CN103293269A - Quality control method of Chinese medicine composition for treating vascular dementia - Google Patents
Quality control method of Chinese medicine composition for treating vascular dementia Download PDFInfo
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- CN103293269A CN103293269A CN2012100621188A CN201210062118A CN103293269A CN 103293269 A CN103293269 A CN 103293269A CN 2012100621188 A CN2012100621188 A CN 2012100621188A CN 201210062118 A CN201210062118 A CN 201210062118A CN 103293269 A CN103293269 A CN 103293269A
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Abstract
The invention relates to a quality control method of a Chinese medicine composition for treating vascular dementia. The composition is prepared from the active ingredients, namely ligusticum wallichii, angelica sinensis, ginkgo leaf and herba epimedii. The quality control method disclosed by the invention comprises identification and content measurement; the identification includes identification of bilobalide and ferulic acid; and content measurement includes measurement of icariin content.
Description
Technical field: the present invention relates to a kind of method of quality control for the treatment of the Chinese medicine composition of vascular dementia, the active component of described composition is made up of Ligusticum wallichii, Radix Angelicae Sinensis, ginkgo leaf, barrenwort.
Background technology: application number is 201210025620.1 Chinese patent application, has put down in writing the Chinese medicine composition that Ligusticum wallichii, Radix Angelicae Sinensis, ginkgo leaf, barrenwort are formed.Be particularly related to Ligusticum wallichii 625g, barrenwort 625g, ginkgo leaf 375g, the Chinese medicine composition of Radix Angelicae Sinensis 375g.Said composition has the function of prevention or treatment senile vascular dementia.
The preparation method of said composition is: Ligusticum wallichii, angelica powder are broken into meal, extract volatile oil, the aqueous solution after distillation device is in addition collected.Dregs of a decoction boiling secondary, each 1 hour, merge decoction liquor, filter, filtrate merges with above-mentioned aqueous solution, is concentrated into the clear cream of relative density 1.05-1.08 (55 ℃), and room temperature to be chilled to adds ethanol and makes that to contain the alcohol amount be 70% to make precipitation, places filtration, filtrate for later use.Barrenwort, ginkgo leaf add 70% alcohol heating reflux and extract secondary, extract 2 hours at every turn, filter, and filtrate and above-mentioned filtrate merge, and reclaim ethanol, and being concentrated into relative density is 1.05-1.10 (55 ℃), and spray drying is made dry extract.Get 5 times of volatilization oil mass cycloheptaamyloses, add 2 times of amount 20% ethanol, grind to form pasty state, add above-mentioned volatile oil, ground 2 hours, low temperature drying is pulverized, with above-mentioned extract powder mixing.The dolomol of adding 2% and an amount of starch, mixing incapsulates, and makes 1000, namely.
The composition function cures mainly: promoting blood circulation and removing blood stasis, kidney tonifying intelligence development is used for the vascular dementia that the stasis of blood hinders brain key, kidney essence deficiency.Usage and dosage: oral, one time 4,3 times on the one.Specification: every dress 0.50g.
Quality how to control said composition fast and accurately is the technical matters of being badly in need of solution.
The technical problem to be solved in the present invention: the method for quality control that a kind of Chinese medicine composition of being made up of Ligusticum wallichii, Radix Angelicae Sinensis, ginkgo leaf, barrenwort is provided.
The objective of the invention is: the method for quality control of the Chinese medicine composition that a kind of active component is made up of Ligusticum wallichii, Radix Angelicae Sinensis, ginkgo leaf, barrenwort is provided, and this method is the quality of control combination thing fast and accurately.
Technical scheme of the present invention is:
Technical scheme of the present invention is: a kind of method of quality control with Chinese medicine composition of vascular dementia is characterized in that comprising discriminating.
Discriminating of the present invention comprises:
(1) gets this product content 4g, add the 20ml hot water dissolving, after the cooling, extract twice with ethyl acetate, each ethyl acetate 30ml that uses merges extract, evaporate to dryness, residue dissolves with 15% ethanol, adds on the polyamide column (3g), uses 5% ethanol elution, collect eluent 200ml, be concentrated into 50ml, cooling, concentrate extracts 2 times with ethyl acetate, and each 50ml merges extract, evaporate to dryness, residue 2ml acetone solution is as need testing solution.Other gets the Bilobalide reference substance, adds acetone and makes the solution that every 1ml contains 0.5mg, in contrast product solution.According to thin-layered chromatography (2000 version " an appendix VI of Chinese pharmacopoeia B test), absorption is to product solution 5ul, need testing solution 10ul, put respectively on the same silica gel H thin layer plate for preparing with the carboxymethylcellulose sodium solution that contains 4% sodium acetate, be developping agent with toluene-ethyl acetate-acetone-methyl alcohol (10: 5: 5: 0.6, volume ratio), launching below 15 ℃, take out, dry, about 30 minutes of 140-160 ℃ of heating, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, showing identical fluorescence spot with the corresponding position of reference substance chromatogram.
(2) get this product content 5g, add the ultrasonic processing of 40ml methyl alcohol 30 minutes, filter, filtrate evaporate to dryness, residue add 10ml water makes dissolving, adds watery hydrochloric acid and transfers PH2-3, with extracted by ether 3 times (using ether 20ml) at every turn, merge ether extracted liquid, extract 3 times (at every turn using 20ml) with 5% sodium bicarbonate solution, merge the sodium bicarbonate extract, add watery hydrochloric acid and transfer PH2-3, merge ether extracted liquid with extracted by ether 3 times (using 20ml) at every turn, fling to ether, residue adds the dissolving of 1ml methyl alcohol, as need testing solution.Other gets the forulic acid reference substance, adds the molten solution that every 1ml contains 1mg, the product solution in contrast made of methyl alcohol.According to thin-layered chromatography (2000 version " an appendix VI of Chinese pharmacopoeia B test), absorption is to product solution 5ul, need testing solution 15ul, put respectively on same silica gel g thin-layer plate with the carboxymethylcellulose sodium solution preparation, be developping agent with benzene-ethyl acetate-formic acid (5: 2: 0.2), launch, take out, dry, put under the ultraviolet lamp (365nm) and inspect.In the test sample chromatogram, showing identical fluorescence spot with the corresponding position of reference substance chromatogram.
Technical scheme of the present invention also comprises Determination on content.
Ligusticum wallichii is the monarch drug in a prescription of this product, once is index with the forulic acid during assay, adopts the HPLC method to measure, but the less stable of forulic acid is not suitable for measuring.Measure with the TLCS method, the forulic acid spot is very fast variable color on thin layer plate, is not suitable for assay.
Barrenwort is the ministerial drug of this product, and its active component is the flavone glycoside composition based on icariin, so this preparation is also controlled index with the icariin in the barrenwort as content.No matter be that the mensuration of icariin adopts high effective liquid chromatography for measuring more in the epimedium herb or in the preparation at present, because it is measured accurately, sensitivity, simple, so the mensuration of icariin also adopts high effective liquid chromatography for measuring in this preparation.
Icariin Determination on content method of the present invention comprises:
Chromatographic condition and system suitability test are filling agent with octadecyl silane, and acetonitrile-water (28: 72, volume ratio) is the phase that flows; The detection wavelength is 270nm.Theoretical cam curve must not calculate by the icariin peak and is lower than 1500.
It is an amount of that the preparation precision of reference substance solution takes by weighing in the phosphorus pentoxide vacuum drying apparatus dry icariin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, shakes up, namely.
The preparation of need testing solution takes by weighing the content 1.0g under the content uniformity item, and accurate the title decides, and puts in the tool plug conical flask, the accurate 50ml50% ethanol that adds claims to decide weight, ultrasonic processing 30 minutes, be placed to room temperature, claim again to decide weight, add 50% ethanol and supply the weight that subtracts mistake, shake up, filter, discard filtrate just, the accurate subsequent filtrate 25ml that draws flings to ethanol, and residue adds water 20ml heating for dissolving, after the cooling, 5 times (consumption is respectively 30,30 with the ethyl acetate extraction, 30,20,20ml) merge the ethyl acetate extract, fling to solvent, residue adds the ethanol dissolving, quantitatively is transferred in the 25ml measuring bottle, adds ethanol to scale, mixing is as need testing solution.
Determination method is accurate reference substance solution and each 20ul of need testing solution of drawing respectively, injects high performance liquid chromatograph, measures, namely.
Every of this product contains barrenwort with icariin (C
33H
10O
15) meter, must not be less than 1.85mg.
Technical scheme of the present invention also comprises: the inspection of proterties.
Proterties: this product is capsule, and content is chocolate brown powder; The little perfume (or spice) of gas, bitter.
The invention has the beneficial effects as follows: the method for quality control of the Chinese medicine composition that a kind of active component is made up of Ligusticum wallichii, Radix Angelicae Sinensis, ginkgo leaf, barrenwort is provided, and this method is the quality of control combination thing fast and accurately.
Embodiment 1 icariin assay
Instrument and reagent: the efficient liquid phase liquid chromatograph in Tianjin, island.Chromatographic column: KromasilC18 (5u, 4.6mm, 30cm).Reagent is for analyzing pure or chromatographically pure.The icariin reference substance is purchased in Nat'l Pharmaceutical ﹠ Biological Products Control Institute (for assay 0737-9709).
Extracting method: " assay method of icariin under barrenwort item of Chinese pharmacopoeia was that solvent adopts ultrasonic facture to extract with 50% ethanol with reference to version in 2000.Experiment shows that adding the ultrasonic processing of quantitative solvent can make extraction reach balance in 30 minutes, so determined the extracting method of this product.Experimental technique and result are as follows:
Precision take by weighing this product (lot number: 201102) 0.4218g, 0.4316g, 0.4267g, insert in the round-bottomed flask each accurate 25ml methyl alcohol that adds respectively, accurate claim surely, ultrasonic processing 10 respectively, 30,60 minutes adds methyl alcohol and mends from the quantity of methyl alcohol of loss after the cooling, method is measured for another example, the results are shown in Table 1.
The selection of table 1 extraction time
| Sampling amount, g | Extraction time (minute) | Icariin content mg/g |
| 0.4218 | 10 | 3.49 |
| 0.4316 | 30 | 4.73 |
| 0.4267 | 60 | 4.70 |
Test findings shows: extraction time is 30 minutes, namely can extract fully.
The same text of preparation of the selection need testing solution of the phase that flows.The same text of the preparation of reference substance is made the solution that every 1ml contains the 0.3mg icariin; The preparation of negative control: get negative control (lacking barrenwort) product, make negative control solution with the method for making of text need testing solution.
Mobile phase has at first been tested the mobile phase under the pharmacopeia barrenwort item: acetonitrile-water (30: 70, volume ratio), the degree of separation of icariin is bad.Test finds that adjusting flows is mutually: during second eyeball-water (28: 72, volume ratio), the degree of separation of icariin is better, so adopt.
The analysis of degree of separation: degree of separation R is with peak, front R=1.62
Blank test absorption reference substance solution, need testing solution, negative control product solution 20ul enter high performance liquid chromatograph respectively, detect by the method for determining.Reference substance solution has corresponding peak with need testing solution in identical retention time as a result, and negative control does not have.Illustrate that the specificity of measuring is good, noiseless.
The investigation of linear relationship: precision takes by weighing reference substance 2.16mg and puts and add methyl alcohol dissolving in the 10ml measuring bottle, and is diluted to scale, and mixing is drawn an amount of reference substance solution, adds the different concentration of the rare one-tenth of methyl alcohol respectively, measures as method.The results are shown in Table 2.
Table 2 linear relationship investigation table
| Reference substance concentration, g/ml | 0.0108 | 0.0216 | 0.0432 | 0.0864 | 0.1296 | 0.1728 | 0.2160 |
| Peak area | 220419 | 447070 | 794792 | 1774852 | 2747567 | 3526878 | 4564575 |
Regression equation Y=-40994.2+21109806.1X
Coefficient R=0.9994
Illustrate that icariin is the better linearity relation between 0.01-0.20mg/ml.With peak area to concentration map a straight line.
The precision test: draw reference substance solution (0.17mg/ml) and need testing solution, METHOD FOR CONTINUOUS DETERMINATION 5 times records peak area, asks and calculates coefficient of variation RSD.The results are shown in Table 3
Table 3 precision is investigated
Test findings shows that the precision of this method mensuration is higher, meets the requirement of assay.
Stability test: for the stability of measuring, same reference substance (0.12mg/ml) and need testing solution were measured once every 2-4 hour, measured altogether 5 times.The results are shown in Table 4
Table 4 methodology stability experiment
Experiment shows: the icariin in icariin reference substance and the test liquid is better at 12 hours internal stabilities, meets the requirement of assay.
Can the recovery is investigated in order to observe assay method determine content Determination of Icariin in the preparation accurately, and we have measured content Determination of Icariin in the sample by the method for formulating, and carry out application of sample and reclaim experiment, calculate recovery rate.
Take by weighing preparation (7.50mg/g content) 0.5g of known icariin content, add icariin solution (3.76mg/ml) 1ml, measure content Determination of Icariin as method, calculate recovery rate the results are shown in Table 5
Table 5 recovery test result
The recovery height of this assay method meets the requirement of assay as shown in Table 5.
The mensuration of repeatability: get this product (lot number 201102), measure content Determination of Icariin by the method for determining, measure altogether 5 times, the results are shown in Table 6
Table 6 replica test result
Experimental result shows the good reproducibility that this law is measured, and the coefficient of variation is little, meets the requirement of assay.
The formulation of content limit
Measured 4 batch samples according to the assay method that text is formulated, every batch sample has been measured twice.The results are shown in Table 7
Icariin assay result in table 74 batch sample
Test findings shows: 4 batch samples are made by two batches of different barrenwort respectively, content Determination of Icariin is respectively 0.52% in two batches of barrenwort, 0.62%, conversion ratio is respectively 60%, 62%, can also find out simultaneously, the content of barrenwort crude drug is low, the conversion ratio of icariin is also low, must not be less than 0.5% requirement to icariin in the barrenwort according to pharmacopeia, the result that 4 batch samples are measured and the conversion ratio of icariin, contain content 0.50g by every capsules and calculate, determine that the content of barrenwort in this product must not be lower than the 1.85mg/ capsules in icariin.
What post was imitated determines: by calculating, the theoretical tray number average at icariin peak can reach more than 1500, is lower than 1500 so the regulation theoretical cam curve must not calculate by the icariin peak.
Claims (8)
1. the method for quality control of a Chinese medicine composition of being made up of Ligusticum wallichii, Radix Angelicae Sinensis, ginkgo leaf, barrenwort is characterized in that comprising discriminating.
2. the described method of quality control of claim 1 is characterized in that also comprising the icariin Determination on content.
3. the described method of quality control of claim 1, its discrimination method is:
Get this product content 4g, add the 20ml hot water dissolving, after the cooling, extract twice with ethyl acetate, each ethyl acetate 30ml that uses merges extract, evaporate to dryness, residue dissolves with 15% ethanol, adds on the polyamide column (3g), uses 5% ethanol elution, collect eluent 200ml, be concentrated into 50ml, cooling, concentrate extracts 2 times with ethyl acetate, and each 50ml merges extract, evaporate to dryness, residue 2ml acetone solution is as need testing solution.Other gets the Bilobalide reference substance, adds acetone and makes the solution that every 1ml contains 0.5mg, in contrast product solution;
According to " the thin-layered chromatography test of an appendix VI of Chinese pharmacopoeia B regulation, absorption is to product solution 5ul, need testing solution 10ul, put respectively on the same silica gel H thin layer plate for preparing with the carboxymethylcellulose sodium solution that contains 4% sodium acetate, with volume ratio 10: 5: 5: toluene-ethyl acetate-acetone of 0.6-methyl alcohol was developping agent, launching below 15 ℃, take out, dry, about 30 minutes of 140-160 ℃ of heating, put under the wavelength 365nm ultraviolet lamp and inspect, in the test sample chromatogram, showing identical fluorescence spot with the corresponding position of reference substance chromatogram.
4. the described method of quality control of claim 1, its discrimination method is: get this product content 5g, add the ultrasonic processing of 40ml methyl alcohol 30 minutes, filter, the filtrate evaporate to dryness, residue adds 10ml water makes dissolving, adds watery hydrochloric acid and transfers PH2-3, with extracted by ether 3 times, each ether 20ml that uses, merge ether extracted liquid, extract 3 times with 5% sodium bicarbonate solution, use 20ml at every turn, merge the sodium bicarbonate extract, add watery hydrochloric acid and transfer PH2-3, with extracted by ether 3 times, use 20ml at every turn, merge ether extracted liquid, fling to ether, residue adds the dissolving of 1ml methyl alcohol, as need testing solution.Other gets the forulic acid reference substance, adds the molten solution that every 1ml contains 1mg, the product solution in contrast made of methyl alcohol.According to " the thin-layered chromatography test of an appendix VI of Chinese pharmacopoeia B regulation, absorption is to product solution 5ul, need testing solution 15ul, put respectively on same silica gel g thin-layer plate with the carboxymethylcellulose sodium solution preparation, be that 5: 2: 0.2 benzene-ethyl acetate-formic acid is developping agent with volume ratio, launch, take out, dry, putting wavelength is to inspect under the 365nm ultraviolet lamp, in the test sample chromatogram, is showing identical fluorescence spot with the corresponding position of reference substance chromatogram.
5. the described method of quality control of claim 2 is characterized in that icariin Determination on content method comprises:
The test of chromatographic condition and system suitability: be filling agent with octadecyl silane, volume ratio is that 28: 72 acetonitrile-water is mobile phase, and the detection wavelength is 270nm, and theoretical cam curve must not calculate by the icariin peak and is lower than 1500;
The preparation of reference substance solution: it is an amount of that precision takes by weighing in the phosphorus pentoxide vacuum drying apparatus dry icariin reference substance, adds methyl alcohol and make the solution that every 1ml contains 0.1mg, shakes up, namely;
The preparation of need testing solution: take by weighing the content 1.0g under the content uniformity item, the accurate title, decide, and puts in the tool plug conical flask, the accurate 50ml50% ethanol that adds claims to decide weight, ultrasonic processing 30 minutes, be placed to room temperature, claim again to decide weight, add 50% ethanol and supply the weight that subtracts mistake, shake up, filter, discard filtrate just, the accurate subsequent filtrate 25ml that draws flings to ethanol, and residue adds water 20ml heating for dissolving, after the cooling, extract 5 times with ethyl acetate, consumption is respectively 30,30,30,20,20ml merges the ethyl acetate extract, flings to solvent, residue adds the ethanol dissolving, quantitatively is transferred in the 25ml measuring bottle, adds ethanol to scale, mixing is as need testing solution;
Determination method: precision is drawn reference substance solution and each 20ul of need testing solution respectively, injects high performance liquid chromatograph, measures, namely.
6. the described method of quality control of claim 1, its every of feature this product contains barrenwort with icariin C
33H
40O
15Meter must not be less than 1.85mg.
7. the described method of quality control of claim 1 comprises the inspection of proterties.
8. the described method of quality control of claim 8, its proterties is that content is chocolate brown powder; The little perfume (or spice) of gas, bitter.
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Citations (3)
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|---|---|---|---|---|
| CN1457852A (en) * | 2003-05-14 | 2003-11-26 | 居小平 | A Chinese medicinal composition for treating traumatic injury and pain in chest and hypochondrium, and its preparation method |
| CN1876028A (en) * | 2005-05-12 | 2006-12-13 | 贵阳云岩西创药物科技开发有限公司 | Pharmaceutical preparation for treating coronary heart disease, its preparation process and quality control method |
| CN101301300A (en) * | 2007-05-09 | 2008-11-12 | 北京本草天源药物研究院 | Medicament composition |
-
2012
- 2012-03-02 CN CN2012100621188A patent/CN103293269A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1457852A (en) * | 2003-05-14 | 2003-11-26 | 居小平 | A Chinese medicinal composition for treating traumatic injury and pain in chest and hypochondrium, and its preparation method |
| CN1876028A (en) * | 2005-05-12 | 2006-12-13 | 贵阳云岩西创药物科技开发有限公司 | Pharmaceutical preparation for treating coronary heart disease, its preparation process and quality control method |
| CN101301300A (en) * | 2007-05-09 | 2008-11-12 | 北京本草天源药物研究院 | Medicament composition |
Non-Patent Citations (3)
| Title |
|---|
| 国家药典委员会 编: "《中华人民共和国药典 2010年版 一部》", 31 January 2010, article "银杏叶，淫羊藿", pages: 296-297 - 306-308 * |
| 崔晓红 等: "益肾强身片中淫羊藿苷的含量测定", 《中国新药杂志》, vol. 14, no. 11, 30 November 2005 (2005-11-30), pages 1323 - 1325 * |
| 李旭明: "康脑灵胶囊抗痴呆大鼠自由基损伤的作用机制研究", 《中国中医药信息杂志》, vol. 14, no. 11, 30 November 2007 (2007-11-30), pages 21 - 22 * |
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Application publication date: 20130911 |