CN102000209A - Quality detection method of asiatic toddalia root gargle - Google Patents
Quality detection method of asiatic toddalia root gargle Download PDFInfo
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Abstract
The invention discloses a quality detection method of asiatic toddalia root gargle, comprising the following steps of: (1) identifying the asiatic toddalia root gargle; and (2) measuring the content according to a high-efficiency liquid chromatography: A, performing of a chromatograph condition and system adaptability test; B, comparison product solution preparation: precisely weighting a proper amount of isoferulic acid comparison product and preparing into the solution containing 20 mug per 1ml by using 10% ethanol; C, preparation of a test sample solution; and D, application of a measuring method: precisely absorbing 10 mul of the comparison production solution and 10 mul of the test sample solution, injecting in a liquid chromatograph for measuring, wherein every 100ml of the product contains at least 4.0mg of rhizoma cimicifugae metered by isoferulic acid. The invention has high test accuracy, can better control the quality of the medicine and ensure the medication safety, and the medicinal materials can be easily obtained.
Description
Technical field
The invention belongs to the field of quality control of Chinese medicine preparation, particularly the dragon palm is sucked the quality determining method of liquid.
Background technology
It is by the Radix Toddaliae Asiaticae root bark that the dragon palm is sucked liquid, Folium Toddaliae Asiaticae, Cortex Lycii, Rhizoma Cimicifugae four Chinese medicine material, decoct with water three times, for the first time, 2 hours for the second time, 1 hour for the third time, collecting decoction, filter, filtrate is concentrated into the clear paste that relative density is 1.10～1.15 (60～70 ℃), adds ethanol and makes that to contain alcohol amount be 70%, leaves standstill 24 hours, get supernatant, filter, filtrate recycling ethanol also is concentrated into the clear paste that relative density is 1.10～1.15 (60～70 ℃), adds polyoxyethylene sorbitan monoleate, glycerol, mixing, boil, be cooled to below 40 ℃, add methyl hydroxybenzoate, ethyl hydroxybenzoate, Mentholum, rose essence, cocoanut flavour, add water to ormal weight, mixing leaves standstill, and filters, fill, promptly.For pale brown color to henna supernatant liquid, postpone for a long time has small amount of precipitate; Gas delicate fragrance, sweet in the mouth, little hardship.Function cures mainly: the Seedling doctor: lift by force, lift and buy (or sell) on credit: the Lip river item, product in the loud, high-pitched sound are reined in the labour palace, rein in Ga Guomian.The traditional Chinese medical science: dissipating blood stasis hemostasis, removing dampness and detoxicating, reducing swelling and alleviating pain.Be used for halitosis, recurrent aphtha (oral ulcer), gingivitis, periodontitis.Assay in the proper mass standard, be to detect the contained ferulic acid of Rhizoma Cimicifugae medical material in the prescription, but in long-term production, find, as containing the survey index, control of product quality there is following some weak point with ferulic acid, 1, a large amount of documents and materials all have report, the ferulic acid solution instability of water or methanol (ethanol) preparation, see that auroral poles easily decomposes, 2h can be reduced to 20% of relative amount after ferulic acid was seen light, thereby reduced the check accuracy.2, with ferulic acid as containing the survey index, the rate of transform of finished product is about about 20%, and is qualified in order to guarantee finished product, and medical material contains ferulic acid must not be less than 0.07%, and commercially available most medical material ferulaic acid content does not all reach this limit, buys satisfactory medical material and is not easy very much.3, the adjacent peak-to-peak separating degree with other in ferulic acid peak is lower than 1.5 in liquid chromatograph, and peak shape is poor, the post effect is low, thereby influences the accuracy of assay.
Summary of the invention
A kind of check accuracy height that the objective of the invention is to overcome above-mentioned shortcoming and provide, the dragon palm that medical material is easy to get is sucked the quality determining method of liquid.
A kind of dragon palm of the present invention is sucked the quality determining method of liquid, comprises the steps:
(1) the dragon palm is sucked the discriminating of liquid: get this product 20ml, add ammonia solution 2ml, extract 2 times with the chloroform jolting, and each 10ml, combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Folium Toddaliae Asiaticae and each 1g of Radix Toddaliae Asiaticae root bark control medicinal material, adds ethanol 20ml, and reflux 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, select respectively on same silica gel g thin-layer plate with 1% potassium dihydrogen phosphate and the preparation of 0.5% sodium carboxymethyl cellulose mixed liquor (1: 1), with toluene-ethyl acetate (8: 2) is developing solvent, launch, taking-up is dried, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(2) according to high effective liquid chromatography for measuring content:
A, chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Acetonitrile-0.1% phosphoric acid (13: 87) is mobile phase; 30 ℃ of column temperatures; The detection wavelength is 316nm.Theoretical cam curve is pressed the Hesperetic acid peak and is calculated, and should be not less than 5000;
The preparation of B, reference substance solution: it is an amount of that precision takes by weighing the Hesperetic acid reference substance, makes the solution that every 1ml contains 20 μ g with 10% ethanol, promptly;
C, need testing solution preparation: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
D, algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The above-mentioned dragon palm is sucked the quality determining method of liquid, and wherein: the every 100ml of this product contains Rhizoma Cimicifugae with Hesperetic acid (C
10H
10O
4) meter, must not be less than 4.0mg.
The present invention compared with prior art has tangible beneficial effect, by above technical scheme as can be known, adopts and sees that the not labile Hesperetic acid of light is as containing the survey index.To guarantee the check accuracy.Commercially available most medical material Hesperetic acid content has all reached requirement, buys satisfactory medical material and is easy to.In liquid chromatograph, between Hesperetic acid peak and other peak good separating arranged all, thereby guaranteed the accuracy of assay.Guarantee the safety of medication, better instruct and produce, make technology controlling and process rationally strict more.
The specific embodiment
Below further specify the beneficial effect that the dragon palm of the present invention is sucked the quality determining method of liquid by testing example:
The test example:
1, reference substance, reagent and reagent
1.1 instrument: Agilent 1100 type high performance liquid chromatographs, VWD detector, Agilent chem workstation; Electronic balance (ten thousand/) BS-210S type (Sai Duolisi company); Electronic balance (100,000/) AE240 type (Mettler company).
1.2 reference substance: Hesperetic acid reference substance (lot number: 111698-200501), purchase in Nat'l Pharmaceutical ﹠ Biological Products Control Institute for assay usefulness.
1.3 reagent: ethanol, phosphoric acid are analytical pure; Acetonitrile is a chromatographically pure; Water is double distilled water.
1.4 reagent: the dragon palm is sucked the liquid sample to be provided by Guiyang Xintian Pharmaceutical Industry Co., Ltd..
2, the preparation of reference substance solution
The reference substance stock solution: precision takes by weighing Hesperetic acid reference substance 11.00mg, puts in the 50ml measuring bottle, adds 10% alcoholic solution, dissolves and is diluted to scale, shakes up, and promptly gets the solution that every 1ml contains 0.22mg.
Reference substance solution: precision is measured above-mentioned reference substance stock solution 5ml, puts in the 50ml measuring bottle, adds 10% dissolve with ethanol solution and is diluted to scale, shakes up, and promptly gets the solution that every 1ml contains 22 μ g.
3, the chromatographic condition test is with reference to " the different Resina Ferulae content assaying method of Chinese pharmacopoeia Rhizoma Cimicifugae medical material of version in 2005
Chromatographic column: octadecylsilane chemically bonded silica is filler (the special ODS2 C18 250mm * 4.6mm of Erie, 5 μ m)
Mobile phase: acetonitrile-phosphoric acid (13: 87)
Flow velocity: 1.0ml/ minute
Detect wavelength: 316nm
The preparation of need testing solution: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, as need testing solution.
Accurate respectively reference substance solution (C=22 μ g/ml) and each 10 μ l of need testing solution of drawing inject chromatograph of liquid, the record chromatogram.
The result has between Hesperetic acid peak and other peak as can be seen from the test sample collection of illustrative plates that good separating degree, peak shape are good, post imitate high, so with the chromatographic condition of this chromatographic condition as this experiment.
4, the preparation of need testing solution is selected:
Method 1: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Method 2: precision is measured this product 5ml, and with ethyl acetate extraction 4 times (20ml, 15ml, 10ml, 10ml), combined ethyl acetate extracting solution, evaporate to dryness, residue add dissolve with ethanol and be transferred in the 25ml measuring bottle, add ethanol dilution to scale, shake up, promptly.
Method 3: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly.
Method 4: precision is measured this product 5ml, puts in the 25ml measuring bottle, and thin up shakes up to scale, filters, and gets subsequent filtrate, promptly.
Accurate respectively Hesperetic acid reference substance solution (C=22 μ g/ml) and 4 each 10 μ l of need testing solution of drawing inject chromatograph of liquid, and the record chromatogram the results are shown in following table:
Conclusion: as can be seen from above result of the test, in each method, between Hesperetic acid peak and other peak good separating arranged all, method 1,4 content are the highest, take all factors into consideration so list method 1 in text, be: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shake up, filter, get subsequent filtrate, promptly.
5, system suitability test
Precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, as need testing solution; Other gets negative sample and makes negative sample solution with method.Accurate each the 10 μ l of reference substance solution (22 μ g/ml), negative sample solution and need testing solution that draw inject chromatograph of liquid, the record chromatogram.From chromatogram, can find out, test sample with the corresponding position of reference substance retention time on the peak is arranged, and peak shape is good, and negative sample does not have the peak on corresponding position, illustrate that negative sample is noiseless to sample determination.The number of theoretical plate at the Hesperetic acid peak of sample in collection of illustrative plates is 20175, with other material good separating arranged, peak shape is good, with reference to " the theoretical cam curve of a Rhizoma Cimicifugae medical material of Chinese pharmacopoeia version in 2005 Hesperetic acid assay defined, the theoretical cam curve of stipulating this experiment should be lower than 5000 by the calculating of Hesperetic acid peak.
6, linear relationship test
Reference substance solution is 1.: precision is measured 2 different Resina Ferulae reference substance solution (C=22 μ g/ml) 2ml down, puts in the 10ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and promptly gets the solution that every 1ml contains 4.4 μ g.
Reference substance solution is 2.: precision is measured 2 different Resina Ferulae reference substance solution (C=22 μ g/ml) 5ml down, puts in the 10ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and promptly gets the solution that every 1ml contains 11 μ g.
Reference substance solution is 3.: get 2 different Resina Ferulae reference substance solution (C=22 μ g/ml) down
Reference substance solution is 4.: precision is measured 2 different Resina Ferulae reference substance stock solution (C=220 μ g/ml) 3ml down, puts in the 20ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and promptly gets the solution that every 1ml contains 33 μ g.
Reference substance solution is 5.: precision is measured 2 different Resina Ferulae reference substance stock solution (C=220 μ g/ml) 2ml down, puts in the 10ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and promptly gets the solution that every 1ml contains 44 μ g.
Accurate each the 10 μ l of above-mentioned 5 reference substance solution that draw inject chromatograph of liquid, and the record chromatogram the results are shown in following table:
With the peak area is vertical coordinate, is that abscissa is made linear relationship chart with concentration (μ g/ml)
Get linear equation Y=46.063x-9.1529 R=0.9999
The linear equation that initial point is crossed in match is: Y=45.776x R=0.9999
Above-mentioned two formulas of reference substance concentration substitution are calculated, and relative standard deviation is less than 1.0%, so can think that standard curve crosses initial point, the regression equation intercept is zero, and assay can adopt one point external standard method calculating thus.Reference substance solution concentration linear relationship between 4.4 μ g/ml～44 μ g/ml is good.
7, accurate Hesperetic acid reference substance solution (C=22 μ g/ml) the 10 μ l that draw of precision test inject chromatograph of liquid, continuous sample introduction 5 times, and the record chromatogram the results are shown in following table:
Experimental result shows that this method has good precision.
8, sample stability test:
Precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, as need testing solution.The accurate need testing solution 10 μ l that draw inject chromatograph of liquid, and record chromatogram, and after need testing solution placed 0,1,2,4,8,12,24 hour is accurately respectively drawn need testing solution 10 μ l sample introductions and measured, and the record chromatogram the results are shown in following table:
Draw from above-mentioned result of the test, need testing solution is good at 24 hours internal stabilities.
9, sample replica test
Precision measure this product (lot number: 070701) 5ml, put in the 25ml measuring bottle, add 10% ethanol dilution to scale, shake up, filter, get subsequent filtrate, as need testing solution.Accurate respectively reference substance solution (concentration is 22 μ g/ml) and 6 parts of each 10 μ l sample introductions mensuration of need testing solution drawn the results are shown in following table:
Draw the sample good reproducibility of this method by above-mentioned result of the test.
10, sample pipetting volume recovery test
The preparation of reference substance solution: the accurate title, decided Hesperetic acid reference substance 12.45mg, puts in the 50ml measuring bottle, adds 10% ethanol and make dissolving, and be diluted to scale, shakes up, promptly.
The preparation of need testing solution: precision is measured this product (lot number: 070701) 5ml (6 parts in parallel sample), put in the 50ml measuring bottle, accurate more above-mentioned different attached Wei of sour reference substance solution (C=0.249mg/ml) 3ml that adds, with 10% ethanol dilution to scale, shake up, filter, get subsequent filtrate, as need testing solution.Accurate respectively Hesperetic acid reference substance solution (C=22 μ g/ml) and each 10 μ l of above-mentioned 6 parts of need testing solutions of drawing, sample introduction is measured respectively, the results are shown in following table:
Draw from above-mentioned experimental result, this method has the good response rate.
11, sample determination
Three batches of pilot scale sample size measurement results see the following form:
| Lot number | Content 1 (mg/100ml) | Content 2 (mg/100ml) | Average content (mg/100ml) |
| 070701 | 14.22 | 14.36 | 14.3 |
| 070702 | 14.41 | 14.24 | 14.3 |
| 070703 | 14.39 | 14.35 | 14.4 |
12, content limit determines
The content data table of the six batches of medical materials, finished product
According to " content limit of Rhizoma Cimicifugae medical material Hesperetic acid in the Chinese pharmacopoeia in conjunction with the Hesperetic acid rate of transform in Rhizoma Cimicifugae medical material recipe quantity in this product and the last table, is calculated as follows the content limit that draws this product:
The content limit computing formula:
According to aforementioned calculation formula result of calculation is 4mg/100ml, so the every 100ml of regulation this product contains Rhizoma Cimicifugae with Hesperetic acid (C
10H
10O
4) meter, must not be less than 4.0mg.
Embodiment:
A kind of dragon palm is sucked the quality determining method of liquid, comprises the steps:
(1) the dragon palm is sucked the discriminating of liquid: get this product 20ml, add ammonia solution 2ml, extract 2 times with the chloroform jolting, and each 10ml, combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Folium Toddaliae Asiaticae and each 1g of Radix Toddaliae Asiaticae root bark control medicinal material, adds ethanol 20ml, and reflux 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ 1 of above-mentioned two kinds of solution, select respectively on same silica gel g thin-layer plate with 1% potassium dihydrogen phosphate and the preparation of 0.5% sodium carboxymethyl cellulose mixed liquor (1: 1), with toluene-ethyl acetate (8: 2) is developing solvent, launch, taking-up is dried, and puts under the ultra-violet lamp (365nm) and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(2) according to high effective liquid chromatography for measuring content:
A, chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Acetonitrile-0.1% phosphoric acid (13: 87) is mobile phase; 30 ℃ of column temperatures; The detection wavelength is 316nm.Theoretical cam curve is pressed the Hesperetic acid peak and is calculated, and should be not less than 5000;
The preparation of B, reference substance solution: it is an amount of that precision takes by weighing the Hesperetic acid reference substance, makes the solution that every 1ml contains 20 μ g with 10% ethanol, promptly;
C, need testing solution preparation: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
D, algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
The every 100ml of this product contains Rhizoma Cimicifugae with Hesperetic acid (C
10H
10O
4) meter, must not be less than 4.0mg.
Claims (2)
1. a dragon slaps the quality determining method of sucking liquid, comprises the steps:
(1) the dragon palm is sucked the discriminating of liquid: get this product 20ml, add ammonia solution 2ml, extract 2 times with the chloroform jolting, and each 10ml, combined chloroform liquid, evaporate to dryness, residue add methanol 2ml makes dissolving, as need testing solution.Other gets Folium Toddaliae Asiaticae and each 1g of Radix Toddaliae Asiaticae root bark control medicinal material, adds ethanol 20ml, and reflux 30 minutes filters, and filtrate evaporate to dryness, residue add methanol 2ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography, draw each 10 μ l of above-mentioned two kinds of solution, select respectively in same be on 1: 1 the silica gel g thin-layer plate of mixed liquor preparation with 1% potassium dihydrogen phosphate and 0.5% sodium carboxymethyl cellulose ratio, with toluene: ethyl acetate=8: 2 is developing solvent, launch, taking-up is dried, and puts under the 365nm ultra-violet lamp and inspects.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
(2) according to high effective liquid chromatography for measuring content:
A, chromatographic condition and system suitability test: with the octadecylsilane chemically bonded silica is filler; Acetonitrile: 0.1% phosphoric acid=13: 87 is mobile phase; 30 ℃ of column temperatures; The detection wavelength is 316nm.Theoretical cam curve is pressed the Hesperetic acid peak and is calculated, and should be not less than 5000;
The preparation of B, reference substance solution: it is an amount of that precision takes by weighing the Hesperetic acid reference substance, makes the solution that every 1ml contains 20 μ g with 10% ethanol, promptly;
C, need testing solution preparation: precision is measured this product 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and with the microporous filter membrane filtration of 0.45 μ m, gets subsequent filtrate, promptly;
D, algoscopy: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
2. the dragon palm as claimed in claim 1 is sucked the quality determining method of liquid, and wherein: the every 100ml of this product contains Rhizoma Cimicifugae in Hesperetic acid, must not be less than 4.0mg.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954381A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for isoferulic acid in Rhizoma Cimicifugae |
| CN106885861A (en) * | 2017-04-11 | 2017-06-23 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine isoferulic acid content in rattletop |
| CN111905025A (en) * | 2020-09-14 | 2020-11-10 | 北京皓尔生物科技有限公司 | Traditional Chinese medicine composition for treating oral ulcer, stopping bleeding, relieving pain and diminishing inflammation and preparation method and application thereof |
| CN114236034A (en) * | 2021-12-15 | 2022-03-25 | 贵州恒霸药业有限责任公司 | Detection method of toddalia asiatica medicinal material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101095800A (en) * | 2006-06-29 | 2008-01-02 | 朱靖华 | Development of paster for treating mouth ulcer |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101095800A (en) * | 2006-06-29 | 2008-01-02 | 朱靖华 | Development of paster for treating mouth ulcer |
Non-Patent Citations (1)
| Title |
|---|
| 《贵阳中医学院学报》 20020925 成文昭等 龙掌***液质量控制方法的研究 第55-56页 1-2 第24卷, 第03期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105954381A (en) * | 2016-04-22 | 2016-09-21 | 广西壮族自治区梧州食品药品检验所 | Determination method for isoferulic acid in Rhizoma Cimicifugae |
| CN106885861A (en) * | 2017-04-11 | 2017-06-23 | 广西壮族自治区梧州食品药品检验所 | A kind of method that ASE HPLC methods determine isoferulic acid content in rattletop |
| CN111905025A (en) * | 2020-09-14 | 2020-11-10 | 北京皓尔生物科技有限公司 | Traditional Chinese medicine composition for treating oral ulcer, stopping bleeding, relieving pain and diminishing inflammation and preparation method and application thereof |
| CN111905025B (en) * | 2020-09-14 | 2022-04-01 | 北京皓尔生物科技有限公司 | Traditional Chinese medicine composition for treating oral ulcer, stopping bleeding, relieving pain and diminishing inflammation and preparation method and application thereof |
| CN114236034A (en) * | 2021-12-15 | 2022-03-25 | 贵州恒霸药业有限责任公司 | Detection method of toddalia asiatica medicinal material |
| CN114236034B (en) * | 2021-12-15 | 2024-03-29 | 贵州恒霸药业有限责任公司 | Method for detecting asiatic toddalia root blood medicinal material |
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| CN102000209B (en) | 2012-05-30 |
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Denomination of invention: Quality detection method of asiatic toddalia root gargle Effective date of registration: 20151202 Granted publication date: 20120530 Pledgee: Agricultural Bank of China, Limited by Share Ltd, Guiyang, Wudang branch Pledgor: Guiyang Xintian Pharmaceutical Industry Co., Ltd. Registration number: 2015520000008 |
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Date of cancellation: 20180606 Granted publication date: 20120530 Pledgee: Agricultural Bank of China, Limited by Share Ltd, Guiyang, Wudang branch Pledgor: Guiyang Xintian Pharmaceutical Industry Co., Ltd. Registration number: 2015520000008 |