CN102000209B - 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 Radix Toddaliae Asiaticae skin, asiatic toddalia leaf, the root bark of Chinese wolf-berry, rattletop four traditional Chinese medicine material that the dragon palm is sucked liquid, boiling three times, for the first time, 2 hours for the second time, 1 hour for the third time; Collecting decoction filters, and filtrating is concentrated into the clear cream that relative density is 1.10～1.15 (60～70 ℃), adds ethanol and makes that to contain the alcohol amount be 70%; Left standstill 24 hours, and got supernatant, filter, filtrate recycling ethanol also is concentrated into the clear cream that relative density is 1.10～1.15 (60～70 ℃); Add polyoxyethylene sorbitan monoleate, glycerine, mixing boils, and is cooled to below 40 ℃; Add methyl hydroxybenzoate, ethyl hydroxy benzoate, menthol, flavoring rose essence, cocoanut flavour, add water to ormal weight, mixing leaves standstill; Filter, can promptly gets.Be pale brown look to henna supernatant liquid, postpone for a long time has small amount of precipitate; Gas delicate fragrance, sweet, little hardship of distinguishing the flavor of.Function cures mainly: the seedling doctor: lift by force, lift and buy (or sell) on credit: the Lip river item, article in the loud, high-pitched sound are reined in the labour palace, rein in Ga Guomian.The traditional Chinese medical science: stasis of blood hemostasis, removing dampness and detoxicating, swelling and pain relieving loose.Be used for halitosis, RAU (canker sore), gingivitis, periodontitis.Assay in the proper mass standard is to detect the contained forulic acid of rattletop medicinal material in the prescription, but in long-term production, finds; As containing the survey index, production quality control there is following some weak point with forulic acid, 1, a large amount of documents and materials all have report; The forulic acid solution of water or methyl alcohol (ethanol) preparation is unstable; See that auroral poles is prone to decompose, 2h can be reduced to 20% of relative content after forulic acid was seen light, thereby reduced the check accuracy.2, with forulic 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 medicinal material contains forulic acid must not be less than 0.07%; And commercially available most medicinal material ferulaic acid content does not all reach this limit, buys satisfactory medicinal material and is not easy very much.3, the adjacent peak-to-peak degree of separation with other in forulic acid peak is lower than 1.5 in liquid chromatography, 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 that the objective of the invention is to overcome above-mentioned shortcoming and provide is high, and the dragon palm that medicinal 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 these article 20ml, add ammonia solution 2ml, extract 2 times with the chloroform jolting, and each 10ml, combined chloroform liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Other gets asiatic toddalia leaf and each 1g of Radix Toddaliae Asiaticae skin control medicinal material, adds ethanol 20ml, and reflux 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 2ml makes dissolving, as control medicinal material solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Draw each 10 μ l of above-mentioned two kinds of solution; Selecting 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), is developping agent with toluene-ethyl acetate (8: 2), launches; Taking-up is dried, and puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot 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 filling agent; Acetonitrile-0.1% phosphoric acid (13: 87) is moving phase; 30 ℃ of column temperatures; The detection wavelength is 316nm.Theoretical cam curve is pressed the isoferulic 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 isoferulic acid reference substance, processes the solution that every 1ml contains 20 μ g with 10% ethanol, promptly gets;
C, need testing solution preparation: precision is measured these article 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and with the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets;
D, determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
The above-mentioned dragon palm is sucked the quality determining method of liquid, and wherein: the every 100ml of these article contains rattletop with isoferulic acid (C
10H
10O
4) meter, must not be less than 4.0mg.
The present invention compared with prior art has tangible beneficial effect, can be known by above technical scheme, adopts and sees that the not labile isoferulic acid of light is as containing the survey index.To guarantee the check accuracy.Commercially available most medicinal material isoferulic acid content has all reached requirement, buys satisfactory medicinal material and is easy to.In liquid chromatography, between isoferulic acid peak and other peak good separating arranged all, thereby guaranteed the accuracy of assay.Guarantee the security of medication, better instruct and produce, make technology controlling and process rationally strict more.
Embodiment
Below further specify the beneficial effect that the dragon palm of the present invention is sucked the quality determining method of liquid through Test Example:
Test Example:
1, reference substance, reagent and reagent
1.1 instrument: Agilent 1100 type high performance liquid chromatographs, VWD detecting device, 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: isoferulic acid reference substance (lot number: 111698-200501) supply assay usefulness, purchase in Nat'l Pharmaceutical & Biological Products Control Institute.
1.3 reagent: ethanol, phosphoric acid are that analysis is 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 isoferulic acid reference substance 11.00mg, puts in the 50ml measuring bottle, adds 10% ethanolic 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 asafoetide content assaying method of Chinese pharmacopoeia rattletop medicinal material of version in 2005
Chromatographic column: octadecylsilane chemically bonded silica is filling agent (the special ODS2 C18 250mm * 4.6mm of Erie, 5 μ m)
Moving phase: acetonitrile-phosphoric acid (13: 87)
Flow velocity: 1.0ml/ minute
Detect wavelength: 316nm
The preparation of need testing solution: precision is measured these article 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 liquid chromatograph, the record chromatogram.
The result can find out from the test sample collection of illustrative plates has good degree of separation between isoferulic acid peak and other peak, peak shape is good, post is imitated height, 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 these article 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly gets.
Method 2: precision is measured these article 5ml, and with ethyl acetate extraction 4 times (20ml, 15ml, 10ml, 10ml), combined ethyl acetate extract, evaporate to dryness, residue add dissolve with ethanol and be transferred in the 25ml measuring bottle, add ethanol dilution to scale, shake up, and promptly get.
Method 3: precision is measured these article 5ml, puts in the 25ml measuring bottle, adds ethanol dilution to scale, shakes up, and filters, and gets subsequent filtrate, promptly gets.
Method 4: precision is measured these article 5ml, puts in the 25ml measuring bottle, and thin up shakes up to scale, filters, and gets subsequent filtrate, promptly gets.
Accurate respectively isoferulic acid reference substance solution (C=22 μ g/ml) and 4 each 10 μ l of need testing solution of drawing inject liquid chromatograph, the record chromatogram, and the result sees the following form:
Conclusion: can find out in each method, between isoferulic acid peak and other peak good separating arranged all from above test findings; Method 1,4 content are the highest, take all factors into consideration so list method 1 in text, and be: precision is measured these article 5ml; Put in the 25ml measuring bottle, add 10% ethanol dilution, shake up to scale; Filter, get subsequent filtrate, promptly get.
5, system suitability test
Precision is measured these article 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 processes 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 liquid chromatograph, 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, explain that negative sample is noiseless to sample determination.The number of theoretical plate at the isoferulic acid peak of sample in collection of illustrative plates is 20175; With other material good separating arranged; Peak shape is good; With reference to " theoretical cam curve of a rattletop medicinal material of Chinese pharmacopoeia version in 2005 isoferulic acid assay defined stipulates that the theoretical cam curve of this experiment is calculated by the isoferulic acid peak, should be lower than 5000.
6, linear relationship test
Reference substance solution is 1.: precision is measured 2 different asafoetide 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 asafoetide 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 asafoetide reference substance solution (C=22 μ g/ml) down
Reference substance solution is 4.: precision is measured 2 different asafoetide 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 asafoetide 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 liquid chromatograph, the record chromatogram, and the result sees the following form:
With the peak area is ordinate, is that horizontal ordinate is made linear relationship chart with concentration (μ g/ml)
Get linear equation Y=46.063x-9.1529 R=0.9999
The straight-line 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 typical 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 isoferulic acid reference substance solution (C=22 μ g/ml) the 10 μ l that draw of precision test inject liquid chromatograph, continuous sample introduction 5 times, and the record chromatogram, the result sees the following form:
Experimental result shows that this method has good precision.
8, sample stability test:
Precision is measured these article 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 liquid chromatograph, 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, the record chromatogram, and the result sees the following form:
Draw from above-mentioned test findings, need testing solution is good at 24 hours internal stabilities.
9, sample replica test
Precision measure these article (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 result sees the following form:
Draw the sample good reproducibility of this method through above-mentioned test findings.
10, sample pipetting volume recovery test
The preparation of reference substance solution: the accurate title, decided isoferulic acid reference substance 12.45mg, puts in the 50ml measuring bottle, adds 10% ethanol and make dissolving, and be diluted to scale, shakes up, and promptly gets.
The preparation of need testing solution: precision measure these article (lot number: 070701) 5ml (parallel appearance 6 parts), put in the 50ml measuring bottle, accurately again add above-mentioned different acid Wei reference substance solution (C=0.249mg/ml) 3ml that attaches;, shake up to scale with 10% ethanol dilution, filter; Get subsequent filtrate, as need testing solution.Accurate respectively isoferulic 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, and the result sees the following form:
Draw from above-mentioned experimental result, this method has the good recovery.
11, sample determination
Three batches of pilot scale sample sizes are measured the result and are seen 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 confirms
The content data table of the six batches of medicinal materials, finished product
According to " content limit of rattletop medicinal material isoferulic acid in the Chinese pharmacopoeia in conjunction with the isoferulic acid rate of transform in rattletop medicinal material recipe quantity in these article and the last table, is calculated as follows the content limit of these article of drawing:
The content limit computing formula:
According to aforementioned calculation formula result of calculation is 4mg/100ml, thus regulation originally the every 100ml of article contain rattletop with isoferulic 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 these article 20ml, add ammonia solution 2ml, extract 2 times with the chloroform jolting, and each 10ml, combined chloroform liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution.Other gets asiatic toddalia leaf and each 1g of Radix Toddaliae Asiaticae skin control medicinal material, adds ethanol 20ml, and reflux 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 2ml makes dissolving, as control medicinal material solution.Test according to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Draw each 10 μ 1 of above-mentioned two kinds of solution; Selecting 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), is developping agent with toluene-ethyl acetate (8: 2), launches; Taking-up is dried, and puts under the ultraviolet lamp (365nm) and inspects.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot 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 filling agent; Acetonitrile-0.1% phosphoric acid (13: 87) is moving phase; 30 ℃ of column temperatures; The detection wavelength is 316nm.Theoretical cam curve is pressed the isoferulic 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 isoferulic acid reference substance, processes the solution that every 1ml contains 20 μ g with 10% ethanol, promptly gets;
C, need testing solution preparation: precision is measured these article 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and with the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets;
D, determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
The every 100ml of these article contains rattletop with isoferulic 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 these article 20ml, add ammonia solution 2ml, extract 2 times with the chloroform jolting, and each 10ml, combined chloroform liquid, evaporate to dryness, residue add methyl alcohol 2ml makes dissolving, as need testing solution; Other gets asiatic toddalia leaf and each 1g of Radix Toddaliae Asiaticae skin control medicinal material, adds ethanol 20ml, and reflux 30 minutes filters, the filtrating evaporate to dryness, and residue adds methyl alcohol 2ml makes dissolving, as control medicinal material solution; Test according to thin-layered 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 be a developping agent, expansion; Taking-up is dried, and puts under the 365nm ultraviolet lamp and inspects; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the fluorescence spot 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 filling agent; Acetonitrile: 0.1% phosphoric acid=13: 87 is moving phase; 30 ℃ of column temperatures; The detection wavelength is 316nm; Theoretical cam curve is pressed the isoferulic 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 isoferulic acid reference substance, processes the solution that every 1ml contains 20 μ g with 10% ethanol, promptly gets;
C, need testing solution preparation: precision is measured these article 5ml, puts in the 25ml measuring bottle, adds 10% ethanol dilution to scale, shakes up, and with the miillpore filter filtration of 0.45 μ m, gets subsequent filtrate, promptly gets;
D, determination method: accurate respectively reference substance solution and each 10 μ l of need testing solution of drawing, inject liquid chromatograph, measure, promptly get.
2. the dragon palm as claimed in claim 1 is sucked the quality determining method of liquid, and wherein: the every 100ml of these article contains rattletop in isoferulic acid, must not be less than 4.0mg.
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| 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 |
| 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 |
| 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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| CN101095800A (en) * | 2006-06-29 | 2008-01-02 | 朱靖华 | Development of paster for treating mouth ulcer |
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| CN101095800A (en) * | 2006-06-29 | 2008-01-02 | 朱靖华 | Development of paster for treating mouth ulcer |
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| Title |
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| 成文昭等.龙掌***液质量控制方法的研究.《贵阳中医学院学报》.2002,第24卷(第03期),第55-56页. * |
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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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