CN103175936B - A kind of detection method of Chinese medicine composition nephritislin capsule - Google Patents
A kind of detection method of Chinese medicine composition nephritislin capsule Download PDFInfo
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Abstract
The invention discloses a kind of by ministry standard [standard number: WS3-B-2538-97] described nephritislin capsule formula, make the method for quality control of the formulation of clinical practice, the method is by the discriminating to part component, and assay, makes product quality obtain effective control.
Description
Technical field
The present invention relates to a kind of method of quality control, particularly a kind of detection side of Chinese medicine composition nephritislin capsuleMethod.
Background technology
Nephritislin capsule effect with cure mainly into: clearing heat and cooling blood, kidney is supported in enriching yin. For CGN. GlomerulonephritisInflammation is a kind of immunity disease, is that the one group of clinical manifestation that is primary in glomerulus that caused by many reasons is similar, pathological changeThe immunity disease differ, prognosis being not quite similar, taking albuminuria, blood urine, oedema, hypertension and renal insufficiency as its feature.But initial quality control method is difficult to product to carry out effective quality control.
Fill a prescription and preparation method by ministry standard kind ［ standard number: WS3-B-2538-97 ］ " nephritislin capsule ": China ink droughtLotus 71.6g, fruit of glossy privet 43g, glutinous rehmannia 43g, Chinese yam 76.6g, Radix Angelicae Sinensis 43g, Ligusticum wallichii 14.4g, radix paeoniae rubrathe 28.8g, rhizoma cibotii (scalding) 143g,Poria cocos 43g, umbellate pore furgus 43g, plantain seed (salt stir-fry) 86g, madder 43g, setose thistle 71.6g, field thistle 71.6g, cape jasmine 43g, purslane172g, garden burnet 143g, above 17 tastes, are ground into fine powder by Radix Angelicae Sinensis, Ligusticum wallichii, cape jasmine; 14 tastes such as all the other ecliptas, add decoctingBoil secondary, 3 hours for the first time, 2 hours for the second time, collecting decoction, filtered, and it is 1.30～1.35 that filtrate is condensed into relative densityThe thick paste of (60 DEG C); Add above-mentioned medicinal powder, mix, dry, pulverize into fine powder, granulation, incapsulates, and makes 1000,Obtain.
Summary of the invention
The object of the invention is to openly a kind of method of quality control of Chinese medicine preparation.
The present invention seeks to be achieved through the following technical solutions: a kind ofly join according to the nephritislin capsule described in national standardSide, the method for quality control of making the formulation of clinical practice comprises to be differentiated and assay.
The detection method of a kind of Chinese medicine composition nephritislin of the present invention capsule, this detection method relates in nephritislin capsule and working asReturn, concrete discrimination method and the Determination of Gardenoside assay method of Ligusticum wallichii, Gardenoside, gallic acid main active, its featureBe:
1) in this detection method, Radix Angelicae Sinensis, Ligusticum wallichii discriminating are: get this product, porphyrize, gets 3.0g, adds n-hexane 25ml, ultrasonic(250W, 40Hz) processes 25-35 minute, filters, and filtrate is concentrated into about 1ml, as need testing solution; Separately get Ligusticum wallichii, Radix Angelicae Sinensis pairAccording to the each 0.5g of medicinal material, be made in the same way of respectively control medicinal material solution; According to thin-layered chromatography test, draw each 10 μ of above-mentioned two kinds of solutionL, puts respectively on same silica gel g thin-layer plate, taking benzinum (60～90 DEG C)-ethyl acetates (9-9.5:0.5-1) as launchingAgent, launches, and takes out, and dries, and puts under ultraviolet lamp (340-380nm) and inspects; In test sample chromatogram, with control medicinal material chromatogram phaseOn the position of answering, the fluorescence spot of aobvious same color;
2) in this detection method, Gardenoside discriminating is: get this product, porphyrize, gets 2.5g, adds 75% ethanol 10ml, puts tepidariumIn soak 1-4 hour, filter, filtrate is concentrated into about 3ml, as need testing solution; Separately get Gardenoside reference substance, add ethanol and make often1ml is containing the solution of 5mg, product solution in contrast; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, point respectivelyOn same silica gel g thin-layer plate, taking ethyl acetate-acetone-formic acid-water (4-7:2-5:0.5-1:0.5-1) as solvent,Launch, take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 110 DEG C clear; In test sample chromatogram,On the corresponding position of reference substance chromatogram, the spot of aobvious same color;
3) in this detection method, gallic acid discriminating is: get this product, porphyrize, gets 1.8g, and the 50ml that adds water boils 30 minutes,Let cool, centrifugal (3000 revs/min) 5 minutes, get supernatant, extract 2 times with the ether jolting that hydrochloric acid is saturated, and each 15ml, mergesEther solution, volatilizes, and residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution; Separately get gallic acid reference substance, add methyl alcohol and makeEvery 1ml is containing the solution of 0.5mg, product solution in contrast; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, pointMore other on same silica gel g thin-layer plate, taking toluene (water saturation)-ethyl acetate-formic acid (4-7:2-5:0.5-1) as solvent,Launch, take out, dry, spray is with 1% ferric trichloride ethanolic solution; In test sample chromatogram, with the corresponding position of reference substance chromatogramUpper, the spot of aobvious same color;
4) in this detection method, Determination of Gardenoside assay method is: with octadecylsilane chemically bonded silica be filler; SecondNitrile-water (5-30:70-95) is mobile phase; Detection wavelength is 220-240nm; Number of theoretical plate calculates and should be not less than by Gardenoside peak1500; The preparation of reference substance solution, it is appropriate that precision takes Gardenoside reference substance, adds methyl alcohol and make the solution of every 1ml containing 30 μ g, shakesEven, to obtain final product; The preparation of need testing solution, gets this preparation under content uniformity, and porphyrize is got 0.65g, accurately weighed, puts the taper of tool plugIn bottle, precision adds methyl alcohol 25ml, close plug, and weighed weight, ultrasonic (power 250W, frequency 40Hz) processes 20 minutes, let cool, thenWeighed weight, supplies the weight of less loss with methyl alcohol, shake up, and filters, and precision measures subsequent filtrate 10ml, puts in 25ml measuring bottle, adds firstAlcohol, to scale, shakes up, and to obtain final product; Determination method, accurate reference substance solution and the each 10 μ l of need testing solution of drawing, inject liquid phase look respectivelySpectrometer, measures, and to obtain final product; Every, preparation contains cape jasmine by Gardenoside (C17H24O10), must not be less than 0.5-1.0mg.
Further, the detection method of a kind of Chinese medicine composition nephritislin capsule of the present invention, is characterized in that deservingReturn, Ligusticum wallichii differentiate concrete grammar be: get this product, porphyrize, gets 3.0g, adds n-hexane 25ml, ultrasonic (250W, 40Hz) process 30 pointsClock, filters, and filtrate is concentrated into about 1ml, as need testing solution; Separately get Ligusticum wallichii, the each 0.5g of Radix Angelicae Sinensis control medicinal material, respectively same legal systemBecome control medicinal material solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively in same silica G thin layerOn plate, taking benzinum (60～90 DEG C)-ethyl acetates (9:1) as solvent, launch, take out, dry, put ultraviolet lamp(365nm) under, inspect; In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
Further, the detection method of a kind of Chinese medicine composition nephritislin capsule of the present invention, is characterized in that this Cape jasmineSub-glycosides differentiates that concrete grammar is: get this product, porphyrize, gets 2.5g, adds 75% ethanol 10ml, puts in tepidarium and soaks 2 hours, filter,Filtrate is concentrated into about 3ml, as need testing solution; Separately get Gardenoside reference substance, add ethanol and make the solution of every 1ml containing 5mg, doFor reference substance solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively in same silica gel g thin-layer plateUpper, taking ethyl acetate-acetone-formic acid-water (5:5:1:1) as solvent, launch, take out, to dry, spray is with 10% sulfuric acid secondAlcoholic solution, is heated to spot colour developing at 110 DEG C clear; In test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious phaseWith the spot of color.
Further, the detection method of a kind of Chinese medicine composition nephritislin capsule of the present invention, is characterized in that this is notGallate-based differentiates that concrete grammar is: get this product, porphyrize, gets 1.8g, and the 50ml that adds water boils 30 minutes, lets cool, centrifugal (3000 turn/Point) 5 minutes, get supernatant, extract 2 times with the ether jolting that hydrochloric acid is saturated, each 15ml, merges ether solution, volatilizes, and residue addsMethyl alcohol 1ml makes to dissolve, as need testing solution; Separately get gallic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg,Product solution in contrast; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively in same silica G thin layerOn plate, taking toluene (water saturation)-ethyl acetate-formic acid (6:3:1) as solvent, launch, take out, dry, spray is with 1% trichlorineChange iron ethanolic solution; In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
Further, the detection method of a kind of Chinese medicine composition nephritislin capsule of the present invention, is characterized in that this Cape jasmineSub-glycosides assay concrete grammar is: with octadecylsilane chemically bonded silica be filler; Acetonitrile-water (18:85) is for flowingPhase; Detection wavelength is 238nm; Number of theoretical plate calculates and should be not less than 1500 by Gardenoside peak; The preparation of reference substance solution, accurate titleGet Gardenoside reference substance appropriate, add methyl alcohol and make the solution of every 1ml containing 30 μ g, shake up, to obtain final product; The preparation of need testing solution, getsThis preparation under content uniformity, porphyrize, gets 0.65g, accurately weighed, puts in tool plug conical flask, and precision adds methyl alcohol 25ml, close plug,Weighed weight, ultrasonic (power 250W, frequency 40Hz) processes 20 minutes, let cool, more weighed weight, supply the weight of less loss with methyl alcoholAmount, shakes up, and filters, and precision measures subsequent filtrate 10ml, puts in 25ml measuring bottle, adds methyl alcohol to scale, shakes up, and to obtain final product; Determination method, pointInaccurate reference substance solution and the each 10 μ l of need testing solution of drawing, injection liquid chromatography, measures, and to obtain final product; Every, preparation contains Cape jasmineSon, by Gardenoside (C17H24O10), must not be less than 0.75mg.
This method of quality control can carry out effective quality control to nephritislin preparation.
Ministry standard Central Plains nephritislin capsule quality standard only differentiates there is no content control to Poria cocos, tannin in prescriptionSystem, this method of quality control in proper mass standard base, increased discriminating, the Jasminoidin in G. jasminoides Ellis Var. Grandiflora of Radix Angelicae Sinensis and Ligusticum wallichii discriminating,The discriminating of gallic acid in garden burnet, and to effective ingredient Gardenoside (C17H24O10) meter in preparation, must not be less than 0.5-1.5mg.
Specific embodiment:
Eclipta 71.6g, fruit of glossy privet 43g, glutinous rehmannia 43g, Chinese yam 76.6g, Radix Angelicae Sinensis 43g, Ligusticum wallichii 14.4g, radix paeoniae rubrathe 28.8g,Rhizoma cibotii (scalding) 143g, Poria cocos 43g, umbellate pore furgus 43g, plantain seed (salt stir-fry) 86g, madder 43g, setose thistle 71.6g, field thistle 71.6g, cape jasmine43g, purslane 172g, garden burnet 143g, above 17 tastes, are ground into fine powder by Radix Angelicae Sinensis, Ligusticum wallichii, cape jasmine; All the other ecliptas etc. tenFour tastes, boiling secondary, 3 hours for the first time, 2 hours for the second time, collecting decoction, filtered, and filtrate is condensed into relative density and isThe thick paste of 1.30～1.35 (60 DEG C); Add above-mentioned medicinal powder, mix, dry, pulverize into fine powder, granulation, incapsulates, systemBecome 1000, to obtain final product, oral, 3 times on the one, one time 6～7, every is heavy 0.28 gram, the careful clothes of pregnant woman.
The method of quality control of nephritislin capsule is: a. differentiates 1: get this product, porphyrize, gets 3.0g, adds n-hexane 25ml, superSound (250W, 40Hz) is processed 30 minutes, filters, and filtrate is concentrated into about 1ml, as need testing solution. Separately get Ligusticum wallichii, Radix Angelicae Sinensis contrastThe each 0.5g of medicinal material, is made in the same way of respectively control medicinal material solution. According to thin-layered chromatography (" Chinese pharmacopoeia " 2010 editions annex IVB) test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with benzinum (60～90 DEG C)-Ethyl acetate (9:1) is solvent, launches, and takes out, and dries, and puts under ultraviolet lamp (365nm) and inspects. In test sample chromatogram,On the corresponding position of control medicinal material chromatogram, the fluorescence spot of aobvious same color.
B. differentiate 2: get this product, porphyrize, gets 2.5g, add 75% ethanol 10ml, put in tepidarium and soak 2 hours, filter filtrateBe concentrated into about 3ml, as need testing solution. Separately get Gardenoside reference substance, add ethanol and make the solution of every 1ml containing 5mg, as rightAccording to product solution. According to thin-layered chromatography (" Chinese pharmacopoeia " 2010 editions one annex IV B) test, draw each 10 μ of above-mentioned two kinds of solutionL, puts respectively on same silica gel g thin-layer plate, taking ethyl acetate-acetone-formic acid-water (5:5:1:1) as solvent, launches,Take out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 110 DEG C clear. In test sample chromatogram, with rightOn the corresponding position of product chromatogram, the spot of aobvious same color.
C. differentiate 3: get this product, porphyrize, gets 1.8g, the 50ml that adds water, boils 30 minutes, lets cool, centrifugal (3000 revs/min) 5Minute, get supernatant, extract 2 times with the ether jolting that hydrochloric acid is saturated, each 15ml, merges ether solution, volatilizes, and residue adds methyl alcohol1ml makes to dissolve, as need testing solution. Separately get gallic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, asReference substance solution. According to thin-layered chromatography (" Chinese pharmacopoeia " 2010 editions one annex IV B) test, draw above-mentioned two kinds of solution each10 μ l, put respectively on same silica gel g thin-layer plate, taking toluene (water saturation)-ethyl acetate-formic acid (6:3:1) as solvent,Launch, take out, dry, spray is with 1% ferric trichloride ethanolic solution. In test sample chromatogram, with the corresponding position of reference substance chromatogramUpper, the spot of aobvious same color.
D. assay: take high picture liquid chromatography (" Chinese pharmacopoeia " 2010 editions one annex IV D) and measure, chromatostripPart and system suitability test: with octadecylsilane chemically bonded silica be filler; Acetonitrile-water (15:85) is mobile phase; InspectionSurvey wavelength is 238nm. Number of theoretical plate calculates and should be not less than 1500 by Gardenoside peak; The preparation of reference substance solution, precision takes Cape jasmineSub-glycosides reference substance is appropriate, adds methyl alcohol and makes the solution of every 1ml containing 30 μ g, shakes up, and to obtain final product; The preparation of need testing solution, gets loading amountThis preparation under difference, porphyrize, gets 0.65g, accurately weighed, puts in tool plug conical flask, and precision adds methyl alcohol 25ml, and close plug is weighedWeight, ultrasonic (power 250W, frequency 40Hz) processing 20 minutes, lets cool, more weighed weight, supplies the weight of less loss with methyl alcohol,Shake up, filter, precision measures subsequent filtrate 10ml, puts in 25ml measuring bottle, adds methyl alcohol to scale, shakes up, and to obtain final product; Determination method, respectivelyAccurate reference substance solution and the each 10 μ l of need testing solution of drawing, injection liquid chromatography, measures, and to obtain final product. Every, preparation contains cape jasmineBy Gardenoside (C17H24O10), must not be less than 0.75mg.
Claims (5)
1. a detection method for Chinese medicine composition nephritislin capsule, this detection method relate to Radix Angelicae Sinensis in nephritislin capsule, Ligusticum wallichii,The concrete discrimination method of Gardenoside, gallic acid main active and Determination of Gardenoside assay method, is characterized in that:
1) in this detection method, Radix Angelicae Sinensis, Ligusticum wallichii discriminating are: get this product, porphyrize, gets 3.0g, adds n-hexane 25ml, ultrasonic 250W,40Hz processes 25-35 minute, filters, and filtrate is concentrated into about 1ml, as need testing solution; Separately get Ligusticum wallichii, Radix Angelicae Sinensis control medicinal material is each0.5g, is made in the same way of respectively control medicinal material solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, point respectivelyOn same silica gel g thin-layer plate, taking 60～90 DEG C-ethyl acetate of benzinum 9-9.5:0.5-1 as solvent, launch, take out,Dry, put under ultraviolet lamp 340-380nm and inspect; In test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, aobvious phaseWith the fluorescence spot of color;
2) in this detection method, Gardenoside discriminating is: get this product, porphyrize, gets 2.5g, adds 75% ethanol 10ml, puts in tepidarium and soaks1-4 hour, filters, and filtrate is concentrated into about 3ml, as need testing solution; Separately get Gardenoside reference substance, add ethanol and make every 1mlContaining the solution of 5mg, product solution in contrast; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively in sameOn one silica gel g thin-layer plate, taking ethyl acetate-acetone-formic acid-water 4-7:2-5:0.5-1:0.5-1 as solvent, launch, getGo out, dry, spray, with 10% ethanol solution of sulfuric acid, is heated to spot colour developing at 110 DEG C clear; In test sample chromatogram, with contrastOn the corresponding position of product chromatogram, the spot of aobvious same color;
3) in this detection method, gallic acid discriminating is: get this product, porphyrize, gets 1.8g, and the 50ml that adds water boils 30 minutes, let cool,Centrifugal 3000 revs/min 5 minutes, get supernatant, extract 2 times with the saturated ether jolting of hydrochloric acid, each 15ml, merges ether solution,Volatilize, residue adds methyl alcohol 1ml to be made to dissolve, as need testing solution; Separately get gallic acid reference substance, add methyl alcohol and make every 1ml and containThe solution of 0.5mg, in contrast product solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively in sameOn one silica gel g thin-layer plate, taking water saturation toluene-ethyl acetate-formic acid 4-7:2-5:0.5-1 as solvent, launch, take out, dry in the airDry, spray is with 1% ferric trichloride ethanolic solution; In test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same colorSpot;
4) in this detection method, Determination of Gardenoside assay method is: with octadecylsilane chemically bonded silica be filler; Acetonitrile-Water 5-30:70-95 is mobile phase; Detection wavelength is 220-240nm; Number of theoretical plate calculates and should be not less than 1500 by Gardenoside peak;The preparation of reference substance solution, it is appropriate that precision takes Gardenoside reference substance, adds methyl alcohol and make the solution of every 1ml containing 30 μ g, shakes up,; The preparation of need testing solution, gets this preparation under content uniformity, and porphyrize is got 0.65g, accurately weighed, put in tool plug conical flask,Precision adds methyl alcohol 25ml, close plug, and weighed weight, ultrasonic power 250W, frequency 40Hz processes 20 minutes, lets cool, more weighed heavyMeasure, supply the weight of less loss with methyl alcohol, shake up, filter, precision measures subsequent filtrate 10ml, puts in 25ml measuring bottle, adds methyl alcohol to carvingDegree, shakes up, and to obtain final product; Determination method, accurate reference substance solution and the each 10 μ l of need testing solution of drawing respectively, injection liquid chromatography,Measure, to obtain final product.
2. a kind of detection method of Chinese medicine composition nephritislin capsule according to claim 1, is characterized in that this Radix Angelicae Sinensis, riverRhizome of chuanxiong differentiates that concrete grammar is: get this product, porphyrize, gets 3.0g, adds n-hexane 25ml, ultrasonic 250W, and 40Hz processes 30 minutes, filterCross, filtrate is concentrated into about 1ml, as need testing solution; Separately get Ligusticum wallichii, the each 0.5g of Radix Angelicae Sinensis control medicinal material, it is right to be made in the same way of respectivelyAccording to medicinal material solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate,Taking 60～90 DEG C-ethyl acetate of benzinum 9:1 as solvent, launch, take out, dry, put under ultraviolet lamp 365nm and inspect; SupplyIn test product chromatogram, with the corresponding position of control medicinal material chromatogram on, the fluorescence spot of aobvious same color.
3. a kind of detection method of Chinese medicine composition nephritislin capsule according to claim 1, is characterized in that this GardenosideDiscriminating concrete grammar is: get this product, porphyrize, gets 2.5g, adds 75% ethanol 10ml, puts in tepidarium and soaks 2 hours, filters filtrateBe concentrated into about 3ml, as need testing solution; Separately get Gardenoside reference substance, add ethanol and make the solution of every 1ml containing 5mg, as rightAccording to product solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, withEthyl acetate-acetone-formic acid-water 5:5:1:1 is solvent, launches, and takes out, and dries, spray with 10% ethanol solution of sulfuric acid,Be heated to spot colour developing at 110 DEG C clear; In test sample chromatogram, with the corresponding position of reference substance chromatogram on, aobvious same colorSpot.
4. a kind of detection method of Chinese medicine composition nephritislin capsule according to claim 1, is characterized in that this nutgallAcid differentiates that concrete grammar is: get this product, porphyrize, gets 1.8g, and the 50ml that adds water boils 30 minutes, lets cool centrifugal 3000 revs/min 5 pointsClock, gets supernatant, extracts 2 times with the ether jolting that hydrochloric acid is saturated, and each 15ml, merges ether solution, volatilizes, and residue adds methyl alcohol1ml makes to dissolve, as need testing solution; Separately get gallic acid reference substance, add methyl alcohol and make the solution of every 1ml containing 0.5mg, asReference substance solution; According to thin-layered chromatography test, draw the each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate,Taking water saturation toluene-ethyl acetate-formic acid 6:3:1 as solvent, launch, take out, dry, spray molten with 1% ferric trichloride ethanolLiquid; In test sample chromatogram, with the corresponding position of reference substance chromatogram on, the spot of aobvious same color.
5. a kind of detection method of Chinese medicine composition nephritislin capsule according to claim 1, is characterized in that this GardenosideAssay concrete grammar is: with octadecylsilane chemically bonded silica be filler; Acetonitrile-water 18:85 is mobile phase; DetectWavelength is 238nm; Number of theoretical plate calculates and should be not less than 1500 by Gardenoside peak; The preparation of reference substance solution, precision takes cape jasmineGlycosides reference substance is appropriate, adds methyl alcohol and makes the solution of every 1ml containing 30 μ g, shakes up, and to obtain final product; The preparation of need testing solution, gets loading amount poorDifferent lower preparation, porphyrize, gets 0.65g, accurately weighed, puts in tool plug conical flask, and precision adds methyl alcohol 25ml, and close plug is weighed heavyAmount, ultrasonic power 250W, frequency 40Hz processing 20 minutes, lets cool, more weighed weight, supplies the weight of less loss with methyl alcohol, shake up,Filter, precision measures subsequent filtrate 10ml, puts in 25ml measuring bottle, adds methyl alcohol to scale, shakes up, and to obtain final product; Determination method, respectively accurate suctionGet the each 10 μ l of reference substance solution and need testing solution, injection liquid chromatography, measures, and to obtain final product.
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| US4257776A (en) * | 1980-01-21 | 1981-03-24 | The United States Of America As Represented By The Secretary Of The Army | Method of visually detecting antioxidant in an organic mixture |
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| US4257776A (en) * | 1980-01-21 | 1981-03-24 | The United States Of America As Represented By The Secretary Of The Army | Method of visually detecting antioxidant in an organic mixture |
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| 乳癖散结片质量标准研究;刘明等;《时珍国医国药》;20071231;第18卷(第8期);1983-1985 * |
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