CN101530506A - Method for analyzing poisonous clear tablet - Google Patents
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- CN101530506A CN101530506A CN200910136265A CN200910136265A CN101530506A CN 101530506 A CN101530506 A CN 101530506A CN 200910136265 A CN200910136265 A CN 200910136265A CN 200910136265 A CN200910136265 A CN 200910136265A CN 101530506 A CN101530506 A CN 101530506A
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Abstract
The invention discloses a method for analyzing poisonous clear tablet which belongs to the Chinese medicine technique field. The method can increase accuracy of each component in poisonous clear tablet and increase accuracy of the product quality.
Description
[technical field]
The invention belongs to the traditional Chinese medicine technology technical field, be specifically related to a kind of analytical method of SHIDUQING PIAN.
[background technology]
SHIDUQING PIAN is to be guidance with the Chinese medical theory, by the pure Chinese medicinal preparation that nine flavor drug matchings such as the meticulous screening Radix Rehmanniae, Radix Salviae Miltiorrhizae, Radix Angelicae Sinensis, Radix Sophorae Flavescentis, Periostracum Cicadae, Radix Scutellariae, Cortex Dictamni, Rhizoma Smilacis Glabrae, Radix Glycyrrhizae form, be the prescription of the ripe notion of cutaneous diseases, the skin allergy one line medication of Chinese medicine treating both the principal and secondary aspects of a disease.
SHIDUQING PIAN is remarkable to the skin pruritus effect that invaded outward by blood deficiency, wind heat and damp invasion of lower energizer etc. causes, pathogeny at skin pruritus, itch to control that to control the heart earlier be general provisions, blood enriching and dryness moistening, removing dampness detoxifcation, Eradicates wind are antipruritic, are usually used in treating eczema, rubella, urticaria etc.
The adaptation symptom of SHIDUQING PIAN comprises:
(1) blood deficiency cutaneouspruritus
First kind is syndrome of wind and dryness due to blood deficiency; Old, deficiency of qi and blood person, its skin pruritus mostly is blood-deficiency and wind-dry.Be more common in old thin weak person, skin pruritus, skin lesion appearing without definite location, more so be difficult to fall asleep night, whole body xerosis cutis desquamation, scratch is innumerable, does not prolongedly heal, and the heavy summer in winter is light, companion's lassitude, it is involved and abstruse to defecate, lusterless complexion, pale tongue, thin fur, thready pulse without strength.Control suitable blood enriching and dryness moistening, dispelling wind for relieving itching.
Second kind is syndrome of stagnation of liver qi and blood deficiency; Cause skin pruritus by anxious state of mind, mostly be hepatic depression and blood deficiency.Skin pruritus is many to be produced when excited, and spirit depressing is with a haggard face, sighs, and is vexed, bitter taste, and women's menoxenia or amenorrhea, the lip and nail color is light, pale tongue or dark, thin fur, thready and hesitant pulse.Control suitable dispersing the stagnated live-QI to relieve the stagnation of QI, nourishing blood to expel wind.
(2) wind heat is invaded the skin pruritus that causes outward rubella and urticaria etc.
Rubella with heating, skin rash is feature, often with behind the ear, the occipital lymph node enlargement, hard to bear or little itching very itches.Welt and erythema then often appear in urticaria.
The pruritus that wind heat stasis skin causes is sent out in summer and autumn well, and temperature can bring out or increase the weight of when dry, or increases the weight of when lying in bed night, fever of the body, and micro evil wind is cold, and is thirsty, perspires constipation with dry stool, urine yellow skin, red tongue, yellow and thin fur or do floating and rapid pulse.Control suitable wind and heat dispersing, harmonizing yingfen and weifen.
(3) damp invasion of lower energizer causes noxious dampness to pent up skin, and dampness smoulders and with the passing of time becomes poison.
Noxious dampness is caused harm, be in to internal organs, outward to the flesh table, the upper, middle and lower three warmers nowhere less than.Noxious dampness easily flows, and is attached to each position of body, and noxious dampness is made a bet and strongly fragrantly then easily given birth to " multiple abscesses due to noxious dampness " in skin.Pruritus is sent out around anus well, scrotum and cysthus position, be difficult to control when itching, cause excessively and scratch, grabbing the part, back can have scratch, redness, with the passing of time then plump, lichenization, sweating, friction and food stimulus etc. can be brought out or increase the weight of, and the married woman can be stench with leukorrhagia, the bitter taste halitosis, red tongue, yellow and greasy fur, slippery and rapid pulse.It is antipruritic to control suitable removing damp-heat.Wherein the common sympton of eczema is: erythema, pimple, vesicle, erosion, ooze out, form a scab, violent pruritus etc.
Etiology and pathogenesis
Skin pruritus, the traditional Chinese medical science are referred to as " pruritus ", " disease of itching " " pruritus caused by wind pathogen ".The record of " all sufferings skin ulcers all belong to the heart ", " all pains are for real, and all itching is void " is promptly arranged in " interior warp ".The meaning is a disease being located in the exterior, links to each other with pathogenesis of five Zang, and every pain or the skin infection of gargalesthesia is arranged all belongs to the heart.Heart governing blood and vessels, the interior filling vital organs of the human body moisten the extremity bones of the body collectively outward, the skin and flesh muscles along the regular meridians, QI-blood circulation, nowhere less than.If the then all cards of stagnation of QI-blood come in great numbers, so the card of the sufferings of the blood vessels stasis of blood due to stagnating all can be from the heart by controlling; Have an itch as if the heavy then fire-toxin Yu Mai of heart-fire; Deficiency of heart-blood then wind syndrome due to blood-deficiency also easily produces pruritus, thus no matter blood deficiency, heat in blood itch all relevant with the deficiency and excess of the heart.
SHIDUQING PIAN is screened nine flavor drug matchings such as the Radix Rehmanniae, Radix Salviae Miltiorrhizae, Radix Angelicae Sinensis, Radix Sophorae Flavescentis, Periostracum Cicadae, Radix Scutellariae, Cortex Dictamni, Rhizoma Smilacis Glabrae, Radix Glycyrrhizae meticulously and is formed, can all medicine compatibilities, rigorous reasonable, be total to nourish blood, dampness, heat clearing away, antipruritic merit, reach that the deficiency of YIN can be mended, heat in blood can clearly, dry then can be moistened, wind then can be dispelled, the wet effect that then can remove.
The main application of SHIDUQING PIAN is in the mountain area and the remote local more medicine that uses, and is suitable for tour in the field, exploration, exploration crowd.And the equipment scarcity of the detection of these medicines from far-off regions thereby gives this problem, need provide can be simple and easy to do the medicine analytical method.
Simultaneously, the detection of traditional Chinese compound medicine often uses analytical equipments such as chromatography of gases and liquid chromatograph, during check fee, effort, expensive, based on these problems, also needs to provide a kind of or analytical method that a class is simple and efficient is determined the true and false of medicine.
For workshop medicine finished product and particulate check, also need to establish its analytical method simultaneously, guarantee the quality of medicine.
[summary of the invention]
The object of the present invention is to provide a kind of analytical method of SHIDUQING PIAN.The analytical method of SHIDUQING PIAN of the present invention is simple and easy to do, and is convenient and swift, and the rapid true and false of differentiating medicine of energy is a kind of analytical method that basic unit promotes that is suitable for tersely.
Particularly, the analytical method of SHIDUQING PIAN of the present invention adopts following method: get this product, putting microscopically observes: starch grain is numerous, simple grain similar round, ellipse, semicircle or class polygon, diameter 10～48 μ m, omphalion point-like, starlike, three forked, slit-likes; Needle-like calcium oxalate crystal bunchy or be dispersed in, long 45～130 μ m, fiber is faint yellow, fusiformis, wall thickness, the hole ditch is thin.
Above-mentioned analytical method adopts following method: get this product, porphyrize, take by weighing 1g, add water 20ml, strong aqua ammonia 1ml, chloroform 20ml, reflux 1 hour divides and gets the chloroform layer, add chloroform extraction again 2 times, each 10ml merges chloroform liquid, volatilize, residue adds methanol 1ml makes dissolving, and as need testing solution, other gets Radix Sophorae Flavescentis control medicinal material 0.5g, shine medical material solution in pairs with legal system, according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution 10ul and control medicinal material solution 5ul, put respectively on same sodium carboxymethyl cellulose silica gel G plate, with benzene-acetone-ethyl acetate-strong ammonia solution (2:3:4:0.5) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Above-mentioned analytical method adopts following method: get this product, porphyrize, take by weighing 3g, put in the tool plug conical flask, add 70% ethanol 30ml, supersound process 30 minutes, centrifugal, get supernatant, add hydrochloric acid 5ml, water 30ml, reflux 1 hour, put coldly, extract 2 times each 60ml with petroleum ether (30-60 ℃), merge petroleum ether liquid, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution, extracting liquorice subacid reference substance in addition, add dehydrated alcohol and make solution that every 1ml contains 1mg product solution in contrast,, draw above-mentioned two kinds of each 5ul of solution according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, put respectively on same sodium carboxymethyl cellulose silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-benzene-ethyl acetate-glacial acetic acid (10:20:7:0.5) is developing solvent, launches, and takes out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing in 105 ℃, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Above-mentioned analytical method adopts following method: get this product, porphyrize, take by weighing 5g, add methanol 30ml, reflux 1 hour, filter, filtrate evaporate to dryness, residue add water 20ml makes dissolving, regulate PH1-2 with dilute hydrochloric acid, extract 2 times each 15ml, combined ethyl acetate liquid with the ethyl acetate jolting, evaporate to dryness in the water-bath, residue adds ethanol makes dissolving, and as need testing solution, other gets the baicalin reference substance, add methanol and make the solution that 1ml contains 1mg, product solution according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, is drawn each 10 μ l of above-mentioned two kinds of solution in contrast, put respectively in same be on the silica gel g thin-layer plate of adhesive with the carboxymethylcellulose sodium solution that contains 4% sodium acetate, with ethyl acetate-butanone-formic acid-water (5:3:1:1) is developing solvent, and pre-equilibration 30 minutes launches, take out, dry, spray is with 1% ferric chloride alcoholic solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Above-mentioned analytical method adopts following method: get this product, porphyrize, take by weighing 3g, add chloroform 20ml, reflux, extract, 30 minutes, filter, filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution Ling Qu fraxinellone reference substance, add methanol and make the solution that every 1ml contains 1mg, in contrast product solution, draw above-mentioned two kinds of each 10ul of solution, put respectively on same sodium carboxymethyl cellulose silica gel g thin-layer plate,, launch with normal hexane-ethyl acetate (3:2), take out, dry, put in the iodine steam smoked to clear spot, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Above-mentioned analytical method, adopt following method: get this product, porphyrize takes by weighing 2g, add chloroform 30ml, supersound process 20 minutes filters, and filtrate is put evaporate to dryness in the water-bath, residue adds petroleum ether (60-90 ℃) 0.5ml makes dissolving, as need testing solution, other Poria control medicinal material 2g that fetches earth shines medical material solution in pairs with legal system, test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), drawing above-mentioned two kinds of each 10ul of solution, put respectively on sodium carboxymethyl cellulose silica gel G plate, is developing solvent with chloroform-ethyl acetate-formic acid (9:1:0.01), launch, take out, dry, spray is with the ferric chloride test solution, about 5 minutes of 105 ℃ of heating, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
The analytical method of above-mentioned arbitrary described SHIDUQING PIAN, can further adopt the further qualitative detection of following method:
This product is got in the preparation of need testing solution, and porphyrize is got 0.2g, and accurate the title decides, and puts in the 50ml tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, and supersound extraction 1 hour claims to decide weight again, supplies the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly
The preparation precision of reference substance solution takes by weighing at 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure an amount of, and add methanol and make the solution that every 1ml contains 60 μ g, that is,
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water-acetic acid (60:40:2) is mobile phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak should be not less than 2500,
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Scutellariae with baicalin (C
21H
180
11) meter, must not be less than 6.5mg.
[specific embodiment]
Following embodiment further describes the present invention, but described embodiment only is used to illustrate the present invention rather than restriction the present invention.
Embodiment 1
Get this product, put microscopically and observe: starch grain is numerous, simple grain similar round, ellipse, semicircle or class polygon, diameter 10～48 μ m, omphalion point-like, starlike, three forked, slit-likes; Needle-like calcium oxalate crystal bunchy or be dispersed in, long 45～130 μ m.Fiber is faint yellow, fusiformis, and wall thickness, the hole ditch is thin.
Embodiment 2
Get this product, porphyrize takes by weighing 1g, adds water 20ml, strong aqua ammonia 1ml, chloroform 20ml, reflux 1 hour divides and gets the chloroform layer, adds chloroform extraction again 2 times, each 10ml, merge chloroform liquid, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Radix Sophorae Flavescentis control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 10ul and control medicinal material solution 5ul, put respectively on same sodium carboxymethyl cellulose silica gel G plate, with benzene-acetone-ethyl acetate-strong ammonia solution (2:3:4:0.5) is developing solvent, launch, take out, dry, spray is with rare bismuth potassium iodide test solution.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiment 3
Get this product, porphyrize takes by weighing 3g, put in the tool plug conical flask, add 70% ethanol 30ml, supersound process 30 minutes, centrifugal, get supernatant, add hydrochloric acid 5ml, water 30ml, reflux 1 hour is put cold, extract 2 times with petroleum ether (30-60 ℃), each 60ml merges petroleum ether liquid, evaporate to dryness, residue add dehydrated alcohol 1ml makes dissolving, as need testing solution.Extracting liquorice subacid reference substance in addition adds dehydrated alcohol and makes solution that every 1ml contains 1mg product solution in contrast.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned two kinds of each 5ul of solution, put respectively on same sodium carboxymethyl cellulose silica gel g thin-layer plate, with petroleum ether (30-60 ℃)-benzene-ethyl acetate-glacial acetic acid (10:20:7:0.5) is developing solvent, launch, take out, dry, spray is with 10% phosphomolybdic acid ethanol solution, and it is clear to be heated to the speckle colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 4
Get this product, porphyrize takes by weighing 5g, add methanol 30ml, reflux 1 hour filters, filtrate evaporate to dryness, residue add water 20ml makes dissolving, regulates PH1-2 with dilute hydrochloric acid, extract 2 times with the ethyl acetate jolting, each 15ml, combined ethyl acetate liquid, evaporate to dryness in the water-bath, residue adds ethanol makes dissolving, as need testing solution.Other gets the baicalin reference substance, adds methanol and makes the solution that 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ 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 carboxymethylcellulose sodium solution that contains 4% sodium acetate, with ethyl acetate-butanone-formic acid-water (5:3:1:1) is developing solvent, pre-equilibration 30 minutes launches, and takes out, dry, spray is with 1% ferric chloride alcoholic solution.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 5
Get this product, porphyrize takes by weighing 3g, adds chloroform 20ml, and reflux, extract, 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Ling Qu fraxinellone reference substance, add methanol and make the solution that every 1ml contains 1mg, product solution in contrast, draw above-mentioned two kinds of each 10ul of solution, put respectively on same sodium carboxymethyl cellulose silica gel g thin-layer plate, with normal hexane-ethyl acetate (3:2), launch, take out, dry, put in the iodine steam smoked to clear spot.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
Embodiment 6
Get this product, porphyrize takes by weighing 2g, adds chloroform 30ml, and supersound process 20 minutes filters, and filtrate is put evaporate to dryness in the water-bath, and residue adds petroleum ether (60-90 ℃) 0.5ml makes dissolving, as need testing solution.Other Poria control medicinal material 2g that fetches earth shines medical material solution in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw above-mentioned two kinds of each 10ul of solution, put respectively on sodium carboxymethyl cellulose silica gel G plate, with chloroform-ethyl acetate-formic acid (9:1:0.01) is developing solvent, launch, take out, dry, spray is with the ferric chloride test solution, about 5 minutes of 105 ℃ of heating.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
Embodiment 7
[inspection] should meet every regulation relevant under the tablet item (an appendix I of Chinese Pharmacopoeia version in 2005 D).
[assay] measured according to high performance liquid chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 D).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water-acetic acid (60:40:2) is mobile phase; The detection wavelength is 280nm.Number of theoretical plate calculates by the baicalin peak should be not less than 2500.
The preparation precision of reference substance solution takes by weighing at 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure an amount of, adds methanol and makes the solution that every 1ml contains 60 μ g, promptly.
This product is got in the preparation of need testing solution, and porphyrize is got 0.2g, and accurate the title decides, and puts in the 50ml tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, and supersound extraction 1 hour claims to decide weight again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 6.5mg.
Claims (7)
1. the analytical method of a SHIDUQING PIAN is characterized in that, adopts following methods analyst: get this product, putting microscopically observes: starch grain is numerous, simple grain similar round, ellipse, semicircle or class polygon, diameter 10～48 μ m, omphalion point-like, starlike, three forked, slit-likes; Needle-like calcium oxalate crystal bunchy or be dispersed in, long 45～130 μ m, fiber is faint yellow, fusiformis, wall thickness, the hole ditch is thin.
2. according to the analytical method of the described SHIDUQING PIAN of claim 1, it is characterized in that, get this product, porphyrize, take by weighing 1g, add water 20ml, strong aqua ammonia 1ml, chloroform 20ml, reflux 1 hour divides and gets the chloroform layer, adds chloroform extraction again 2 times, each 10ml, merge chloroform liquid, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution, other gets Radix Sophorae Flavescentis control medicinal material 0.5g, shines medical material solution in pairs with legal system, according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw need testing solution 10ul and control medicinal material solution 5ul, putting respectively on same sodium carboxymethyl cellulose silica gel G plate, is developing solvent with benzene-acetone-ethyl acetate-strong ammonia solution (2:3:4:0.5), launches, take out, dry, spray is with rare bismuth potassium iodide test solution, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
3. according to the analytical method of the described poisonous clear tablet of claim 2; It is characterized in that; Get this product; Porphyrize; Take by weighing 3g; Put in the tool plug conical flask; Add 70% ethanol 30ml; Ultrasonic processing 30 minutes, centrifugal, get supernatant; Add hydrochloric acid 5ml; Water 30ml added hot reflux 1 hour, let cool; Extract 2 times with benzinum (30-60 ℃); Each 60ml merges benzinum liquid, evaporate to dryness; Residue adds absolute ethyl alcohol 1ml makes dissolving; As need testing solution, extracting liquorice hypo acid reference substance in addition adds absolute ethyl alcohol and makes in contrast product solution of solution that every 1ml contains 1mg; Test according to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005); Draw above-mentioned two kinds of each 5ul of solution, put respectively on same sodium carboxymethylcellulose silica gel g thin-layer plate, take benzinum (30-60 ℃)-benzene-ethyl acetate-glacial acetic acid (10:20:7:0.5) as solvent; Launch; Take out, dry, spray is with 10% phosphomolybdic acid ethanol solution; It is clear to be heated to the spot colour developing in 105 ℃; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
4. according to the analytical method of the described SHIDUQING PIAN of claim 3, it is characterized in that, get this product, porphyrize takes by weighing 5g, adds methanol 30ml, reflux 1 hour filters the filtrate evaporate to dryness, residue adds water 20ml makes dissolving, regulates PH1-2 with dilute hydrochloric acid, extracts 2 times with the ethyl acetate jolting, each 15ml, combined ethyl acetate liquid, evaporate to dryness in the water-bath, residue add ethanol makes dissolving, as need testing solution, other gets the baicalin reference substance, adds methanol and makes the solution that 1ml contains 1mg, in contrast product solution, test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw each 10 μ 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 carboxymethylcellulose sodium solution that contains 4% sodium acetate, be developing solvent with ethyl acetate-butanone-formic acid-water (5:3:1:1), pre-equilibration 30 minutes, launch, take out, dry, spray is with 1% ferric chloride alcoholic solution, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
5. according to the analytical method of the described SHIDUQING PIAN of claim 4, it is characterized in that, get this product, porphyrize takes by weighing 3g, adds chloroform 20ml, reflux, extract, 30 minutes filters the filtrate evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution, and Ling Qu fraxinellone reference substance, add methanol and make the solution that every 1ml contains 1mg, product solution is drawn above-mentioned two kinds of each 10ul of solution in contrast, puts respectively on same sodium carboxymethyl cellulose silica gel g thin-layer plate, with normal hexane-ethyl acetate (3:2), launch, take out, dry, put in the iodine steam smoked to clear spot, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
6. according to the analytical method of the described SHIDUQING PIAN of claim 5, it is characterized in that, get this product, porphyrize, take by weighing 2g, add chloroform 30ml, supersound process 20 minutes, filter, filtrate is put evaporate to dryness in the water-bath, and residue adds petroleum ether (60-90 ℃) 0.5ml makes dissolving, as need testing solution, other is the Poria control medicinal material 2g that fetches earth, shine medical material solution in pairs with legal system,, draw above-mentioned two kinds of each 10ul of solution according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, put respectively on sodium carboxymethyl cellulose silica gel G plate, with chloroform-ethyl acetate-formic acid (9:1:0.01) is developing solvent, launches, and takes out, dry, spray is with the ferric chloride test solution, about 5 minutes of 105 ℃ of heating, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
7. according to the analytical method of the arbitrary described SHIDUQING PIAN of claim 1-6, it is characterized in that,
This product is got in the preparation of need testing solution, and porphyrize is got 0.2g, and accurate the title decides, and puts in the 50ml tool plug conical flask, the accurate methanol 25ml that adds, close plug claims to decide weight, and supersound extraction 1 hour claims to decide weight again, supplies the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly
The preparation precision of reference substance solution takes by weighing at 4 hours baicalin reference substance of 60 ℃ of drying under reduced pressure an amount of, and add methanol and make the solution that every 1ml contains 60 μ g, that is,
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water-acetic acid (60:40:2) is mobile phase; The detection wavelength is 280nm, and number of theoretical plate calculates by the baicalin peak should be not less than 2500,
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
Every of this product contains Radix Scutellariae with baicalin (C
21H
18O
11) meter, must not be less than 6.5mg.
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| CN101797334A (en) * | 2010-04-26 | 2010-08-11 | 严德华 | External ointment for treating onychomycosis and paronychia |
| CN104991031A (en) * | 2015-07-23 | 2015-10-21 | 河北中医学院 | Rapid multiple information thin-layer identification method of smilax glabra and water extract thereof |
| CN108535399A (en) * | 2018-04-09 | 2018-09-14 | 吉林省中研药业有限公司 | A kind of detection method of Fuyankang pill |
| CN113769010A (en) * | 2021-10-29 | 2021-12-10 | 何彦生 | Traditional Chinese medicine formula for treating damp-heat and yang-deficiency type chronic eczema |
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2009
- 2009-05-05 CN CN2009101362653A patent/CN101530506B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101797334A (en) * | 2010-04-26 | 2010-08-11 | 严德华 | External ointment for treating onychomycosis and paronychia |
| CN101797334B (en) * | 2010-04-26 | 2011-09-07 | 严德华 | External ointment for treating onychomycosis and paronychia |
| CN104991031A (en) * | 2015-07-23 | 2015-10-21 | 河北中医学院 | Rapid multiple information thin-layer identification method of smilax glabra and water extract thereof |
| CN108535399A (en) * | 2018-04-09 | 2018-09-14 | 吉林省中研药业有限公司 | A kind of detection method of Fuyankang pill |
| CN108535399B (en) * | 2018-04-09 | 2020-05-08 | 吉林省中研药业有限公司 | Detection method of Fuyankang pills |
| CN113769010A (en) * | 2021-10-29 | 2021-12-10 | 何彦生 | Traditional Chinese medicine formula for treating damp-heat and yang-deficiency type chronic eczema |
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