CN102841095A - Quality testing method for Liuwei Mingmu preparation of Tibetan medicine composition - Google Patents
Quality testing method for Liuwei Mingmu preparation of Tibetan medicine composition Download PDFInfo
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Abstract
The invention discloses a quality testing method for a Liuwei Mingmu preparation of a Tibetan medicine composition. The preparation comprises various preparations prepared by prepared ferrous powder, cortex berberidis, carum carvi, fructus chebulae, fructus terminaliae billericae and phyllanthus emblica according to a conventional pharmaceutical method. The quality testing method comprises a content testing method of the ferrous powder and/or a content testing method of gallic acid. According to the quality testing method for the Liuwei Mingmu preparation of the Tibetan medicine composition, the iron content in the Liuwei Mingmu tablets of the Tibetan medicine composition is detected at the first time, the iron content in the Liuwei Mingmu tablets of the Tibetan medicine composition is tested through a mercury-free potassium dichromate titration method which is convenient, quick and accurate to use and operate, and the active constituent gallic acid in the Liuwei Mingmu tablets of the Tibetan medicine composition is quantitatively tested through a high performance liquid chromatography. With the adoption of the method provided by the invention, the content testing method of the iron and the content testing method of the Liuwei Mingmu tablets of the Tibetan medicine composition is increased, the quality of the Liuwei Mingmu preparation of the Tibetan medicine composition can be ensured, and the preparation can be guaranteed to be safe, effective, stable and controllable in quality.
Description
Technical field
The present invention relates to a kind of quality determining method of Tibetan medicine composite preparation, the make eye bright quality determining method of preparation of particularly a kind of Tibetan medicine composition Six-element.
Background technology
At present, because the variation of living environment, working pressure, eating habit makes numerous illness in eye be state occurred frequently.Popularizing of Internet, the incorrect eye custom of using is more and more grown in strength the visual fatigue crowd, and annual growth has reached 25%.The Tibetan medicine thinks that the red crust high (liver-fire flaming) that is of illness in eye injures due to the grand functional disturbance disorder of dimension life that can look red crust function and Si Li transmission body light.According to this theory; Scold unit initiations such as Tibetan medicine by northwest plateau biological study institute, Qinghai Tibetan medicine and pharmacology research institute, gold; In conjunction with traditional handicraft and modern science and technology, developed the LIUWEI MINGMU WAN of treatment cataract, vitreous opacity, chronic conjunctivitis and keratitis etc.
LIUWEI MINGMU WAN records in Chinese patent drug provincial standard rising national standard part, standard numbering: WS-10787 (ZD-0787)-2002.LIUWEI MINGMU WAN is made up of 6 flavor medicines such as iron powder (system), barberry skin, Caraway, myrobalan, terminaliae billericae,fructus, emblic; Cure mainly ophthalmology class diseases such as cataract, glaucoma, diabetic keratopathy retinopathy, macular degeneration, chronic conjunctivitis, keratitis, xerophthalmia, effect is obvious.The Tibetan medicine thinks, has to regulate to look into redly, and heat-clearing disappears dim, and the effect that nourishes the liver to improve visual acuity is used to look into red hot eyes photophobia, the epiphora induced by wind, the blurred vision that causes.The traditional Chinese medical science is thought, clearing heat-fire, and the effect that flat liver makes eye bright is used for that red eye, swell pain, photophobia due to the liver-fire flaming shed tears, blurring of vision.
Iron powder is a monarch drug in a prescription in the LIUWEI MINGMU WAN prescription." Kaibao Bencao " record iron powder has tranquilizing mind, hard marrow, effects such as profit skin.Iron is the trace element of human body, has vital role such as the erythropoiesis of promotion.Used iron powder is after concocting, to be used as medicine in Tibetan medicine composition LIUWEI MINGMU WAN and the pharmaceutical formulation thereof, helps more absorbing.But the iron Excessive Intake possibly cause acute iron poisoning, and severe patient possibly cause shock, and is dead even.Therefore in order to guarantee patient's safe medication, should control, when reaching the treatment disease, not cause other healthy hidden danger the content of iron.The LIUWEI MINGMU WAN primary standard has only Berberine hydrochloride discriminating, berberine hydrochloride content item; Iron content mensuration item in the monarch drug in a prescription iron powder in not square; And a large amount of gallic acids that myrobalan, terminaliae billericae,fructus, emblic do not contain among the other side carry out assay, thereby can not guarantee the safe, effective of said preparation.
Summary of the invention
The objective of the invention is for overcoming the deficiency of above-mentioned prior art the quality determining method that provides a kind of Tibetan medicine composition Six-element to make eye bright preparation.
The invention provides a kind of Tibetan medicine composition Six-element control method of iron content in the iron powder that makes eye bright in the preparation, the content assaying method of gallic acid guarantees that iron content is inexcessive, makes said preparation in effective treatment disease, guarantees the security of medication.
Iron powder (system) is the routine techniques term of Tibetan medicine, and " system " in the bracket is to concoct according to the method for " Qinghai Province's Tibetan medicine concocted specification " (food and medicine Surveillance Authority in Qinghai Province's compiles, the versions in 2010 that the Qinghai People's Press publishes) lining.
The term explanation:
Six-element makes eye bright that preparation (or cry " LIUWEI MINGMU WAN and preparation thereof ") comprises LIUWEI MINGMU WAN and with other preparations of LIUWEI MINGMU WAN bulk drug formulation; Like eyesight-improving granule with six ingredients, eyesight-improving capsule with six ingredients, the Six-element sheet etc. that makes eye bright; The proportioning of the bulk drug of each preparation can be identical with LIUWEI MINGMU WAN, also can carry out suitable adjustment according to the treatment needs.
For realizing above-mentioned purpose, the present invention adopts following technical proposals:
The make eye bright quality determining method of preparation of a kind of Tibetan medicine composition Six-element; The various preparations of said preparation for being processed by the pharmacy conventional method by iron powder (system), barberry skin, Caraway, myrobalan, terminaliae billericae,fructus, emblic, quality determining method comprises the content assaying method of iron powder in the preparation and/or the content assaying method of gallic acid.
The present invention makes contributions to the Six-element assay of iron powder that makes eye bright in the preparation, and the content assaying method of its iron powder is, after preparation ashing to be determined, with the concentrated hydrochloric acid dissolving, adds the methyl orange indicator solution, drips stannous chloride solution with Fe
3+Be reduced to Fe
2+, solution becomes pale red, is indicator with the diphenylamine sulfonic acid sodium salt then, is purple with potassium dichromate standard solution titration to solution and is terminal point, calculates the content of iron powder with the amount of known potassium dichromate standard solution.
Further, the content assaying method concrete steps of said iron powder are: it is an amount of to get LIUWEI MINGMU WAN preparation powder, and accurate the title decides; The crucible that fills sample is put slowly vehement burning on the electric furnace, blazing to the whole charings of test sample, black in color; And no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1 ~ 5ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 500 ~ 700 ℃ blazing 3 ~ 5 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, 60 ~ 70 ℃ of left and right sides heating for dissolving 3 ~ 5 hours; After the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle, and thin up is to scale; Shake up, accurate amount 25ml puts in the 250ml conical flask, adds the 8ml concentrated hydrochloric acid solution; Be heated to nearly boiling, add 6 methyl orange indicator solutions after, drip ratio of quality and the number of copies 5% stannous chloride solution to solution while hot while shaking and become pale pink, take off if shake the back pink colour; Then add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 2 ~ 10ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions, fixed with the dichromate titration drop immediately.
The preparation method of said mixture of sulfuric phosphoric acid solution is: 150ml concentration expressed in percentage by volume 95% ~ 98% concentrated sulphuric acid is under agitation slowly injected 500ml water, add 150ml phosphoric acid after the cooling again, be diluted with water to 1000ml, mixing promptly gets.
The present invention makes eye bright to Six-element, and the technical scheme that provides of the assay of gallic acid is in the preparation: the content assaying method of said gallic acid is; Get gallic acid reference substance adding volume parts and be mixed with reference substance solution than 50% methanol aqueous solution; Getting preparation adding volume parts to be detected and be mixed with need testing solution than 50% methanol aqueous solution, is filling agent with the octadecylsilane chemically bonded silica; Is moving phase than the methyl alcohol-volume parts of 2～6:98～94 than 1% glacial acetic acid aqueous solution with volume parts; Detecting wavelength is the high performance liquid chromatography of 270 ~ 280nm.
Further, the assay of said gallic acid is specifically:
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D);
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than the methyl alcohol-volume parts of 2～6:98～94 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 270 ~ 280nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get preparation powder 0.5 ~ 1.5g to be detected, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution, 20 ~ 30ml; Close plug is claimed to decide weight, ultrasonic 20 ~ 40 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 5 ~ 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
The Six-element that bulk drug was formed below the present invention the was preferred preparation that makes eye bright: iron powder (system) 132.0 weight portions, barberry skin 132.0 weight portions, Caraway 132.0 weight portions, myrobalan's 66.5 weight portions, terminaliae billericae,fructus 66.5 weight portions, emblic 66.5 weight portions.
For above-mentioned preferred preparation, quality determining method is:
A. the assay of iron powder:
It is an amount of to get the LIUWEI MINGMU WAN powder, and accurate the title decides, and the crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), and be blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, (shook frequently in 4 hours 65 ℃ of left and right sides heating for dissolving; Avoid boiling), after the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle; Thin up shakes up to scale, and accurate amount 25ml puts in the 250ml conical flask; Add the 8ml concentrated hydrochloric acid solution, be heated to nearly boiling, adds 6 methyl orange indicator solutions after, dropping ratio of quality and the number of copies 5% stannous chloride solution to solution becomes pale pink while shaking while hot; Take off if shake the back pink colour, can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions, fixed with the dichromate titration drop immediately.
B. the assay of gallic acid:
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D);
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than methyl alcohol-volume parts of 4:96 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 275nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get Tibetan medicine composition LIUWEI MINGMU WAN powder 1g, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution 25ml; Close plug is claimed to decide weight, ultrasonic 30 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
Iron content is 13.2mg/g ~ 22.1mg/g in the assay project of said iron powder; Gallic acid content (C in the assay project of said gallic acid
7H
6O
5) must not be less than 1.83mg/g.
Described preparation is meant gets Tibetan medicine composition LIUWEI MINGMU WAN bulk drug, presses common process, adds conventional auxiliary material and is prepared into clinical acceptable any formulation, comprises micropill, dripping pill, tablet, capsule, particle, medicine materical crude slice or dispersing tablet.
These article gallic acid content (C
7H
6O
5) must not be less than 1.83mg/g.
The unit corresponding relation of weight portion described in this instructions and parts by volume is g/ml or kg/l.
The present invention detects the content of iron in the Tibetan medicine composition LIUWEI MINGMU WAN for the first time; Use easy and simple to handle, do not have the mercury dichromate method fast and accurately the iron in the Tibetan medicine composition LIUWEI MINGMU WAN carried out content detection, adopt high performance liquid chromatography that effective constituent gallic acid in the Tibetan medicine composition LIUWEI MINGMU WAN has been carried out quantitative measurement.The inventive method can guarantee the quality of Tibetan medicine composition LIUWEI MINGMU WAN, guarantees said preparation safety, effective, stable, quality controllable.Simultaneously this law also can be used for other preparations of LIUWEI MINGMU WAN, like eyesight-improving granule with six ingredients, eyesight-improving capsule with six ingredients, the Six-element sheet etc. that makes eye bright.
For further verifying beneficial effect of the present invention, the present invention provides following experimental example.
Experimental example 1: the assay experiment of iron
1. instrument, reagent and confession test agent
Instrument: BT125D Sai Duolisi electronic analytical balance (German Sai Duolisi sartorius company); 2.5-10 molding box formula resistance furnace (the bright forever medical apparatus and instruments factory in Beijing); HH-4 digital display thermostat water bath (Changzhou Rong Guan experimental analysis instrument plant).Main agents: (take by weighing stannous chloride and be dissolved in the 40ml concentrated hydrochloric acid, thin up is to 100ml for 5% stannous chloride solution.Face with one times of preceding dilute with water, promptly get); Methyl orange indicator solution (get methyl orange 0.1g and be dissolved in the 100ml water, promptly get); Diphenylamine sulfonic acid sodium salt indicator solution (get diphenylamine sulfonic acid sodium salt 0.2g and be dissolved in the 100ml water, promptly get); Mixture of sulfuric phosphoric acid solution (the 150ml concentrated sulphuric acid is under agitation slowly injected 500ml water, add 150ml phosphoric acid after the cooling again, be diluted with water to 1000ml, mixing promptly gets).(standard reagent is stored in the exsiccator in 150 ~ 160 ℃ of dryings 2 hours the potassium dichromate standard solution, accurately takes by weighing the 0.0980g potassium dichromate in the 250ml beaker; Quantitatively change in the 1000ml volumetric flask after adding the suitable quantity of water dissolving; Be diluted with water to scale, shake up, its concentration is 0.002mol/l).
Sample: LIUWEI MINGMU WAN (the Qinghai gold is scolded Tibetan medicine medicine company incorporated company and provided), lot number is respectively: 20100201,20100202,20100203.
2. the ashing of sample
The crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.Dropping sulfuric acid is an amount of, makes carbide all moistening, is excellent with 0.5ml to 2ml, and wherein 1ml is optimum.Continue to be heated to steam and eliminate, white cigarette emits to the greatest extent, and is blazing 3 ~ 5 hours in 500 ~ 700 ℃.Wherein with 600 ℃ blazing 4 hours be optimum.The charing purpose is: remove the interference of other flavour of a drug in the Tibetan medicinal preparation, make iron be converted into Fe simultaneously
3+, be convenient to measure.
3. the selection of concentration of hydrochloric acid
Be reflected in hydrochloric acid (HCl) medium and carry out, reduction Fe
3+The time hydrochloric acid (HCl) concentration with 4mol/l for well, Sn during greater than 6mol/l
2+Then reduction methyl orange is colourless earlier, makes it can't indicate Fe
3+Reduction, Cl simultaneously
-Excessive concentration also possibly consume K
2Cr
2O
7, HCl concentration be lower than 2mol/l then methyl orange fade slowly.
4. dissolve the selection of appearance temperature
Molten appearance temperature has considerable influence to the mensuration result of iron content.When a molten appearance temperature is lower than 55 ℃, dissolve appearance slowly; It is too fast to surpass 75 ℃ of HCl volatilizations, and concentration reduces, and dissolves appearance not exclusively.Experiment shows that dissolving the appearance temperature is controlled at 65 ℃ of left and right sides best results.
5. redox temperature controlling
When reducing with stannous chloride, temperature should be controlled at 70～80 ℃, and constantly shakes.And in last oxidimetric titration, solution temperature should be controlled at 20～30 ℃ for well, so that reaction can comparatively fast be carried out.
6. the selection of mixture of sulfuric phosphoric acid solution
The Fe that generates in the titration process
3+Be yellow, influence the observation of terminal point, if in solution, add phosphoric acid (H
3PO
4), H
3PO
4With Fe
3+Generate colourless Fe (HPO4)
2-, can shelter Fe
3+Simultaneously because Fe (HPO4)
2-Generation, make Fe
3+/ Fe
2+The right conditional potential of electricity reduces, and titration jump increases, and indicator can variable color in mutation range, thereby reduces titration error.
7. principle
These article sample is behind sample ashing, dissolving with hydrochloric acid, and iron wherein is converted into Fe
3+Under strong acidic condition, Fe
3+Can pass through SnCl
2Be reduced to Fe
2+Sn
2+With Fe
3+After reduction finished, methyl orange also can be by Sn
2+Be reduced into hydrogenation methyl orange and fade, thereby methyl orange can be indicated Fe
3+The reduction terminal point.Sn
2+Can also continue to make hydrogenation methyl orange to be reduced into N, N-dimethyl-p-phenylenediamine and sodium sulfanilate.Its reaction equation is:
(CH
3)
2NC
6H
4N=NC
6H
4SO
3Na+2e+2H
+→(CH
3)
2NC
6H
4NH-NHC
6H
4SO
3Na
(CH
3)
2NC
6H
4NH-NHC
6H
4SO
3Na＋2e
-＋2H
+→(CH
3)
2NC
6H
4NH
2+NH
2C
6H
4SO
3Na
So, slightly excessive Sn
2+Also be eliminated.Because above-mentioned reaction is irreversible, so the reduzate of methyl orange does not consume K
2Cr
2O
7After having reacted, be indicator, use K with the diphenylamine sulfonic acid sodium salt
2Cr
2O
7Standard solution titration to solution is purple and is terminal point, and the key reaction formula is following:
2FeCl
4 -+SnCl
2-+2Cl
-=2FeCl
4 2-+SnCl
6 2-
6Fe
2++Cr
2O
7 2-+14H
+=6Fe
3++2Cr
3++7H
2O
8. the assay of iron in the sample
Get LIUWEI MINGMU WAN powder 0.5g, the accurate title, decide, and the crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), and be blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, (shook frequently in 4 hours 65 ℃ of left and right sides heating for dissolving; Avoid boiling), after the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle; Thin up shakes up to scale, and accurate amount 25ml puts in the 250ml conical flask; Add the 8ml concentrated hydrochloric acid solution, be heated to nearly boiling, adds 6 methyl orange indicator solutions after, dropping ratio of quality and the number of copies 5% stannous chloride solution to solution becomes pale pink while shaking while hot; Take off if shake the back pink colour, can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions are used dichromate titration liquid (0.002mol/l) titration immediately.Every 1ml dichromate titration liquid (0.002mol/l) is equivalent to the iron of 0.6702mg.The result sees table 1.
Iron content is measured the result in table 1 LIUWEI MINGMU WAN
9. reappearance test
Get with a collection of LIUWEI MINGMU WAN sample (product batch number: 20100201), accurate claim surely, totally 6 parts, measure according to the iron content determination method respectively.The result shows that this method repeatability is good.The result sees table 2.
Iron content is measured replica test in table 2 LIUWEI MINGMU WAN
10. the iron content of iron powder blank sample is measured
Do not contain the sample of iron powder in the ratio autogamy of Tibetan medicine composition LIUWEI MINGMU WAN prescription consumption, get the about 0.5g of this blank sample, the accurate title calmly; The accurate about 0.1g of standard iron powder that adds known content; Carry out ashing treatment, measure content and calculate recovery rate as stated above.The result shows that it is accurate that this assay method is measured the result.See table 3.
Table 3 iron powder blank sample iron content is measured the result
Experimental example 2: the assay experiment of gallic acid
1. instrument, reagent and confession test agent
Instrument: 1220 type Agilent high performance liquid chromatographs; Tianjin, island AuW220D electronic balance.
Reference substance: gallic acid reference substance (Nat'l Pharmaceutical & Biological Products Control Institute) lot number: 110831-200803.
Sample: LIUWEI MINGMU WAN (the Qinghai gold is scolded Tibetan medicine medicine company incorporated company and provided), lot number is respectively: 20100201,20100202,20100203.
2. detect the selection of wavelength
Get the gallic acid reference substance solution, in the 190-400nm wavelength coverage, scan, according to ultraviolet absorpting spectrum, selected 275nm is for detecting wavelength.
3. moving phase is selected
Discover, when being moving phase than the methyl alcohol-volume parts of 2～6:98～94 than 1% glacial acetic acid aqueous solution, all can reach good chromatographic resolution effect with volume parts.Be that 4:96 is that moving phase is optimum than the volume ratio of 1% glacial acetic acid aqueous solution wherein, about relative retention time 7.5min with methyl alcohol-volume parts.
4. system suitability test
Under above-mentioned chromatographic condition, accurate respectively reference substance solution, each 10 μ l of need testing solution of drawing inject liquid chromatograph, the record chromatogram.The result shows that the degree of separation that gallic acid is adjacent chromatographic peak in reference substance, the test sample chromatogram is all greater than 1.5.The result sees Fig. 1, Fig. 2.
5. reference substance preparation
It is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets.
6. test sample preparation
6.1 the investigation of method for distilling
By method under the assay item need testing solution is detected.According to the preparation of the test solution was prepared under the three copies, respectively, ultrasound, reflux, vibration rockers for 30 minutes.Content with gallic acid in every gram medicine is that index is confirmed method for distilling.The result sees table 4.
Table 4 method for distilling is investigated test findings
The result shows, the content basically identical of gallic acid considers that ultrasonic Extraction is easy, easy to operate in ultrasonic and the every gram medicine of refluxing extraction gained, is ultrasonic Extraction so select method for distilling for use.
6.2 extract the investigation of solvent
By method under the assay item need testing solution is detected.The method for preparing under the item of pressing need testing solution prepares 3 parts, and precision adds entry, volume parts than 50% methanol aqueous solution, each 25ml of methyl alcohol respectively.Content with gallic acid in every gram medicine is that index confirms to extract solvent.The result sees table 5.
Table 5 extracts solvent and investigates test findings
The result shows, the gallic acid content basically identical that volume parts is surveyed than 50% methanol aqueous solution and methyl alcohol because pure methyl alcohol toxicity is bigger, is that volume parts is than 50% methanol aqueous solution so select the extraction solvent for use.
6.3 the investigation of extraction time
By method under the assay item need testing solution is detected.The method for preparing under the item of pressing need testing solution prepares 3 parts, and sonicated is 20 minutes, 30 minutes, 40 minutes respectively.Content with gallic acid in every gram medicine is that index is confirmed extraction time.The result sees table 6.
Table 6 extraction time investigation test findings
The result shows, the content basically identical of gallic acid is 30 minutes so select extraction time for use in ultrasonic Extraction 30 minutes and the 40 minutes every gram medicines of gained.
7. the investigation of the preparation of typical curve and linear relationship
Precision is measured gallic acid reference substance stock solution solution (gallic acid content is 185.6 μ g/ml) 1ml, 3ml, 5ml, 8ml, 10ml; Put respectively in the 10ml volumetric flask, volume parts is diluted to scale than 50% methanol aqueous solution, shakes up; Each accurate sample introduction 10 μ l; With peak area (A) reference substance concentration (C) is carried out linear regression, get gallic acid regression equation: A=75.648C-28.439, related coefficient: R=0.9997.The result shows that gallic acid is in 18.56 μ g/ml ~ 185.60 μ g/ml scopes, and the peak area of gallic acid (A) is good with reference substance concentration (C) linear relationship.The result sees table 7, Fig. 3.
Table 7 gallic acid linear relationship is investigated the result
8. precision test
The accurate gallic acid reference substance solution 10 μ l that draw inject liquid chromatograph, each METHOD FOR CONTINUOUS DETERMINATION 6 times, and the record peak area also calculates relative standard deviation.The result shows that instrument precision is good.The result sees table 8.
Table 8 gallic acid Precision test result
9. stability test
After the need testing solution preparation was accomplished, the accurate 10 μ l that draw injected liquid chromatograph, and the record peak area was whenever measured once at a distance from 2 hours later on, investigated 8 hours, and the record peak area also calculates relative standard deviation.The result shows, in 8 hours, to measure the result stable for gallic acid in the need testing solution.The result sees table 9.
Table 9 gallic acid stability test result
10. replica test
Get with a collection of LIUWEI MINGMU WAN sample (product batch number: 20100201) 1g, accurate claim fixed, totally 6 parts; The method for preparing under the item by need testing solution prepares need testing solution; The accurate respectively 10 μ l that draw inject liquid chromatograph, the content of gallic acid in the calculation sample.The result shows that this analytical approach repeatability is good.The result sees table 10.
Table 10 gallic acid replica test result
11. recovery test
Precision takes by weighing that (product batch number: 20100201) 6 parts, each accurate gallic acid reference substance that adds is measured its content, calculate recovery rate with a collection of LIUWEI MINGMU WAN sample.The result shows that it is accurate that this assay method is measured the result.The result sees table 11.
Table 11 gallic acid recovery test result
12. sample determination
Get three batches of Tibetan medicine composition LIUWEI MINGMU WANs, measure and calculate gallic acid content.The result sees table 12.
Table 12 sample size is measured the result
Following embodiment all can realize the described effect of above-mentioned experimental example.
Description of drawings
Fig. 1 is a gallic acid contrast high-efficient liquid phase chromatogram;
Fig. 2 is a Tibetan medicine composition LIUWEI MINGMU WAN test sample high-efficient liquid phase chromatogram;
Fig. 3 is the gallic acid linear relationship chart;
Wherein, the horizontal ordinate of Fig. 1, Fig. 2 is the time, unit: minute (min); Ordinate is absorbance (mAU).
Embodiment
Below in conjunction with embodiment the present invention is done detailed elaboration, but be not limited to the embodiment of these concrete records.The Tibetan medicine composition LIUWEI MINGMU WAN that is detected is scolded Tibetan medicine medicine company incorporated company product for the Qinghai gold and is sold.
Embodiment 1: the LIUWEI MINGMU WAN quality testing
A. iron content is measured:
Get LIUWEI MINGMU WAN powder 0.5g, the accurate title, decide, and the crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), and be blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, (shook frequently in 4 hours 65 ℃ of left and right sides heating for dissolving; Avoid boiling), after the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle; Thin up shakes up to scale, and accurate amount 25ml puts in the 250ml conical flask; Add the 8ml concentrated hydrochloric acid solution, be heated to nearly boiling, adds 6 methyl orange indicator solutions after, dropping ratio of quality and the number of copies 5% stannous chloride solution to solution becomes pale pink while shaking while hot; Take off if shake the back pink colour, can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions are used dichromate titration liquid (0.002mol/l) titration immediately.Every 1ml dichromate titration liquid (0.002mol/l) is equivalent to the iron of 0.6702mg.
These article iron content is 13.2mg/g ~ 22.1mg/g.
B. gallic acid content is measured:
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D);
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than methyl alcohol-volume parts of 4:96 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 275nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get Tibetan medicine composition LIUWEI MINGMU WAN powder 1g, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution 25ml; Close plug is claimed to decide weight, ultrasonic 30 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
These article gallic acid content (C
7H
6O
5) must not be less than 1.83mg/g.
Embodiment 2: the eyesight-improving granule with six ingredients quality testing
A. iron content is measured:
Get eyesight-improving granule with six ingredients powder 0.5g, the accurate title, decide, and the crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), and be blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, (shook frequently in 4 hours 65 ℃ of left and right sides heating for dissolving; Avoid boiling), after the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle; Thin up shakes up to scale, and accurate amount 25ml puts in the 250ml conical flask; Add the 8ml concentrated hydrochloric acid solution, be heated to nearly boiling, adds 6 methyl orange indicator solutions after, dropping ratio of quality and the number of copies 5% stannous chloride solution to solution becomes pale pink while shaking while hot; Take off if shake the back pink colour, can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions are used dichromate titration liquid (0.002mol/l) titration immediately.Every 1ml dichromate titration liquid (0.002mol/l) is equivalent to the iron of 0.6702mg.
These article iron content is 13.2mg/g ~ 22.1mg/g.
B. gallic acid content is measured:
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D);
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than methyl alcohol-volume parts of 4:96 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 275nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get Tibetan medicine composition eyesight-improving granule with six ingredients powder 1g, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution 25ml; Close plug is claimed to decide weight, ultrasonic 30 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
These article gallic acid content (C
7H
6O
5) must not be less than 1.83mg/g.
Described Tibetan medicine composition eyesight-improving granule with six ingredients is meant with LIUWEI MINGMU WAN bulk drug prescription iron powder (system) 132.0g, barberry skin 132.0g, Caraway 132.0g, myrobalan 66.5g, terminaliae billericae,fructus 66.5g, emblic 66.5g; Add conventional auxiliary material, according to the granule of common process preparation.
Embodiment 3: the eyesight-improving capsule with six ingredients quality testing
A. iron content is measured:
Get eyesight-improving capsule with six ingredients content powder 0.5g, the accurate title, decide, and the crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), and be blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, (shook frequently in 4 hours 65 ℃ of left and right sides heating for dissolving; Avoid boiling), after the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle; Thin up shakes up to scale, and accurate amount 25ml puts in the 250ml conical flask; Add the 8ml concentrated hydrochloric acid solution, be heated to nearly boiling, adds 6 methyl orange indicator solutions after, dropping ratio of quality and the number of copies 5% stannous chloride solution to solution becomes pale pink while shaking while hot; Take off if shake the back pink colour, can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions are used dichromate titration liquid (0.002mol/l) titration immediately.Every 1ml dichromate titration liquid (0.002mol/l) is equivalent to the iron of 0.6702mg.
These article iron content is 13.2mg/g ~ 22.1mg/g.
B. gallic acid content is measured:
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D);
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than methyl alcohol-volume parts of 4:96 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 275nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get Tibetan medicine composition eyesight-improving capsule with six ingredients content powder 1g, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution 25ml; Close plug is claimed to decide weight, ultrasonic 30 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
These article gallic acid content (C
7H
6O
5) must not be less than 1.83mg/g.
Described Tibetan medicine composition eyesight-improving capsule with six ingredients is meant with LIUWEI MINGMU WAN bulk drug prescription iron powder (system) 132.0g, barberry skin 132.0g, Caraway 132.0g, myrobalan 66.5g, terminaliae billericae,fructus 66.5g, emblic 66.5g; Add conventional auxiliary material, according to the capsule of common process preparation.
Embodiment 4: the Six-element tablet quality that makes eye bright detects
A. iron content is measured:
Get the Six-element sheet powder 0.5g that makes eye bright, accurately claim surely, the crucible that fills sample is put slowly vehement burning on the electric furnace (avoiding burning, expanding, overflow), blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature.It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, (shook frequently in 4 hours 65 ℃ of left and right sides heating for dissolving; Avoid boiling), after the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle; Thin up shakes up to scale, and accurate amount 25ml puts in the 250ml conical flask; Add the 8ml concentrated hydrochloric acid solution, be heated to nearly boiling, adds 6 methyl orange indicator solutions after, dropping ratio of quality and the number of copies 5% stannous chloride solution to solution becomes pale pink while shaking while hot; Take off if shake the back pink colour, can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions are used dichromate titration liquid (0.002mol/l) titration immediately.Every 1ml dichromate titration liquid (0.002mol/l) is equivalent to the iron of 0.6702mg.
These article iron content is 13.2mg/g ~ 22.1mg/g.
B. gallic acid content is measured:
Measure according to high performance liquid chromatography (" an appendix VI of Chinese pharmacopoeia version in 2010 D);
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than methyl alcohol-volume parts of 4:96 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 275nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get the Tibetan medicine composition Six-element sheet powder 1g that makes eye bright, accurately claim surely, put in the tool plug conical flask, the accurate volume parts that adds is than 50% methanol aqueous solution 25ml; Close plug is claimed to decide weight, ultrasonic 30 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
These article gallic acid content (C
7H
6O
5) must not be less than 1.83mg/g.
The described Tibetan medicine composition Six-element sheet that makes eye bright is meant with LIUWEI MINGMU WAN bulk drug prescription iron powder (system) 132.0g, barberry skin 132.0g, Caraway 132.0g, myrobalan 66.5g, terminaliae billericae,fructus 66.5g, emblic 66.5g; Add conventional auxiliary material, according to the tablet of common process preparation.
Claims (10)
1. the Six-element quality determining method of preparation that makes eye bright; The various preparations of said preparation for processing by the pharmacy conventional method by iron powder (system), barberry skin, Caraway, myrobalan, terminaliae billericae,fructus, emblic; It is characterized in that quality determining method comprises the content assaying method of iron powder in the preparation and/or the content assaying method of gallic acid.
2. quality determining method as claimed in claim 1 is characterized in that, the content assaying method of said iron powder is that after preparation ashing to be determined, with the concentrated hydrochloric acid dissolving, adding methyl orange indicator solution drips stannous chloride solution with Fe
3+Be reduced to Fe
2+, solution becomes pale red, is indicator with the diphenylamine sulfonic acid sodium salt then, is purple with potassium dichromate standard solution titration to solution and is terminal point, calculates the content of iron powder with the amount of known potassium dichromate standard solution.
3. quality determining method as claimed in claim 2 is characterized in that, the content assaying method concrete steps of said iron powder are: it is an amount of to get LIUWEI MINGMU WAN preparation powder; The accurate title, decide; The crucible that fills sample is put slowly vehement burning on the electric furnace, blazing to the whole charings of test sample, black in color; And no longer smolder, put and be chilled to room temperature; It is an amount of to drip 1 ~ 5ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 500 ~ 700 ℃ blazing 3 ~ 5 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, 60 ~ 70 ℃ of left and right sides heating for dissolving 3 ~ 5 hours; After the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle, and thin up is to scale; Shake up, accurate amount 25ml puts in the 250ml conical flask, adds the 8ml concentrated hydrochloric acid solution; Be heated to nearly boiling, add 6 methyl orange indicator solutions after, drip ratio of quality and the number of copies 5% stannous chloride solution to solution while hot while shaking and become pale pink, take off if shake the back pink colour; Then add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 2 ~ 10ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions, fixed with the dichromate titration drop immediately.
4. quality determining method as claimed in claim 3 is characterized in that, the preparation method of said mixture of sulfuric phosphoric acid solution is: 150ml concentration expressed in percentage by volume 95% ~ 98% concentrated sulphuric acid is under agitation slowly injected 500ml water; Add 150ml phosphoric acid after the cooling again; Be diluted with water to 1000ml, mixing promptly gets.
5. quality determining method as claimed in claim 1; It is characterized in that; The content assaying method of said gallic acid is; Getting gallic acid reference substance adding volume parts and be mixed with reference substance solution than 50% methanol aqueous solution, get preparation adding volume parts to be detected and be mixed with need testing solution than 50% methanol aqueous solution, is filling agent with the octadecylsilane chemically bonded silica; Is moving phase than the methyl alcohol-volume parts of 2～6:98～94 than 1% glacial acetic acid aqueous solution with volume parts; Detecting wavelength is the high performance liquid chromatography of 270 ~ 280nm.
6. quality determining method as claimed in claim 5 is characterized in that, specifically:
According to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than the methyl alcohol-volume parts of 2～6:98～94 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 270 ~ 280nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get preparation powder 0.5 ~ 1.5g to be detected, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution, 20 ~ 30ml; Close plug is claimed to decide weight, ultrasonic 20 ~ 40 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 5 ~ 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
7. quality determining method as claimed in claim 1; It is characterized in that the bulk drug of said preparation consists of: iron powder (system) 132.0 weight portions, barberry skin 132.0 weight portions, Caraway 132.0 weight portions, myrobalan's 66.5 weight portions, terminaliae billericae,fructus 66.5 weight portions, emblic 66.5 weight portions.
8. quality determining method as claimed in claim 7 is characterized in that, said quality determining method is:
A. the assay of iron powder:
It is an amount of to get preparation powder to be detected, and accurate the title decides, and the crucible that fills sample is put slowly vehement burning on the electric furnace, and be blazing to the whole charings of test sample, black in color, and no longer smolder, put and be chilled to room temperature; It is an amount of to drip 1ml sulfuric acid, makes carbide all moistening, continues to be heated to steam and eliminates, and white cigarette emits to the greatest extent; In 600 ℃ blazing 4 hours, put coldly, move in the 250ml tool plug conical flask with 50ml concentrated hydrochloric acid gradation washing, 65 ℃ of left and right sides heating for dissolving 4 hours; After the cooling solution is moved in the 250ml volumetric flask, with low amounts of water gradation washing container, washing lotion is incorporated in the same measuring bottle, and thin up is to scale; Shake up, accurate amount 25ml puts in the 250ml conical flask, adds the 8ml concentrated hydrochloric acid solution; Be heated to nearly boiling, add 6 methyl orange indicator solutions after, drip ratio of quality and the number of copies 5% stannous chloride solution to solution while hot while shaking and become pale pink, take off if shake the back pink colour; Can add 1 methyl orange to solution and present stable pale pink, be cooled to room temperature with cold water rapidly after, add distilled water 50ml; Mixture of sulfuric phosphoric acid solution 4ml, 15 of diphenylamine sulfonic acid sodium salt indicator solutions, fixed with the dichromate titration drop immediately;
B. the assay of gallic acid:
According to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filling agent; Is moving phase than methyl alcohol-volume parts of 4:96 than 1% glacial acetic acid aqueous solution with volume parts; The detection wavelength is 275nm; Number of theoretical plate calculates by the gallic acid peak should be not less than 2000;
The preparation of reference substance solution: it is an amount of to get the gallic acid reference substance, and accurate the title decides, and adds volume parts and processes the solution that every 1ml contains 0.1mg than 50% methanol aqueous solution, promptly gets;
The preparation of need testing solution: get Tibetan medicine composition LIUWEI MINGMU WAN powder 1g, the accurate title, decide, and puts in the tool plug conical flask, and the accurate volume parts that adds is than 50% methanol aqueous solution 25ml; Close plug is claimed to decide weight, ultrasonic 30 minutes; Put coldly, supply the weight that subtracts mistake than 50% methanol aqueous solution, shake up with volume parts; Filter, get subsequent filtrate, promptly get;
Determination method: draw each 10 μ l of reference substance solution and need testing solution respectively, inject liquid chromatograph, measure, promptly get.
9. quality determining method as claimed in claim 1 is characterized in that quality determining method as claimed in claim 8 is characterized in that, iron content is 13.2mg/g ~ 22.1mg/g in the assay project of said iron powder; Gallic acid content must not be less than 1.83mg/g in the assay project of said gallic acid.
10. quality determining method as claimed in claim 1; It is characterized in that; Described preparation is meant gets Tibetan medicine composition LIUWEI MINGMU WAN bulk drug; Press common process, add conventional auxiliary material and be prepared into clinical acceptable any formulation, comprise micropill, dripping pill, tablet, capsule, particle, medicine materical crude slice or dispersing tablet.
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| CN102590203A (en) * | 2012-02-03 | 2012-07-18 | 合肥国轩高科动力能源有限公司 | Method for measuring iron content of lithium iron phosphorous oxide iron source raw material of lithium ion power battery anode material |
| CN102662026A (en) * | 2012-05-30 | 2012-09-12 | 山东阿如拉药物研究开发有限公司 | Quality detecting method for traditional Chinese medicine Qianliening preparation |
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