pipewort, akebi, prepared rhizome of rehmannia, Chinese yam, rhizoma alismatis, Poria cocos, moutan bark, glutinous rehmannia and betel nut boiling secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15, temperature is 60 ℃ clear cream, is prepared into condensed pill or adds auxiliary material to be prepared into tablet, granule or capsule.
A kind of quality determining method of preparation for vision rehabilitation is characterized in that:
(1) gets this product, put microscopically and observe: pericarp 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 methyl alcohol 40ml, ultrasonic processing 25 minutes filters, filtrate is added on the neutral alumina column 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 methyl alcohol 1ml and make dissolving, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution; Test according to thin-layered chromatography, draw each 4 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take toluene: ethyl acetate: methyl alcohol: isopropyl alcohol: the volume ratio of strong ammonia solution as 6:3:2.5:1.5:1 as developping agent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, the exhibition distance is 15cm approximately, takes out, and dries, put under the 365nm ultraviolet light and inspect, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product 7.5g, porphyrize adds methyl alcohol 30ml, flooded 1 hour, constantly jolting filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, added hot reflux 30 minutes, extracted by ether 2 times are used in immediately cooling, each 20ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the Chrysophanol reference substance, add methyl alcohol and make the solution that every 1ml contains 1mg, product solution in contrast, test according to thin-layered chromatography, draw each 5 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, sherwood oil take temperature as 30-60 ℃: ethyl formate: the volume ratio of formic acid is developping agent as 20:5:0.5, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(4) Yan Suan Xiao ?the assay of alkali
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: the volume ratio of 0.05% phosphoric acid solution is mobile phase as 39:61; The detection wavelength is 349nm, number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 g, and get final product;
This product 7.5g is got in the preparation of need testing solution, and is accurately weighed, porphyrize, get approximately 2g, accurately weighed, put 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, weighed weight, ultrasonic processing 30 minutes, take out, let cool, more weighed weight, hydrochloric acid with volume ratio 1:100: methyl alcohol mixed liquor is supplied the weight of less loss, shakes up, and filters, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 l of need testing solution of drawing respectively, and the injection liquid chromatography is measured the content of Berberine hydrochloride in the calculation sample;
The used auxiliary material of preparation tablet is polyvidone and dolomol.
The used auxiliary material of preparation granule is dextrin and stevioside.
The used auxiliary material of preparation capsule is starch.
The every 0.3g of described Chinese medicine preparation contains the coptis 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 preparation for vision rehabilitation, fundamentally improved the dissolution rate of effective constituent, content with effective constituent, 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 this preparation method's basis and has marked convenient, fast and accurate quality determining method.
Embodiment
Laboratory report
1, purpose: carry out assay relatively by moutan bark, the coptis, pipewort, the boiling of betel nut four traditional Chinese medicine and temperature being soaked two kinds of prepared 'Fuming 's of Different Extraction Method, thereby determine to adopt the preparation method of moutan bark, the coptis, pipewort, the boiling of betel nut four traditional Chinese medicine more superior.
2, experimental technique:
(1) sample preparation
'Fuming ' preparation method one
20 four traditional Chinese medicines in the prescription, puncture vine, scouring rush, chrysanthemum, plantain seed, cassia seed, the fruit of medicinal cornel (system), ginseng, the stem of noble dendrobium 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 fruits of Chinese wolfberry, boiling secondary, each 2 hours, decocting liquid filters, filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear cream, be prepared into condensed pill or add appropriate amount of auxiliary materials and be prepared into the regular dosage forms such as tablet, granule or capsule;
'Fuming ' preparation method two
In the prescription 24 flavors, puncture vine, scouring rush, chrysanthemum, plantain seed, cassia seed, the fruit of medicinal cornel (system), the stem of noble dendrobium be ground into fine powder, sieve, mixing.Antelope's horn, ginseng are ground into separately fine powder, again with above-mentioned fine powder mixing.The fruit of Chinese wolfberry etc. ten simply, boiling twice, each two hours.Moutan bark, the coptis, pipewort, betel nut four traditional 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 cream, with above-mentioned medicinal powder and medicinal extract granulation, be prepared into condensed pill or add appropriate amount of auxiliary materials and be prepared into the regular dosage forms such as tablet, granule or capsule;
According to above-mentioned two kinds of preparation methods, every kind of formulation prepares respectively 3 batches, for assay.
(2) assay
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g sodium dodecylsulphonate) as mobile phase; The detection wavelength is 349nm.Number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 g, and get final product;
'Fuming ' 7.5g is got in the preparation of need testing solution, and is accurately weighed, and porphyrize is got approximately 2g, accurately weighed, put in the tool plug conical flask accurate hydrochloric acid-methyl alcohol (1:100) 50ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40kHz) 30 minutes, take out, let cool, weighed weight is again supplied the weight of less loss with hydrochloric acid-methyl alcohol (1:100), shake up, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and be get final product, and the every 0.3g of this product contains the coptis in Berberine hydrochloride, must not be less than 50 g.
3, measurement result
(1) ball of recovering lost eyesight
(2) Fuming Tablet
(3) Fuming Granules
(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 be significantly higher than Yan Suan Xiao in the 'Fuming ' that adopts the method two preparation ?the content of alkali, be better than 'Fuming ' preparation method two therefore can determine 'Fuming ' preparation method one, can determine that namely the extraction process of moutan bark, the coptis, pipewort, the boiling of betel nut four traditional Chinese medicine is better than the technique that the warm lixiviate of its four flavor is got.
Embodiment 1
The ball preparation method recovers lost eyesight:
20 four traditional Chinese medicines in the prescription, puncture vine, scouring rush, chrysanthemum, plantain seed, cassia seed, the fruit of medicinal cornel (system), ginseng, the stem of noble dendrobium are ground into fine powder, sieve mixing; Cornu Saigae Tataricae powder is broken into fine powder, and again with above-mentioned fine powder mixing, ten five tastes such as all the other fruits of Chinese wolfberry, the boiling secondary, each 2 hours, decocting liquid filtered, filtrate merges, being evaporated to relative density is 1.12-1.15(60 ℃) clear cream, be prepared into condensed pill.
The ball detection method of recovering lost eyesight:
(1) getting this product microscopically observes: pericarp 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 methyl alcohol 40ml, ultrasonic processing 25 minutes, filter, filtrate is added on the neutral alumina column (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath near and do, add methyl alcohol 1ml and make dissolving, as need testing solution.Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (6:3:2.5:1.5:1) as developping agent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, the exhibition distance is 15cm approximately, takes out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product 7.5g, porphyrize adds methyl alcohol 30ml, flooded 1 hour, constantly jolting filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, added hot reflux 30 minutes, extracted by ether 2 times are used in immediately cooling, each 20ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets the Chrysophanol reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take sherwood oil (30-60 ℃)-ethyl formate-formic acid (20:5:0.5) as developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(4) Yan Suan Xiao ?the assay of alkali
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g sodium dodecylsulphonate) as mobile phase; The detection wavelength is 349nm.Number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 g, and get final product;
This product 7.5g is got in the preparation of need testing solution, and is accurately weighed, and porphyrize is got approximately 2g, accurately weighed, put in the tool plug conical flask accurate hydrochloric acid-methyl alcohol (1:100) 50ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40kHz) 30 minutes, take out, let cool, weighed weight is again supplied the weight of less loss with hydrochloric acid-methyl alcohol (1:100), shake up, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and the result is as follows:
Embodiment 2
The Fuming Tablet preparation method:
20 four traditional Chinese medicines in the prescription, puncture vine, scouring rush, chrysanthemum, plantain seed, cassia seed, the fruit of medicinal cornel (system), ginseng, the stem of noble dendrobium 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 fruits of Chinese wolfberry, the boiling secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear cream, mixing fine powder and 15g polyvidone mix, with the concentrated clear cream spraying granulation of gained, particle and dolomol 1.5g are always mixed, make tablet.
The Fuming Tablet detection method:
(1) getting this product microscopically observes: pericarp 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 methyl alcohol 40ml, ultrasonic processing 25 minutes, filter, filtrate is added on the neutral alumina column (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath near and do, add methyl alcohol 1ml and make dissolving, as need testing solution.Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (6:3:2.5:1.5:1) as developping agent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, the exhibition distance is 15cm approximately, takes out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product 7.5g, porphyrize adds methyl alcohol 30ml, flooded 1 hour, constantly jolting filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, added hot reflux 30 minutes, extracted by ether 2 times are used in immediately cooling, each 20ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets the Chrysophanol reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take sherwood oil (30-60 ℃)-ethyl formate-formic acid (20:5:0.5) as developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(4) Yan Suan Xiao ?the assay of alkali
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g sodium dodecylsulphonate) as mobile phase; The detection wavelength is 349nm.Number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 g, and get final product;
This product 7.5g is got in the preparation of need testing solution, and is accurately weighed, and porphyrize is got approximately 2g, accurately weighed, put in the tool plug conical flask accurate hydrochloric acid-methyl alcohol (1:100) 50ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40kHz) 30 minutes, take out, let cool, weighed weight is again supplied the weight of less loss with hydrochloric acid-methyl alcohol (1:100), shake up, filter, get subsequent filtrate, and get final product.
Determination method is accurate reference substance solution and each 10 l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and the result is as follows:
Embodiment 3
The preparation method of granules of recovering lost eyesight:
20 four traditional Chinese medicines in the prescription, puncture vine, scouring rush, chrysanthemum, plantain seed, cassia seed, the fruit of medicinal cornel (system), ginseng, the stem of noble dendrobium 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 fruits of Chinese wolfberry, boiling secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear cream, mixing fine powder and 300g dextrin and 5g stevioside mix, with the concentrated clear cream spraying granulation of gained, granulation agent.
The particle detection of recovering lost eyesight method:
(1) getting this product microscopically observes: pericarp 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 methyl alcohol 40ml, ultrasonic processing 25 minutes, filter, filtrate is added on the neutral alumina column (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath near and do, add methyl alcohol 1ml and make dissolving, as need testing solution.Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (6:3:2.5:1.5:1) as developping agent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, the exhibition distance is 15cm approximately, takes out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product 7.5g, porphyrize adds methyl alcohol 30ml, flooded 1 hour, constantly jolting filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, added hot reflux 30 minutes, extracted by ether 2 times are used in immediately cooling, each 20ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets the Chrysophanol reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take sherwood oil (30-60 ℃)-ethyl formate-formic acid (20:5:0.5) as developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(4) Yan Suan Xiao ?the assay of alkali
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g sodium dodecylsulphonate) as mobile phase; The detection wavelength is 349nm.Number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 g, and get final product;
This product 7.5g is got in the preparation of need testing solution, and is accurately weighed, and porphyrize is got approximately 2g, accurately weighed, put in the tool plug conical flask accurate hydrochloric acid-methyl alcohol (1:100) 50ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40kHz) 30 minutes, take out, let cool, weighed weight is again supplied the weight of less loss with hydrochloric acid-methyl alcohol (1:100), shake up, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and the result is as follows:
Embodiment 4
The capsule preparation method thereof of recovering lost eyesight:
20 four traditional Chinese medicines in the prescription, puncture vine, scouring rush, chrysanthemum, plantain seed, cassia seed, the fruit of medicinal cornel (system), ginseng, the stem of noble dendrobium 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 fruits of Chinese wolfberry, boiling secondary, each 2 hours, decocting liquid filters, and filtrate merges, and being evaporated to relative density is 1.12-1.15(60 ℃) clear cream, mixing fine powder and 1.5g starch mix, and with the concentrated clear cream spraying granulation of gained, make capsule.
The capsule detection method of recovering lost eyesight:
(1) getting this product microscopically observes: pericarp 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 methyl alcohol 40ml, ultrasonic processing 25 minutes, filter, filtrate is added on the neutral alumina column (100-200 order, 10g, internal diameter 1cm), collect eluent, put to steam in the water-bath near and do, add methyl alcohol 1ml and make dissolving, as need testing solution.Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution.Test according to thin-layered chromatography (an appendix VI of 2005 editions pharmacopeia B), draw each 4 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take toluene-ethyl acetate-methyl alcohol-isopropyl alcohol-strong ammonia solution (6:3:2.5:1.5:1) as developping agent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, the exhibition distance is 15cm approximately, takes out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product 7.5g, porphyrize adds methyl alcohol 30ml, flooded 1 hour, constantly jolting filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, added hot reflux 30 minutes, extracted by ether 2 times are used in immediately cooling, each 20ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution.Other gets the Chrysophanol reference substance, adds methyl alcohol and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (appendix VI B), draw each 5 l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take sherwood oil (30-60 ℃)-ethyl formate-formic acid (20:5:0.5) as developping agent, launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(4) Yan Suan Xiao ?the assay of alkali
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile-0.05% phosphoric acid solution (39:61) (every 100ml adds the 0.05g sodium dodecylsulphonate) as mobile phase; The detection wavelength is 349nm.Number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 g, and get final product;
This product 7.5g is got in the preparation of need testing solution, and is accurately weighed, and porphyrize is got approximately 2g, accurately weighed, put in the tool plug conical flask accurate hydrochloric acid-methyl alcohol (1:100) 50ml that adds, close plug, weighed weight, ultrasonic processing (power 250W, frequency 40kHz) 30 minutes, take out, let cool, weighed weight is again supplied the weight of less loss with hydrochloric acid-methyl alcohol (1:100), shake up, filter, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 l of need testing solution of drawing respectively, and the injection liquid chromatography is measured, and the result is as follows:
Claims (1)
1. the quality determining method of a preparation for vision rehabilitation, described preparation for vision rehabilitation prescription is: antelope's horn, puncture vine, scouring rush, chrysanthemum, plantain seed, selfheal, cassia seed, ginseng, Fructus Corni (processed), the stem of noble dendrobium, the fruit of Chinese wolfberry, the seed of Chinese dodder, the fruit of glossy privet, the shell of seaear, the coptis, pipewort, akebi, prepared rhizome of rehmannia, Chinese yam, rhizoma alismatis, Poria cocos, moutan bark, glutinous rehmannia, betel nut
It is characterized in that: operation steps is as follows:
(1) gets this product, put microscopically and observe: pericarp 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 methyl alcohol 40ml, ultrasonic processing 25 minutes filters, filtrate is added on the neutral alumina column 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 methyl alcohol 1ml and make dissolving, as need testing solution; Other gets the Berberine hydrochloride reference substance, adds methyl alcohol and makes the solution that contains 0.5mg among every 1ml, in contrast product solution; Test according to thin-layered chromatography, draw each 4 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, take toluene: ethyl acetate: methyl alcohol: isopropyl alcohol: the volume ratio of strong ammonia solution as 6:3:2.5:1.5:1 as developping agent, put in the expansion cylinder of ammonia saturated with vapor, presaturation 15 minutes, launch, the exhibition distance is 15cm approximately, takes out, and dries, put under the 365nm ultraviolet light and inspect, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(3) get this product 7.5g, porphyrize adds methyl alcohol 30ml, flooded 1 hour, constantly jolting filters, filtrate evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again, added hot reflux 30 minutes, extracted by ether 2 times are used in immediately cooling, each 20ml merges ether solution, evaporate to dryness, residue adds methyl alcohol 1ml makes dissolving, as need testing solution; Other gets the Chrysophanol reference substance, add methyl alcohol and make the solution that every 1ml contains 1mg, product solution in contrast, test according to thin-layered chromatography, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate take sodium carboxymethyl cellulose as binder, sherwood oil take temperature as 30-60 ℃: ethyl formate: the volume ratio of formic acid is developping agent as 20:5:0.5, launch, take out, dry, put under the 365nm ultraviolet lamp and inspect, in the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the fluorescence spot of aobvious same color;
(4) Yan Suan Xiao ?the assay of alkali
Chromatographic condition and system suitability are take octadecylsilane chemically bonded silica as filling agent; Take acetonitrile: the volume ratio of 0.05% phosphoric acid solution is mobile phase as 39:61; The detection wavelength is 349nm, number of theoretical plate by Yan Suan Xiao ?the alkali peak calculate and should be not less than 2000;
It is an amount of, accurately weighed that the little ?alkali reference substance of salt acid is got in the preparation of reference substance solution, adds methyl alcohol and make the solution that every 1ml contains 6 μ g, and get final product;
This product 7.5g is got in the preparation of need testing solution, and is accurately weighed, porphyrize, get approximately 2g, accurately weighed, put 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, weighed weight, ultrasonic processing 30 minutes, take out, let cool, more weighed weight, hydrochloric acid with volume ratio 1:100: methyl alcohol mixed liquor is supplied the weight of less loss, shakes up, and filters, get subsequent filtrate, and get final product;
Determination method is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and the injection liquid chromatography is measured the content of Berberine hydrochloride in the calculation sample.
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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 |
| 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 |
| 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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