CN102038785B - Detection method for traditional Chinese medicinal preparation of children eyesight pills - Google Patents
Detection method for traditional Chinese medicinal preparation of children eyesight pills Download PDFInfo
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Abstract
The invention relates to a quality control method for a traditional Chinese medicinal preparation of children eyesight pills, which comprises the following steps of: firstly, performing characteristic and microscopical identification; secondly, identifying whether a prescription for the children eyesight pills contains golden thread, rhubarb, baical skullcap root and cape jasmine fruit components by adopting thin layer chromatography; and finally, measuring the content of red paeony root in the prescription of the galactagogue pills by taking paeoniflorin as a reference substance through high performance liquid chromatography. On the basis of the original standard, the microscopical identification method for the baical skullcap root, the cape jasmine fruit, the rhubarb, honeysuckle and liquorice in the prescription is increased; meanwhile, the thin layer identification method for the baical skullcap root, the cape jasmine fruit, the rhubarb and the golden thread is increased; by taking the paeoniflorin as the reference substance, the method for measuring the content of the red paeony root is formulated; and the revised method can more accurately test quack medicines and inferior medicines and has important significance for modernizing traditional Chinese medicines and making the traditional Chinese medicines spread to the world.
Description
Technical field
The invention belongs to technical field of traditional Chinese medicines, relate to the detection method of Chinese medicine, especially a kind of method of quality control of Chinese medicine preparation children's pills for improving acuity of sight.
Background technology
Children's's pills for improving acuity of sight is made up of the radix paeoniae rubrathe, the root of large-flowered skullcap, cape jasmine, root of Chinese trichosanthes, rheum officinale, honeysuckle, chrysanthemum, plantain seed (salt system), the coptis, peppermint, Radix Glycyrrhizae, and its preparation method is: above ten simply, is ground into fine powder; Sieve, mixing, every 100g powder add refined honey 150～170g and process big honeyed pills and promptly get; Children's's pills for improving acuity of sight has removing heat to brighten vision, and the antipruritic effect of wind of loosing is used for part of the body cavity above the diaphragm housing the heart and lungs heat and contains; Eyes were puffy and red, the painful uneasiness of itching, difficulty in urination and defecation.
Though still there is not the international standard of plant medicine at present in the world; The trend of Chinese medicine standard but the south east asia of the U.S., European Union, China and tradition outlet Chinese medicine is improved; In the case, the standard that needs to propose to be fit to China's product quality is to adapt to international standard, and it is historical that China has the Chinese medicine in thousands of years to use; Countries in the world are many Chinese medicine standards with reference to China in working out corresponding autonomic drug target level of product quality, so quality standard perfect, that improve Chinese medicine is more extremely urgent.
The existing quality standard of children's's pills for improving acuity of sight does not have the concrete authentication method about each composition; Just describe from microstructure; The qualitative and quantitative detection that is unfavorable for so very much this medicine brings very big difficulty for the quality control of this medicine, according to retrieval; Do not have the related patent U.S. Patent No. about the method for quality control of children's's pills for improving acuity of sight at present, existing patent mainly concentrates on the important prescription and method of children's's pills for improving acuity of sight.
Summary of the invention
The objective of the invention is to overcome the weak point of prior art, a kind of method of quality control of Chinese medicine preparation children's pills for improving acuity of sight that can the qualitative and quantitative analysis drug ingedient is provided.
The objective of the invention is to realize through following technical scheme:
A kind of method of quality control of Chinese medicine preparation children's pills for improving acuity of sight, step is:
(1) proterties and microscopical identification;
(2) be reference substance with the coptis and Berberine hydrochloride, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain coptis composition;
(3) with the rheum officinale be control medicinal material, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain the rheum officinale composition;
(4) with the scutelloside be reference substance, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain root of large-flowered skullcap composition;
(5) with the Gardenoside reference substance, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain the cape jasmine composition;
(6) with the Paeoniflorin be reference substance, high-efficient liquid phase technique is measured the radix paeoniae rubrathe content in children's's pills for improving acuity of sight prescription.
And said proterties and microscopical identification step are:
1. character identification: these article are the big honeyed pills of sepia to pitchy, bitter;
2. putting microscopically observes: bast fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin; Plant skin lithocyte yellow or light brown, how broken, complete person long polygon, rectangle or out-of-shape, wall thickness has big circular pit, the cell brownish red; Calcium oxalate cluster crystal is big, diameter 60-140 μ m; The pollen granule class is spherical, and the about 76 μ m of diameter, outer wall have thorn-like carving line, 3 germinal aperatures of tool; Parenchyma cell contains prism of calcium oxalate around the fibrous bundle, forms crystal fiber.
And said thin-layered chromatography differentiates that the method for the coptis in children's's pills for improving acuity of sight prescription is:
Get children's's pills for improving acuity of sight sample 4.5g, shred, add methyl alcohol 40ml, sonicated 45 minutes filters, and filtrating is as need testing solution; Other gets coptis control medicinal material 50mg, adds methyl alcohol 5ml, shines medicinal material solution in pairs with legal system, gets the Berberine hydrochloride reference substance again, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; Each 1～2 μ l of need testing solution 2～5 μ l, control medicinal material and reference substance solution is drawn in the thin-layered chromatography test, puts respectively on same silica gel g thin-layer plate; With normal butyl alcohol: glacial acetic acid: water=7: 1: 2 is developping agent, launches, and takes out; Dry, put under the ultraviolet lamp 365nm and inspect, in the test sample chromatogram; With control medicinal material and the corresponding position of reference substance chromatogram on same blob whether, to confirm whether medicine contains coptis composition.
And said thin-layered chromatography differentiates that the method for the rheum officinale in children's's pills for improving acuity of sight prescription is:
Get the need testing solution in the coptis detection, evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Heating is 30 minutes in the water-bath, divides jolting to extract 3 times with ether, and each 20ml merges ether solution; Evaporate to dryness, residue add methenyl choloride 2ml makes dissolving, as need testing solution; Other gets rheum officinale control medicinal material 0.1g, adds methyl alcohol 20ml, soaks 1 hour, filters, and gets filtrating 5ml, and evaporate to dryness shines medicinal material solution in pairs with legal system; Thin-layered chromatography is drawn each 4～8 μ l of above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate; With sherwood oil: ethyl acetate: formic acid=6: 2: 0.25 is developping agent, launches, and takes out; Dry, put under the ultraviolet lamp 365nm and inspect, in the test sample chromatogram; With the corresponding position of control medicinal material chromatogram on same blob whether, to confirm whether medicine contains the rheum officinale composition.
And said thin-layered chromatography differentiates that the method for the root of large-flowered skullcap in children's's pills for improving acuity of sight prescription is:
Get children's's pills for improving acuity of sight sample 2g, shred, add methyl alcohol 10ml, sonicated 45 minutes filters, and filtrating is concentrated into about 4ml, as need testing solution; Other gets the scutelloside reference substance and adds methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution; Each 2～5 μ l of above-mentioned two kinds of solution are drawn in thin-layered chromatography test, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 4% sodium acetate; With ethyl acetate: butanone: formic acid: water=5: 3: 1: 1 is developping agent, and pre-equilibration 30 minutes launches; Take out, dry, spray is with 1% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on same blob whether, to confirm whether medicine contains root of large-flowered skullcap composition.
And said thin-layered chromatography differentiates that the method for the cape jasmine in children's's pills for improving acuity of sight prescription is:
Get children's's pills for improving acuity of sight sample 9g, chopping adds zeyssatite 3g, grinds well, and 50ml adds diethyl ether; Sonicated 15 minutes filters, and discards ether liquid, and residue adds ethyl acetate 50ml, reflux 1 hour; Filter, the filtrating evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; Each 2～5 μ l of above-mentioned two kinds of solution are drawn in the thin-layered chromatography test, put respectively on same silica gel g thin-layer plate; With ethyl acetate: acetone: formic acid: water=10: 6: 2: 0.5 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 the test sample chromatogram with the corresponding position of reference substance chromatogram on same blob whether, to confirm whether medicine contains the cape jasmine composition.
And the method that said high-efficient liquid phase technique is measured the radix paeoniae rubrathe content in children's's pills for improving acuity of sight prescription is:
1. chromatographic condition: use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol: 0.05mol/L potassium dihydrogen phosphate: acetic acid: isopropyl alcohol=67: 173: 4: 4 is moving phase; The detection wavelength is 230nm, and number of theoretical plate calculates by the Paeoniflorin peak should be not less than 5000;
2. the preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and adds Diluted Alcohol and processes the solution that every 1ml contains 40 μ g, gets subsequent filtrate, injects liquid chromatograph;
3. the preparation of need testing solution: get children's's pills for improving acuity of sight sample, shred, get 1.2g, the accurate title, decide, the accurate Diluted Alcohol 50ml that adds; Claim decide weight, sonicated 45 minutes is put coldly, and weight decided in title again, supplies the weight that subtracts mistake again with Diluted Alcohol; Shake up, filter, get subsequent filtrate, inject liquid chromatograph;
4. detect and result's mensuration: precision is drawn reference substance solution, need testing solution and is used respectively 10 μ l of solvent respectively; Inject liquid chromatograph; Measure content of paeoniflorin in the test sample; And then through calculating the content of the radix paeoniae rubrathe, with reference to " content limit calculates under radix paeoniae rubrathe item of Chinese pharmacopoeia version in 2005, and every ball contains the radix paeoniae rubrathe with Paeoniflorin C
23H
28O
11Meter must not be less than 0.61mg.
Advantage of the present invention and good effect are:
1, detection method of the present invention is on the basis of second primary standard of " the Sanitation Ministry medicine standard " Chinese traditional patent formulation preparation; Increased the thin layer identification of test method of control medicinal material and reference substance; Formulate high performance liquid chromatography and carried out the method for assay; Revised quality standard control method; Improved the controllability of children's's pills for improving acuity of sight quality standard, further guaranteed product inherent quality and curative effect, to promoting production marketing, increase the competitiveness of product in market, guaranteeing that patient's drug safety is significant.
2, children's's pills for improving acuity of sight of the present invention has increased the microscopical identification method of the root of large-flowered skullcap, cape jasmine, rheum officinale, honeysuckle and Radix Glycyrrhizae in the prescription on the primary standard basis; Increased the thin layer discrimination method of the root of large-flowered skullcap, cape jasmine, rheum officinale and the coptis simultaneously; With the Paeoniflorin is reference substance, has formulated the content assaying method of the radix paeoniae rubrathe, can check out counterfeit drug and substandard drug more exactly after the modification, and the modernization of Chinese medicine and Chinese medicine are gone abroad to be significant.
Description of drawings
Fig. 1 inspects figure for the present invention supplies in the test agent coptis to detect thin-layer chromatogram at ultraviolet lamp (365nm), and wherein band is followed successively by from left to right: 1 coptis control medicinal material; 2 sample 1 (lot numbers: 200601); 3 sample 2 (lot numbers: 200602); 4 sample 3 (lot numbers: 200603); 5 Berberine hydrochloride reference substances; 6 negative samples;
Fig. 2, Fig. 3 are respectively the present invention and supply in the test agent rheum officinale to detect chromatogram under ultraviolet lamp (365nm) and daylight, to inspect figure, and wherein Fig. 2 and Fig. 3 are followed successively by from left to right: 1 negative sample; 2 sample 1 (lot numbers: 200601); 3 sample 2 (lot numbers: 200602); 4 sample 3 (lot numbers: 200603); 5 rheum officinale control medicinal materials;
Fig. 4 inspects figure for the present invention supplies the root of large-flowered skullcap in the test agent to detect thin-layer chromatogram under daylight, wherein, wherein band is followed successively by from left to right: 1, negative sample; 2, sample 1 (lot number: 200601); 3, sample 2 (lot number: 200602); 4, sample 3 (lot number: 200603); 5, scutelloside reference substance
Fig. 5 inspects under daylight for the present invention supplies in the test agent cape jasmine to detect thin-layer chromatogram, is followed successively by 1 from left to right: the Gardenoside reference substance; 2 negative samples; 3 sample 1 (lot numbers: 200601); 4 sample 2 (lot numbers: 200602); 5 sample 3 (lot numbers: 200603);
Fig. 6 is a Paeoniflorin reference substance liquid chromatogram of the present invention;
Fig. 7 is children's's pills for improving acuity of sight sample liquid chromatogram of the present invention;
Fig. 8 is a Paeoniflorin negative sample liquid chromatogram of the present invention.
Embodiment
Below in conjunction with embodiment, the present invention is further specified, following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
The method of quality control of Chinese medicine preparation children's pills for improving acuity of sight, the step of its method is:
Honeysuckle source in this confession reagent article: the kind that these article use be the dry flower of caprifoliaceae plant honeysuckle Lonicera japonicaThunb. or be with at the beginning of the flower opened, the flowers are in blossom gathers drying before putting for early summer.
(1) proterties and microscopical identification:
1. character identification: the color description of primary standard is the big honeyed pills of pitchy, and existing three lot sample article actual colors are sepia, passes appearance color in time in view of honeyed bolus and can deepen, so on the primary standard basis, revise is: these article are the big honeyed pills of sepia to pitchy; Bitter.
2. putting microscopically observes: bast fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin; Plant skin lithocyte yellow or light brown, how broken, complete person long polygon, rectangle or out-of-shape, wall thickness has big circular pit, the cell brownish red; Calcium oxalate cluster crystal is big, diameter 60-140 μ m; The pollen granule class is spherical, and the about 76 μ m of diameter, outer wall have thorn-like carving line, 3 germinal aperatures of tool; Parenchyma cell contains prism of calcium oxalate around the fibrous bundle, forms crystal fiber.
(2) adopting thin-layered chromatography, is reference substance with the coptis and Berberine hydrochloride, differentiates the coptis in children's's pills for improving acuity of sight prescription.
Get children's's pills for improving acuity of sight sample 4.5g, shred, add methyl alcohol 40ml, sonicated 45 minutes filters, and filtrating is as need testing solution; Other gets coptis control medicinal material 50mg, adds methyl alcohol 5ml, shines medicinal material solution in pairs with legal system, gets the Berberine hydrochloride reference substance again, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution.According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test, draw respectively 1～2 μ l of need testing solution 2～5 μ l, control medicinal material and reference substance solution, put respectively on same silica gel g thin-layer plate; With normal butyl alcohol: glacial acetic acid: water=7: 1: 2 is developping agent, launches, and takes out; Dry, put under the ultraviolet lamp 365nm and inspect, in the test sample chromatogram; With control medicinal material and the corresponding position of reference substance chromatogram on, show identical yellow fluorescence spot, testing result is seen Fig. 1
(3) adopting thin-layered chromatography, is control medicinal material with the rheum officinale, differentiates rheum officinale in children's's pills for improving acuity of sight prescription.
Get the need testing solution in the step item (2), evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Heating is 30 minutes in the water-bath, divides jolting to extract 3 times with ether, and each 20ml merges ether solution; Evaporate to dryness, residue add methenyl choloride 2ml makes dissolving, as need testing solution; Other gets rheum officinale control medicinal material 0.1g, adds methyl alcohol 20ml, soaks 1 hour, filters, and gets filtrating 5ml, and evaporate to dryness shines medicinal material solution in pairs with legal system; According to thin-layered chromatography (" an appendix VI of Chinese pharmacopoeia version in 2005 B) test; Draw each 4～8 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with sherwood oil (60～90 ℃): ethyl acetate: formic acid=6: 2: 0.25 is developping agent; Launch; Take out, dry, put under the ultraviolet lamp 365nm and inspect.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color, put in the ammonia steam smoked after, spot becomes redness, testing result is seen Fig. 2, Fig. 3.
(4) adopting thin-layered chromatography, is reference substance with the scutelloside, differentiates the root of large-flowered skullcap in children's's pills for improving acuity of sight prescription.
Get children's's pills for improving acuity of sight sample 2g, shred, add methyl alcohol 10ml, sonicated 45 minutes filters, and filtrating is concentrated into about 4ml, as need testing solution.Other gets the scutelloside reference substance and adds 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 2～5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 4% sodium acetate; With ethyl acetate: butanone: formic acid: water=5: 3: 1: 1 is developping agent; Pre-equilibration 30 minutes launches, and takes out; Dry, spray is with 1% ferric trichloride ethanolic solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color, testing result is seen Fig. 4.
(5) adopting thin-layered chromatography, is reference substance with the Gardenoside, differentiates cape jasmine in children's's pills for improving acuity of sight prescription.
Get children's's pills for improving acuity of sight sample 9g, chopping adds zeyssatite 3g, grinds well, and 50ml adds diethyl ether; Sonicated 15 minutes filters, and discards ether liquid, and residue adds ethyl acetate 50ml, reflux 1 hour; Filter, the filtrating evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution.Other gets the Gardenoside reference substance, adds methyl alcohol and processes 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 2～5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With ethyl acetate: acetone: formic acid: water=10: 6: 2: 0.5 is developping agent; Launch, take out, dry; Spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the spot colour developing.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color, testing result is seen Fig. 5.
(6) adopting high-efficient liquid phase technique, is reference substance with the Paeoniflorin, measures the radix paeoniae rubrathe content in children's's pills for improving acuity of sight prescription.
1. the test of chromatographic condition and system suitability uses octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol: 0.05mol/L potassium dihydrogen phosphate: acetic acid: isopropyl alcohol=67: 173: 4: 4 is moving phase; The detection wavelength is 230nm.Number of theoretical plate calculates by the Paeoniflorin peak should be not less than 5000.
2. the preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and adds Diluted Alcohol and processes the solution that every 1ml contains 40 μ g, gets subsequent filtrate, injects liquid chromatograph, and the result sees Fig. 6.
3. the preparation of need testing solution: get children's's pills for improving acuity of sight sample, shred, get 1.2g, the accurate title, decide; The accurate Diluted Alcohol 50ml that adds claims to decide weight, sonicated (power 50W, frequency 50kHz) 45 minutes; Put coldly, claim again to decide weight, supply the weight that subtracts mistake again, shake up with Diluted Alcohol; Filter, get subsequent filtrate, inject liquid chromatograph, testing result is seen Fig. 7.
4. the preparation of negative sample solution: get the flavour of a drug of respectively distinguishing the flavor of by prescription, make sample, press 2. need testing solution preparation method again, make negative sample solution by [method for making] except that Chinese herbaceous peony.
5. detect and result's mensuration: the radix paeoniae rubrathe accounts for 9.68% of prescription total amount in the prescription; In view of these article are starch; Require (starch calculates by 80% rate of transform) according to Chinese Pharmacopoeia Commission; With reference to " content limit calculates under radix paeoniae rubrathe item of Chinese pharmacopoeia version in 2005, and every ball contains the radix paeoniae rubrathe with Paeoniflorin (C
23H
28O
11) meter, must not be less than 0.61mg.
Claims (1)
1. the detection method of a Chinese medicine preparation children's pills for improving acuity of sight, it is characterized in that: the step of its method is:
(1) proterties and microscopical identification;
(2) be reference substance with the coptis and Berberine hydrochloride, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain coptis composition;
(3) with the rheum officinale be control medicinal material, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain the rheum officinale composition;
(4) with the scutelloside be reference substance, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain root of large-flowered skullcap composition;
(5) with the Gardenoside reference substance, thin-layered chromatography differentiates in children's's pills for improving acuity of sight prescription whether contain the cape jasmine composition;
(6) with the Paeoniflorin be reference substance, high-efficient liquid phase technique is measured the radix paeoniae rubrathe content in children's's pills for improving acuity of sight prescription;
Said proterties and microscopical identification step are:
1. character identification: these article are the big honeyed pills of sepia to pitchy, bitter;
2. putting microscopically observes: bast fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin; Plant skin lithocyte yellow or light brown, how broken, complete person long polygon, rectangle or out-of-shape, wall thickness has big circular pit, the cell brownish red; Calcium oxalate cluster crystal is big, diameter 60-140 μ m; The pollen granule class is spherical, and the about 76 μ m of diameter, outer wall have thorn-like carving line, 3 germinal aperatures of tool; Parenchyma cell contains prism of calcium oxalate around the fibrous bundle, forms crystal fiber;
Said thin-layered chromatography differentiates that the method for the coptis in children's's pills for improving acuity of sight prescription is:
Get children's's pills for improving acuity of sight sample 4.5g, shred, add methyl alcohol 40ml, sonicated 45 minutes filters, and filtrating is as need testing solution; Other gets coptis control medicinal material 50mg, adds methyl alcohol 5ml, shines medicinal material solution in pairs with legal system, gets the Berberine hydrochloride reference substance again, adds methyl alcohol and processes the solution that every 1ml contains 0.5mg, as reference substance solution; Each 1～2 μ l of need testing solution 2～5 μ l, control medicinal material and reference substance solution is drawn in the thin-layered chromatography test, puts respectively on same silica gel g thin-layer plate; With normal butyl alcohol: glacial acetic acid: water=7: 1: 2 is developping agent, launches, and takes out; Dry, put under the ultraviolet lamp 365nm and inspect, in the test sample chromatogram; With control medicinal material and the corresponding position of reference substance chromatogram on same blob whether, to confirm whether medicine contains coptis composition;
Said thin-layered chromatography differentiates that the method for the rheum officinale in children's's pills for improving acuity of sight prescription is:
Get the need testing solution in the coptis detection, evaporate to dryness, residue add water 10ml makes dissolving, adds hydrochloric acid 1ml again; Heating is 30 minutes in the water-bath, divides jolting to extract 3 times with ether, and each 20ml merges ether solution; Evaporate to dryness, residue add methenyl choloride 2ml makes dissolving, as need testing solution; Other gets rheum officinale control medicinal material 0.1g, adds methyl alcohol 20ml, soaks 1 hour, filters, and gets filtrating 5ml, and evaporate to dryness shines medicinal material solution in pairs with legal system; Thin-layered chromatography is drawn each 4～8 μ l of above-mentioned two kinds of solution, puts respectively on same silica gel g thin-layer plate; With sherwood oil: ethyl acetate: formic acid=6: 2: 0.25 is developping agent, launches, and takes out; Dry, put under the ultraviolet lamp 365nm and inspect, in the test sample chromatogram; With the corresponding position of control medicinal material chromatogram on same blob whether, to confirm whether medicine contains the rheum officinale composition;
Said thin-layered chromatography differentiates that the method for the root of large-flowered skullcap in children's's pills for improving acuity of sight prescription is:
Get children's's pills for improving acuity of sight sample 2g, shred, add methyl alcohol 10ml, sonicated 45 minutes filters, and filtrating is concentrated into 4ml, as need testing solution; Other gets the scutelloside reference substance and adds methyl alcohol and process the solution that every 1ml contains 1mg, as reference substance solution; Each 2～5 μ l of above-mentioned two kinds of solution are drawn in thin-layered chromatography test, put respectively in same be on the silica gel g thin-layer plate of binder with the carboxymethylcellulose sodium solution that contains 4% sodium acetate; With ethyl acetate: butanone: formic acid: water=5: 3: 1: 1 is developping agent, and pre-equilibration 30 minutes launches; Take out, dry, spray is with 1% ferric trichloride ethanolic solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on same blob whether, to confirm whether medicine contains root of large-flowered skullcap composition;
Said thin-layered chromatography differentiates that the method for the cape jasmine in children's's pills for improving acuity of sight prescription is:
Get children's's pills for improving acuity of sight sample 9g, chopping adds zeyssatite 3g, grinds well, and 50ml adds diethyl ether; Sonicated 15 minutes filters, and discards ether liquid, and residue adds ethyl acetate 50ml, reflux 1 hour; Filter, the filtrating evaporate to dryness, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the Gardenoside reference substance, adds methyl alcohol and processes the solution that every 1ml contains 1mg, as reference substance solution; Each 2～5 μ l of above-mentioned two kinds of solution are drawn in the thin-layered chromatography test, put respectively on same silica gel g thin-layer plate; With ethyl acetate: acetone: formic acid: water=10: 6: 2: 0.5 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 the test sample chromatogram with the corresponding position of reference substance chromatogram on same blob whether, to confirm whether medicine contains the cape jasmine composition;
The method that said high-efficient liquid phase technique is measured the radix paeoniae rubrathe content in children's's pills for improving acuity of sight prescription is:
1. chromatographic condition: use octadecylsilane chemically bonded silica to be filling agent; Methyl alcohol: 0.05mol/L potassium dihydrogen phosphate: acetic acid: isopropyl alcohol=67: 173: 4: 4 is moving phase; The detection wavelength is 230nm, and number of theoretical plate calculates by the Paeoniflorin peak should be not less than 5000;
2. the preparation of reference substance solution: it is an amount of to get the Paeoniflorin reference substance, and accurate the title decides, and adds Diluted Alcohol and processes the solution that every 1ml contains 40 μ g, gets subsequent filtrate, injects liquid chromatograph;
3. the preparation of need testing solution: get children's's pills for improving acuity of sight sample, shred, get 1.2g, the accurate title, decide, the accurate Diluted Alcohol 50ml that adds; Claim decide weight, sonicated 45 minutes is put coldly, and weight decided in title again, supplies the weight that subtracts mistake again with Diluted Alcohol; Shake up, filter, get subsequent filtrate, inject liquid chromatograph;
4. detect and result's mensuration: precision is drawn reference substance solution, need testing solution and is used respectively 10 μ l of solvent respectively; Inject liquid chromatograph; Measure content of paeoniflorin in the test sample; And then through calculating the content of the radix paeoniae rubrathe, with reference to " content limit calculates under 2005 editions radix paeoniae rubrathe items of Chinese pharmacopoeia, and every ball radix paeoniae rubrathe is with Paeoniflorin C
23H
28O
11Meter must not be less than 0.61mg;
Said children's's pills for improving acuity of sight is made up of the radix paeoniae rubrathe, the root of large-flowered skullcap, cape jasmine, root of Chinese trichosanthes, rheum officinale, honeysuckle, chrysanthemum, salt system plantain seed, the coptis, peppermint, Radix Glycyrrhizae; Its preparation method is: above ten simply; Be ground into fine powder; Sieve, mixing, every 100g powder add refined honey 150～170g and process big honeyed pills and promptly get.
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|---|---|---|---|
| CN2009100709591A CN102038785B (en) | 2009-10-26 | 2009-10-26 | Detection method for traditional Chinese medicinal preparation of children eyesight pills |
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| CN105628665A (en) * | 2016-02-05 | 2016-06-01 | 四川德成动物保健品有限公司 | Method for detecting rhizoma coptidis in powder with effects of clearing acute communicable diseases and counteracting toxin |
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| CN101408531A (en) * | 2008-07-11 | 2009-04-15 | 包头中药有限责任公司 | Method for detecting quality of Sijisanhuangwan |
| CN101485762A (en) * | 2008-01-16 | 2009-07-22 | 韩勇 | Quality control method of Chinese medicine preparation |
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| CN101408531A (en) * | 2008-07-11 | 2009-04-15 | 包头中药有限责任公司 | Method for detecting quality of Sijisanhuangwan |
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Address after: No.21, 10th Street, Binhai New Area Development Zone, Tianjin 300457 Patentee after: Jinyao Darentang Group Co.,Ltd. Darentang Pharmaceutical Factory Address before: 300457 No. tenth, 21 Avenue, Tianjin economic and Technological Development Zone Patentee before: DARENTANG PHARMACEUTICAL FACTORY, TIANJIN ZHONGXIN PHARMACEUTICAL GROUP Co.,Ltd. |