CN1527053A - Quality control method for rehmannia prepn of six ingredients - Google Patents
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Abstract
The present invention relates to six ingredient rehmannia preparation, and is especially the quality control method for six ingredient rehmannia preparation. On the basis of original quality standard, thin layer chromatography process for the qualitative identification of prepared rhizome of rehmannia and oriental water plantain is increased as two specific identification methods, the peonol identification is altered from thin layer chromatography method to vapor chromatography method, and two content determining items including the thin layer scanning determination of ursolic acid content and capillary column vapor chromatography determination of peonol content are increased.
Description
Technical field
The present invention relates to Liuwei Dihuang preparation, particularly the method for quality control of six drugs containing rehmanniae software capsule.
Background technology
Liuwei Dihuang Wan is the representative side of nourishing kidney yin, is used for damage of kidney-YIN, dizziness and tinnitus, and soreness and weakness of waist and knees, osteopyrexia and fever, the night sweat seminal emission is quenched one's thirst.Done many researchs to it modern age, thinks that it has the effect of the metabolic function that strengthens function of human body, adjustment and raising human body.On this basis, for purposes such as taking convenience, raising curative effects, many other formulations except that honeyed bolus have been developed, as the water-bindered pill, oral liquid, soft capsule etc.Soft capsule is my company's product, in the quality standard promulgated by the ministries or commissions of the Central Government, the qualitative identification method comprises ursolic acid and the Paeonol in the thin-layered chromatography qualitative identification product, the quantitative quality control method that does not have product, in order to control the end product quality of six drugs containing rehmanniae soft capsule better, make it to reach stable, controlled, homogeneous, we carry out standard to former ministerial standard and improve.By experimental study, on the proper mass standard base, increased prepared rhizome of rehmannia and these two discrimination methods that specificity is stronger of rhizoma alismatis in the thin-layered chromatography qualitative identification product, and the thin-layer chromatography discrimination method revision of Paeonol in the proper mass standard has been differentiated for gas chromatography; Increase by two assay items, that is: adopt the tlc scanning determination ursolic acid content, adopt the capillary column gas chromatography method to measure paeonol content.By improving quality standard, stricter to the technological requirement of this product, quality standard is more rigorous simultaneously, science.These method of quality control are not only applicable to the six drugs containing rehmanniae soft capsule, and are applicable to the six drugs containing rehmanniae class preparation with any formulation of the prescription of six drugs containing rehmanniae preparation.
Summary of the invention
The object of the present invention is to provide six drugs containing rehmanniae class preparation, especially the new method of quality control of six drugs containing rehmanniae soft capsule.It thes contents are as follows:
[assay] 1. in the gas chromatography determination product content of Paeonol measure according to vapor-phase chromatography (" appendix VIE of Chinese pharmacopoeia version in 2000).
Chromatographic condition and system suitability test 5% diphenyl-95% dimethyl-silicon alkyl copolymer are the capillary chromatographic column (30m * 0.32mm * 0.25 μ m) of stationary phase; Injector temperature: 240 ℃; Detector temperature (FID): 240 ℃; Split sampling is measured (split ratio is 50: 1); Column temperature: 150 ℃; Flow rate of carrier gas: 1.0ml/min; Number of theoretical plate calculates by the Paeonol peak should be not less than 25000; The degree of separation of Paeonol peak and internal standard compound mass peak should be greater than 1.5.
It is an amount of that correction factor mensuration is got the n-pentadecane reference substance, and accurate the title decides, and adds absolute ethyl alcohol and make the solution of determining concentration, as inner mark solution.It is an amount of that other gets the Paeonol reference substance, accurate claims surely, adds absolute ethyl alcohol and make solution with the close concentration of inner mark solution, shakes up promptly.Precision is measured reference substance solution and inner mark solution, and each is an amount of, puts in the same volumetric flask, adds absolute ethyl alcohol and is diluted to scale, shakes up, the accurate solution inject gas chromatograph of drawing an amount of volume, the calculation correction factor.
It is an amount of that the determination method precision is got the product or the product content thing that meet the content uniformity standard, extracts constant volume in right amount with absolute ethyl alcohol.Precision is measured extract and inner mark solution, and each is an amount of, puts in the volumetric flask of proper volume, adds the absolute ethyl alcohol constant volume, shakes up, and accurately draws an amount of volume, and inject gas chromatograph is measured, promptly.
2. the content of ursolic acid precision is got product or the product content thing is an amount of in the tlc scanning determination product, and with methanol extraction, constant volume is as need testing solution; Other gets the ursolic acid reference substance, adds methyl alcohol and makes the solution of determining concentration, product solution in contrast.According to thin-layered chromatography (" Chinese pharmacopoeia appendix VIB in 2000) test, the accurate need testing solution of drawing, and quantitatively draw the reference substance solution of different volumes, the reference substance solution difference point of crossing of need testing solution and each volume is on same silica gel g thin-layer plate, with toluene-ethyl acetate-glacial acetic acid (12: 4: 0.5) is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to dry by the fire to the spot colour developing at 110 ℃, take out, on thin layer plate, cover onesize glass plate, use immobilization with adhesive tape on every side, scan according to thin-layered chromatography (" an appendix VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography scanning), wavelength: λ S=520nm, λ R=700nm measures test sample absorbance log integrated value and reference substance absorbance log integrated value, calculate, promptly.
[discriminating] (1) gets product or the product content thing is an amount of, adds alcohol extract, and extract evaporate to dryness, residue add the small amount of ethanol dissolving, as need testing solution.It is an amount of that other gets the prepared rhizome of rehmannia control medicinal material, makes the methanol solution of control medicinal material after the extraction; According to thin-layered chromatography (" appendix VIB of Chinese pharmacopoeia version in 2000) test, each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (70: 30: 5) is developping agent, launch, take out, dry, spray is with the anisaldehyde test solution, 105 ℃ dry by the fire to the spot colour developing clear.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
(2) qualitative identification of Paeonol extracts product with absolute ethyl alcohol and makes need testing solution, the ethanol solution of preparation Paeonol standard items is a reference substance solution, measure by the GC conditions under [assay] item, in the chromatogram, test sample main peak retention time should be consistent with reference substance.
(3) it is an amount of to get the rhizoma alismatis control medicinal material, and with alcohol extract, extract evaporate to dryness, residue add methyl alcohol makes dissolving in right amount, in contrast medicinal material solution.According to thin-layered chromatography (" appendix VIB of Chinese pharmacopoeia version in 2000) test, each is an amount of for need testing solution under absorption control medicinal material solution and [discriminating] (1) item, point is on same silica gel g thin-layer plate, with benzene-ethyl acetate (9: 1) is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings several minutes.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Quantitatively reach the extraction described in the qualitative identification method and comprise Extraction by Ultrasound, backflow.
More than quantitatively and qualitative method of quality control be based on the six drugs containing rehmanniae prescription and formulate, be not only applicable to the six drugs containing rehmanniae soft capsule, and be suitable for as method of quality control with the product of any formulation of the prescription preparation of six drugs containing rehmanniae.
Embodiment
Embodiment 1Preparation six drugs containing rehmanniae soft capsule
Get raw material: prepared rhizome of rehmannia 480g, the fruit of medicinal cornel (system) 240g, moutan bark 180g, Chinese yam 240g, Poria cocos 180g, rhizoma alismatis 180g.
Above Six-element, volatile oil is extracted in the moutan bark distillation, and the aqueous solution after distillation device is in addition collected; The fruit of medicinal cornel each 2 hours, merges extract, filtration, filtrate for later use with 70% alcohol reflux secondary; Prepared rhizome of rehmannia, Chinese yam, rhizoma alismatis boiling secondary, 2 hours for the first time, 1 hour for the second time, collecting decoction, filter, the aqueous solution after filtrate and the moutan bark distillation merges, and being evaporated to relative density is the clear cream of 1.15～1.20 (50 ℃ of heat are surveyed), put cold, add ethanol and make and contain alcohol amount and reach 70%, left standstill 48 hours, get the merging of supernatant and above-mentioned fruit of medicinal cornel extract, decompression recycling ethanol is to there not being the alcohol flavor, and is standby; After Poria cocos adds water boil, soak secondary, each 1.5 hours in 80 ℃ of temperature, merge leachate, filter, filtrate decompression is concentrated into the clear cream that relative density is 1.15～1.20 (50 ℃ of heat are surveyed), merge with above-mentioned reserve liquid, being concentrated into relative density is the thick paste of 1.30 (50 ℃ of heat are surveyed), and drying under reduced pressure is ground into fine powder, add moutan bark volatile oil and vegetable oil, appropriate amount of auxiliary materials, mixing is made 1000 of soft capsules, promptly.
This product is a soft capsule, and content is the sepia viscous liquid; It is sweet to distinguish the flavor of, little acid.Every contains content 0.38g.Oral, one time 3,2 times on the one.
Embodiment 2The content of moutan bark in the gas chromatography determination six drugs containing rehmanniae soft capsule
Chromatographic condition and system suitability test 5% diphenyl-95% dimethyl-silicon alkyl copolymer are the capillary chromatographic column (30m * 0.32mm * 0.25 μ m) of stationary phase; Injector temperature: 240 ℃; Detector temperature (FID): 240 ℃; Split sampling is measured (split ratio is 50: 1); Column temperature: 150 ℃; Flow rate of carrier gas: 1.0ml/min; Number of theoretical plate calculates by the Paeonol peak should be not less than 25000; The degree of separation of Paeonol peak and internal standard compound mass peak should be greater than 1.5.
It is an amount of that correction factor mensuration is got the n-pentadecane reference substance, and accurate the title decides, and adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, shakes up, as inner mark solution.It is an amount of that other gets the Paeonol reference substance, and accurate the title decides, and adds absolute ethyl alcohol and makes the solution that every 1ml contains Paeonol 1mg, shakes up, promptly.Precision measures reference substance solution 2ml and inner mark solution 1ml puts in the 10ml measuring bottle, adds absolute ethyl alcohol and is diluted to scale, shakes up, and draws 5 μ l, inject gas chromatograph, the calculation correction factor.
Determination method is got the about 2g of six drugs containing rehmanniae soft capsule content that meets the content uniformity standard, and accurate the title decides, and puts in the tool plug conical flask, the accurate absolute ethyl alcohol 20ml that adds, close plug claims to decide weight, and sonicated 20 minutes is put cold, weight decided in title, supplies with absolute ethyl alcohol to subtract weight loss, shakes up, centrifugal.Precision is measured supernatant 5ml and inner mark solution 1ml, puts in the 10ml measuring bottle, adds absolute ethyl alcohol to scale, shakes up, and draws 5 μ l, and inject gas chromatograph is measured, promptly.
Every of this product contains moutan bark with Paeonol (C
9H
10O
3) meter, should be less than 0.80mg.
Embodiment 3The content of the fruit of medicinal cornel in the tlc scanning determination six drugs containing rehmanniae soft capsule
Get this product content 10g, the accurate title, decide, the accurate methyl alcohol 40ml that adds, close plug claims to decide weight, ultrasonic Extraction 40 minutes, put coldly, claim to decide weight, supply with methyl alcohol and subtract weight loss, shake up, centrifugal, precision is measured supernatant 20ml, water-bath is steamed to an amount of, and residue, adds methyl alcohol and is diluted to scale to the 5ml measuring bottle with dissolve with methanol, shake up, as need testing solution.Other gets the ursolic acid reference substance, adds methyl alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin-layered chromatography (" Chinese pharmacopoeia appendix VIB in 2000) test, draw need testing solution 5 μ l, reference substance solution 4 μ l and 8 μ l, the point of crossing is on same silica gel g thin-layer plate respectively, with toluene-ethyl acetate-glacial acetic acid (12: 4: 0.5) is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to dry by the fire to the spot colour developing at 110 ℃, takes out, on thin layer plate, cover onesize glass plate, use immobilization with adhesive tape on every side, the photograph thin-layered chromatography (" an appendix VIB of Chinese pharmacopoeia version in 2000 thin layer chromatography scanning) scan wavelength: λ S=520nm, λ R=700nm, measure test sample absorbance log integrated value and reference substance absorbance log integrated value, calculate, promptly.
Every of this product contains the fruit of medicinal cornel with ursolic acid (C
30H
48O
3) meter, must not be less than 0.11mg.
Embodiment 4Prepared rhizome of rehmannia in the thin-layered chromatography qualitative identification six drugs containing rehmanniae soft capsule
Get this product content 1g, add ethanol 20ml, ultrasonic Extraction 30 minutes filters, and filtrate evaporate to dryness, residue add 5ml ethanol makes dissolving, as need testing solution.Other gets prepared rhizome of rehmannia control medicinal material 1g, adds ethanol 20ml, puts in the water-bath reflux 1 hour, filters, and the filtrate evaporate to dryness adds methyl alcohol 5ml and makes dissolving, in contrast medicinal material solution.According to thin-layered chromatography (" appendix VIB of Chinese pharmacopoeia version in 2000) test, draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (70: 30: 5) is developping agent, launch, take out, dry, spray is with the anisaldehyde test solution, 105 ℃ dry by the fire to the spot colour developing clear.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Embodiment 5Rhizoma alismatis in the thin-layered chromatography qualitative identification six drugs containing rehmanniae soft capsule
Get rhizoma alismatis control medicinal material 0.5g, grind, add ethanol 20ml, ultrasonic Extraction 30 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, in contrast medicinal material solution.According to thin-layered chromatography (" appendix VIB of Chinese pharmacopoeia version in 2000) test, draw control medicinal material solution and press each 10 μ l of need testing solution of embodiment 4 methods preparation, put respectively on same silica gel g thin-layer plate, with benzene-ethyl acetate (9: 1) is developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings several minutes.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Embodiment 6Moutan bark in the vapor-phase chromatography qualitative identification six drugs containing rehmanniae soft capsule
Get this product content 1g, add absolute ethyl alcohol 10ml, ultrasonic Extraction 20 minutes filters, as need testing solution.Get the Paeonol standard items, make the solution that every 1ml contains the about 1mg of Paeonol with absolute ethyl alcohol, product solution is pressed the GC conditions of paeonol content in the embodiment 2 gas chromatography determination products and is measured in contrast, in the chromatogram, test sample main peak retention time should be consistent with reference substance.
Claims (7)
1. the method for quality control of a Liuwei Dihuang preparation is characterized in that this method comprises a kind of in the following assay or two kinds:
A. gas chromatography determination paeonol content
Chromatographic condition and system suitability test 5% diphenyl-95% dimethyl-silicon alkyl copolymer are the capillary chromatographic column of stationary phase, and column parameter is 30m * 0.32mm * 0.25 μ m; Injector temperature: 240 ℃; Fid detector temperature: 240 ℃; It is 50: 1 that split sampling is measured split ratio; Column temperature: 150 ℃; Flow rate of carrier gas: 1.0ml/min; Number of theoretical plate calculates by the Paeonol peak should be not less than 25000; The degree of separation of Paeonol peak and internal standard compound mass peak should be greater than 1.5;
It is an amount of that correction factor mensuration is got the n-pentadecane reference substance, and accurate the title decides, and adds absolute ethyl alcohol and make the solution of determining concentration, as inner mark solution; It is an amount of that other gets the Paeonol reference substance, accurate claims surely, adds absolute ethyl alcohol and make solution with the close concentration of inner mark solution; Precision is measured reference substance solution and inner mark solution, and each is put in the same volumetric flask in right amount, with absolute ethyl alcohol dilution constant volume; The accurate solution inject gas chromatograph of drawing an amount of volume, the calculation correction factor;
The determination method precision gets product or the product content thing is an amount of, extracts constant volume in right amount with absolute ethyl alcohol; Precision is measured extract and inner mark solution, and each is an amount of, puts in the volumetric flask of same proper volume, adds the absolute ethyl alcohol constant volume, shakes up, and accurately draws an amount of volume, and inject gas chromatograph is measured, promptly;
B. tlc scanning determination ursolic acid
Precision gets product or the product content thing is an amount of, and with methanol extraction, constant volume is as need testing solution; Other gets the ursolic acid reference substance, adds methyl alcohol and makes the solution of determining concentration, product solution in contrast; The accurate need testing solution of drawing, and quantitatively draw the reference substance solution of different volumes, the reference substance solution difference point of crossing of need testing solution and each volume is on same silica gel g thin-layer plate, with volume proportion is that toluene-ethyl acetate-glacial acetic acid mixed solvent of 12: 4: 0.5 is a developping agent, launch, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to the spot colour developing, on thin layer plate, cover onesize glass plate, scan wavelength with thin-layer chromatogram scanner: λ S=520nm, λ R=700nm, measure test sample absorbance log integrated value and reference substance absorbance log integrated value, calculate, promptly.
2. the method for quality control of a Liuwei Dihuang preparation is characterized in that containing in this method in the following qualitative identification one or more:
A. the qualitative identification of prepared rhizome of rehmannia is got product or the product content thing is an amount of, adds alcohol extract, and extract is as need testing solution; It is an amount of that other gets the prepared rhizome of rehmannia control medicinal material, makes the methanol solution of control medicinal material after the extraction; Each is an amount of to draw above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, and be that chloroform-methanol-water of 70: 30: 5 is that developping agent launches with volume proportion, take out, to dry, spray is with the anisaldehyde test solution, and it is clear to be heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
B. the qualitative identification of Paeonol extracts product or product content thing with absolute ethyl alcohol, make need testing solution, the ethanol solution of preparation Paeonol standard items is a reference substance solution, measure by the described GC conditions of claim 1, in the chromatogram, test sample main peak retention time should be consistent with reference substance;
C. it is an amount of that the qualitative identification of rhizoma alismatis is got the rhizoma alismatis control medicinal material, makes methanol solution after the extraction, in contrast medicinal material solution; Each is an amount of for need testing solution under absorption control medicinal material solution and this claim discriminating a item, put respectively on same silica gel g thin-layer plate, with volume proportion is that benzene-ethyl acetate mixed solvent of 9: 1 is a developping agent, launches, and takes out, dry, spray is heated to colour developing with 10% ethanol solution of sulfuric acid, in the test sample chromatogram, with the corresponding method according to claim 1 and 2 of control medicinal material chromatogram, the spot of color.
3. method according to claim 1 and 2 is characterized in that described extraction comprises backflow and Extraction by Ultrasound.
4. the method for quality control of a six drugs containing rehmanniae soft capsule is characterized in that containing in this method a kind of in the following assay or two kinds:
A. gas chromatography determination paeonol content
Chromatographic condition and system suitability test 5% diphenyl-95% dimethyl-silicon alkyl copolymer are the capillary chromatographic column of stationary phase, and column parameter is 30m * 0.32mm * 0.25 μ m; Injector temperature: 240 ℃; Fid detector temperature: 240 ℃; It is 50: 1 that split sampling is measured split ratio; Column temperature: 150 ℃; Flow rate of carrier gas: 1.0ml/min; Number of theoretical plate calculates by the Paeonol peak should be not less than 25000; The degree of separation of Paeonol peak and internal standard compound mass peak should be greater than 1.5;
It is an amount of that correction factor mensuration is got the n-pentadecane reference substance, and accurate the title decides, and adds absolute ethyl alcohol and makes the solution that every 1ml contains 1mg, shakes up, as inner mark solution; It is an amount of that other gets the Paeonol reference substance, and accurate the title decides, and add absolute ethyl alcohol and make the solution that every 1ml contains Paeonol 1mg; Precision measures reference substance solution 2ml and inner mark solution 1ml puts in the 10ml measuring bottle, adds the absolute ethyl alcohol constant volume, draws 5 μ l, inject gas chromatograph, the calculation correction factor;
Determination method is got the about 2g of six drugs containing rehmanniae soft capsule content, accurate claims surely, and the accurate absolute ethyl alcohol 20ml that adds claims to decide weight, and ultrasonic Extraction 20 minutes is supplied with absolute ethyl alcohol and to be subtracted weight loss, shakes up, and is centrifugal; Precision is measured supernatant 5ml and inner mark solution 1ml, puts in the 10ml measuring bottle, adds absolute ethyl alcohol to scale, shakes up, and draws 5 μ l, and inject gas chromatograph is measured, promptly;
B. the content of the fruit of medicinal cornel in the tlc scanning determination six drugs containing rehmanniae soft capsule
Get this product content 10g, the accurate title, decide, the accurate methyl alcohol 40ml that adds, close plug claims to decide weight, ultrasonic Extraction 40 minutes, put coldly, claim to decide weight, supply with methyl alcohol and subtract weight loss, shake up, centrifugal, precision is measured supernatant 20ml, water-bath is steamed to an amount of, and residue, adds methyl alcohol and is diluted to scale to the 5ml measuring bottle with dissolve with methanol, shake up, as need testing solution; Other gets the ursolic acid reference substance, adds methyl alcohol and makes the solution that every 1ml contains 0.5mg, in contrast product solution; Draw need testing solution 5 μ l, reference substance solution 4 μ l and 8 μ l, the point of crossing is on same silica gel g thin-layer plate respectively, with volume proportion is that toluene-ethyl acetate-glacial acetic acid mixed solvent of 12: 4: 0.5 is a developping agent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, it is clear to be heated to the spot colour developing, take out, on thin layer plate, cover onesize glass plate, use immobilization with adhesive tape on every side, scan with thin-layer chromatogram scanner, wavelength: λ S=520nm, λ R=700nm measures test sample absorbance log integrated value and reference substance absorbance log integrated value, calculate, promptly.
5. the method for quality control of a six drugs containing rehmanniae soft capsule is characterized in that containing in this method in the following qualitative identification one or more:
A. the qualitative identification of prepared rhizome of rehmannia
Get product content thing 1g, add ethanol 20ml, ultrasonic Extraction 30 minutes filters, and filtrate evaporate to dryness, residue add 5ml ethanol makes dissolving, as need testing solution; Other gets prepared rhizome of rehmannia control medicinal material 1g, adds ethanol 20ml, puts in the water-bath reflux 1 hour, filters, and the filtrate evaporate to dryness adds methyl alcohol 5ml and makes dissolving, in contrast medicinal material solution; Draw each 10 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with volume proportion is that chloroform-methanol-water mixed solvent of 70: 30: 5 is a developping agent, launches, and takes out, dry, spray is with the anisaldehyde test solution, and it is clear to be heated to the spot colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
B. the qualitative identification of rhizoma alismatis
Get rhizoma alismatis control medicinal material 0.5g, grind, add ethanol 20ml, ultrasonic Extraction 30 minutes filters, and filtrate evaporate to dryness, residue add methyl alcohol 5ml makes dissolving, in contrast medicinal material solution; Draw control medicinal material solution and press each 10 μ l of need testing solution of the qualitative identification method preparation of the described prepared rhizome of rehmannia of this claim step a, put respectively on same silica gel g thin-layer plate, with volume proportion is that benzene-ethyl acetate mixed solvent of 9: 1 is a developping agent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to colour developing, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color
C. the qualitative identification of moutan bark
Extract the content of soft capsule with absolute ethyl alcohol and make need testing solution, the ethanol solution of preparation Paeonol standard items is a reference substance solution, measure by the described GC conditions of claim 4, in the chromatogram, test sample main peak retention time should be consistent with reference substance.
6. according to claim 4 or 5 described methods, volume, point sample amount or sample size after wherein said sampling amount, the consumption that extracts sample or dissolving extract and standard items solvent for use, constant volume or the dissolving can be that benchmark changes with described occurrence, or changes in proportion.
7. claim 4 or 5 described methods, extraction wherein both can be adopted Extraction by Ultrasound, also can adopt refluxing extraction.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100370251C (en) * | 2004-09-23 | 2008-02-20 | 江西江中药业股份有限公司 | Quality control method for liuwei Dihuang soft extract |
| CN100408069C (en) * | 2005-12-29 | 2008-08-06 | 贵州益佰制药股份有限公司 | Quality control method of oral preparation for yin enriching kidney supplementing |
| CN101362074B (en) * | 2007-08-08 | 2010-09-01 | 中国计量科学研究院 | Use of double-phenyl hybridization silica gel material monolithic column in chromatogram |
| CN101229308B (en) * | 2008-01-11 | 2010-12-15 | 天津海世达检测技术有限公司 | Detection method of liu-wei tonic tablets dual-wavelength fingerprint chromatogram |
| CN101773592B (en) * | 2009-01-13 | 2012-04-25 | 北京亚东生物制药有限公司 | Method fro controlling quality of pill of six ingredients with rehmannia |
| CN102818861A (en) * | 2012-05-10 | 2012-12-12 | 丽珠医药集团股份有限公司 | Quality control method and application of Qingdu Anshen capsule |
| CN105203687A (en) * | 2015-09-18 | 2015-12-30 | 西安科技大学 | Paeonol quick detection method |
| CN111398508A (en) * | 2020-04-10 | 2020-07-10 | 山东中大千方制药有限公司 | Method for identifying paeonol in sophora flower-scutellaria ointment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100370251C (en) * | 2004-09-23 | 2008-02-20 | 江西江中药业股份有限公司 | Quality control method for liuwei Dihuang soft extract |
| CN100408069C (en) * | 2005-12-29 | 2008-08-06 | 贵州益佰制药股份有限公司 | Quality control method of oral preparation for yin enriching kidney supplementing |
| CN101362074B (en) * | 2007-08-08 | 2010-09-01 | 中国计量科学研究院 | Use of double-phenyl hybridization silica gel material monolithic column in chromatogram |
| CN101229308B (en) * | 2008-01-11 | 2010-12-15 | 天津海世达检测技术有限公司 | Detection method of liu-wei tonic tablets dual-wavelength fingerprint chromatogram |
| CN101773592B (en) * | 2009-01-13 | 2012-04-25 | 北京亚东生物制药有限公司 | Method fro controlling quality of pill of six ingredients with rehmannia |
| CN102818861A (en) * | 2012-05-10 | 2012-12-12 | 丽珠医药集团股份有限公司 | Quality control method and application of Qingdu Anshen capsule |
| CN105203687A (en) * | 2015-09-18 | 2015-12-30 | 西安科技大学 | Paeonol quick detection method |
| CN111398508A (en) * | 2020-04-10 | 2020-07-10 | 山东中大千方制药有限公司 | Method for identifying paeonol in sophora flower-scutellaria ointment |
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Effective date of registration: 20190920 Address after: 222047 Jiangning economic and Technological Development Zone, Jiangsu, Lianyungang industrial city Co-patentee after: JIANGSU KANION SUNSHINE PHARMACEUTICAL CO.,LTD. Patentee after: JIANGSU KANION PHARMACEUTICAL Co.,Ltd. Address before: 222001 Jiangsu Province, Lianyungang city Sinpo District Haichang Road No. 58 Patentee before: JIANGSU KANION PHARMACEUTICAL Co.,Ltd. |
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