CN102204998B - Method for measuring content of verbascoside in callicarpa nudiflora preparation - Google Patents
Method for measuring content of verbascoside in callicarpa nudiflora preparation Download PDFInfo
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- CN102204998B CN102204998B CN 201010289134 CN201010289134A CN102204998B CN 102204998 B CN102204998 B CN 102204998B CN 201010289134 CN201010289134 CN 201010289134 CN 201010289134 A CN201010289134 A CN 201010289134A CN 102204998 B CN102204998 B CN 102204998B
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Abstract
The invention discloses a method for measuring the content of verbascoside in a callicarpa nudiflora preparation, relating to a method for measuring the content of effective ingredients in the callicarpa nudiflora preparation. A high performance liquid chromatography (HPLC) is used for measuring the content of verbascoside in the test article solution of the callicarpa nudiflora preparation. Chromatographic conditions and system suitability are as follows: octadecylsilane chemically bonded silica is used as a filler, a flowing phase contains an organic solvent and an acidic solution, the volume percent of the organic solvent in the flowing phase is 10-30%, the volume percent of the acidic solution in the flowing phase is 70-90%, the concentration of the acidic solution is 0-0.3%, and the detection wavelength is 322-345nm. The method disclosed by the invention can be used for accurately and effectively measuring the content of verbascoside in the callicarpa nudiflora preparation, has a small error, can further improve the quality standard of the callicarpa nudiflora preparation, and can ensure the quality and clinical effect of the callicarpa nudiflora preparation.
Description
Technical field
The present invention relates to the assay method of active constituent content in the callicarpa nudiflora preparation, relate in particular to the assay method of acteoside content in the callicarpa nudiflora preparation.
Background technology
Callicarpa nudiflora (Callicarpanudiflorae) is Verenaceae undershrub plant, the effect that hemostasis, antibiotic, convergence, detoxifcation, analgesia is arranged and promote healing.Its antibiotic, antivirus action especially all has different inhibiting effect to golden staphylococci, typhoid bacillus, Diplococcus pneumopniae etc., and wherein to golden staphylococci, the typhoid bacillus bacteriostasis is the strongest.The callicarpa nudiflora permeability that also can suppress capillary, to early stage inflammation ooze out, swelling has obvious anti-inflammatory response effect, can obviously shorten simultaneously, the clotting time, haemostatic effect is remarkable.Callicarpa nudiflora principal ingredient is glycosides displayed, condensed tannins, neutral resins, phenols, polysaccharide, hydroxyl compound and magnesium, calcium, molysite etc., wherein, the content of the Flavonoid substances such as Japanses beauty-berry terpene ketone, apiolin, acteoside, cyanidenon and glycocide thereof is about 5%.When the pharmacological effect of antibiotic, the anti-inflammatory take acteoside as the callicarpa nudiflora medicinal extract of Study of indices and hemostasis, experimental result shows that along with the rising of acteoside content, antibacterial anti-inflammatory and the anastalsis of callicarpa nudiflora medicinal extract all strengthen.
Callicarpa nudiflora preparation mainly contains granule, capsule, tablet, dispersing tablet, mixture, soft capsule, suppository etc. in the market, the quality standard of above-mentioned preparation only part preparation has been carried out the assay of general flavone, assay method is ultraviolet spectrophotometry, quantitatively very inaccurate, there is not the content assaying method about acteoside in the callicarpa nudiflora preparation.
Summary of the invention
The objective of the invention is for the deficiencies in the prior art, provide a kind of can Accurate Determining the assay method of acteoside content in the callicarpa nudiflora preparation of content.
The objective of the invention is to be achieved by the following technical programs:
The assay method of acteoside content in the callicarpa nudiflora preparation, adopt the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring, it is characterized in that, chromatographic condition and system suitability are: be filling agent with octadecylsilane chemically bonded silica, mobile phase is You machine Rong Ji – acid solution, the percent by volume of organic solvent is 10-30% in the mobile phase, the percent by volume of acid solution is 70-90%, acid solution concentration is 0-0.3%, and the detection wavelength is 322-345nm.
Organic solvent in the described mobile phase comprises a kind of in methyl alcohol or the acetonitrile, and methyl alcohol and acetonitrile are chromatographically pure; The acid of acid solution comprise a kind of in acetic acid or the phosphoric acid, acetic acid and phosphoric acid be analyze pure.
The more excellent condition of described chromatographic condition and system suitability is: be that filling agent Yi Jing – acetum is mobile phase with octadecylsilane chemically bonded silica, the percentage by weight of acetonitrile is 16% in the mobile phase, the percentage by weight of acetum is 84%, the concentration of acetum is 0.1%, and the detection wavelength is 332nm.
The preparation method of described callicarpa nudiflora preparation need testing solution is: get callicarpa nudiflora preparation, be equivalent to callicarpa nudiflora medicinal extract 0.05-1.5g, weighed, put in the tool plug triangular flask, adding concentration is 30-100% methyl alcohol 15-50ml, weighed weight, ultrasonic processing is 15-45 minute under power 250w and frequency 33kHz, lets cool, more weighed weight, adding concentration is the weight that 30-100% methyl alcohol is supplied minimizing, shakes up.Filter, get subsequent filtrate and again filter with the miillpore filter of 0.45 μ m, get subsequent filtrate, and get final product.
The more excellent preparation method of described callicarpa nudiflora particle need testing solution is: get 2 bags of callicarpa nudiflora particles, porphyrize is got 0.7g, be equivalent to callicarpa nudiflora medicinal extract 0.187g, weighed, put in the tool plug triangular flask, adding concentration is 50% methyl alcohol 25ml, weighed weight, ultrasonic processing is 30 minutes under power 250w and frequency 33kHz, lets cool, more weighed weight, adding concentration is the weight that 50% methyl alcohol is supplied minimizing, shakes up.Filter, get subsequent filtrate with the miillpore filter filtration of 0.45 μ m, get subsequent filtrate, and get final product.
Described callicarpa nudiflora preparation is: take callicarpa nudiflora single preparations of ephedrine as main ingredient.
Described callicarpa nudiflora preparation is: contain callicarpa nudiflora compound preparation.
Described callicarpa nudiflora preparation is: contain callicarpa nudiflora solid pharmaceutical preparation, liquid preparation, external preparation, soft capsule, dripping pill and parenteral solution.
Described solid pharmaceutical preparation is particle, capsule, tablet, dispersing tablet, powder, pill; Liquid preparation is mixture, oral liquid, syrup; External preparation is suppository, ointment, cream.
The invention has the beneficial effects as follows: can measure accurately and effectively the content of acteoside in the callicarpa nudiflora preparation, error is little, can further improve the quality standard of callicarpa nudiflora preparation, guarantees quality and the clinical effectiveness of callicarpa nudiflora preparation.
1.1 the selection of chromatographic conditionChromatographic column: Dikma Diamonsil C18 (2) post, 4.6mm * 250mm, 5 μ m, mobile phase: acetonitrile-concentration is 0.1% acetum (percent by volume of acetonitrile and acetum is 16:84), flow velocity: 1ml/min detects wavelength 332nm, column temperature: room temperature.Reference substance, test sample have a chromatographic peak at about 15min same time with this understanding, see Fig. 1-Fig. 2.
1.2 negative control testGet other auxiliary materials that do not contain callicarpa nudiflora medicinal material by prescription, make the negative control sample, preparation method by described callicarpa nudiflora preparation need testing solution makes negative control product solution again, get negative control sample and each 10ml of negative control product solution, the injection liquid chromatography, the result occurs without other chromatographic peak on the corresponding position of reference substance acteoside chromatographic peak, negative control is noiseless to sample determination, the results are shown in negative control chromatogram 3.
1.3 extract the selection of solventSelecting respectively concentration is that 70% ethanol, methyl alcohol, concentration are that 50% methyl alcohol, ethanol are for extracting solvent, take by weighing respectively totally 4 parts of the about 0.8g of sample fine powder, put in the tool plug triangular flask, each adds above-mentioned solvent 25ml, weighed weight, ultrasonic processing 30 minutes lets cool, add respectively above-mentioned solvent and supply the weight that subtracts mistake, filter.Draw subsequent filtrate, filter with miillpore filter (0.45 μ m), get filtrate, namely get need testing solution; It is an amount of that other gets the acteoside reference substance, and adding concentration is that 50% methyl alcohol is made the reference substance solution that every 1ml contains 0.040mg.Draw respectively each 10ml of above-mentioned need testing solution and reference substance solution, inject respectively the liquid phase instrument, record the acteoside content results and see Table 1.
Table 1 different solvents extracts the content of acteoside
Table 1 measurement result shows, acteoside content is low in the ethanol extract, concentration is that 50% methyl alcohol, concentration are that acteoside content is higher in 70% ethanol extract, but concentration is that 70% ethanol extract color is darker, is that 50% methyl alcohol is as extracting solvent so adopt concentration.
1.4 the investigation of sample extraction timeSample thief, porphyrize takes by weighing about 0.7g, and totally 3 parts, put in the 50ml tool plug triangular flask, adding respectively concentration is 50% methyl alcohol 25ml, weighed weight, ultrasonic processing is 15 minutes, 30 minutes, 45 minutes respectively, lets cool, and adding concentration is the weight that 50% methyl alcohol is supplied minimizing.Filter, draw subsequent filtrate, filter with miillpore filter (0.45 μ m), get filtrate, and get final product.Draw respectively reference substance solution in 1.3, each 10ml of need testing solution, the injection liquid chromatography is measured, and be get final product.The results are shown in Table 2.
Table 2 different extraction times are on the impact of measurement result
With 30 minutes effects of ultrasonic extraction for well, so select ultrasonic extraction 30 minutes.
1.5 extract the investigation of solvent loadSample thief, porphyrize takes by weighing about 0.7g, totally three parts, put in the 100ml tool plug triangular flask, add 50%(concentration?) methyl alcohol (being respectively 15ml, 25ml, 50ml), weighed weight, ultrasonic processing 30 minutes lets cool, add 50%(concentration?) methyl alcohol supplies the weight of minimizing.Filter, draw subsequent filtrate, filter with miillpore filter (0.45 μ m), get (continuing) filtrate, and get final product.Draw respectively reference substance solution in 1.3, each 10ml of need testing solution, the injection liquid chromatography is measured.The results are shown in Table 3.
Table 3 different solvents amount is on the impact of measurement result
The 25ml extraction effect is better, so intend extracting with 25ml.
1.6 the investigation of linear relationshipTake by weighing acteoside reference substance 5.15mg, put in the 25ml measuring bottle, add methyl alcohol to scale, shake up, namely get (every 1ml contains acteoside 0.206mg).It is an amount of to get reference substance, adding respectively concentration is that 50% methyl alcohol is diluted to following concentration: 8.24mg/ml, 16.48mg/ml, 24.72mg/ml, 41.2mg/ml, 82.4mg/ml, 123.6mg/ml, draw respectively 10ml, in the injection liquid chromatography, measure the reference substance peak area by above-mentioned chromatographic condition, return processing with sample concentration and peak area, regression equation is: Y=13.85X-5.54 r=0.9998(n=6), acteoside reference substance sample concentration and peak area in 8.24mg/ml～206mg/ml scope are good linear relationship, the results are shown in Table 4.
Table 4 acteoside linear relationship measurement result
1.7 precision testDraw need testing solution 10ml, by above-mentioned chromatographic condition, repeat sample introduction 6 times, measure acteoside peak area value in the need testing solution, the relative standard deviation who calculates the test sample peak area value is 1.74%.The results are shown in Table 5.
Table 5 Precision test result
1.8 stability testDraw need testing solution 10ml, by above-mentioned chromatographic condition, every half an hour or 1 hour, measure acteoside peak area value in the need testing solution, the relative standard deviation who calculates test sample acteoside peak area value is 1.64%.The results are shown in Table 6.
Table 6 stability test result
1.9 reappearance testTake by weighing the about 0.7g of sample fine powder, totally 6 parts, the preparation method of shining described callicarpa nudiflora preparation need testing solution makes need testing solution, measures by above-mentioned chromatographic condition, and measurement result is processed through data, and RSD is 2.12%, the results are shown in Table 7.
Table 7 reproducible test results
1.10 average recovery testTake by weighing the about 0.35g of sample fine powder, totally 6 parts, put in the 50ml tool plug triangular flask, each adds acteoside reference substance solution (0.02552mg/ml) 25ml, after making by the preparation method of described callicarpa nudiflora preparation need testing solution, draw in the 10ml injection liquid chromatography and carry out assay, calculate recovery rate.The results are shown in Table 8.
Table 8 determination of recovery rates result
Average recovery rate 98.7% RSD=2.5%
1.11 sample determinationSample thief, porphyrize is got 0.7g, and is weighed, puts in the 50ml tool plug triangular flask, and adding concentration is 50% methyl alcohol 25ml, weighed weight, ultrasonic (power 250w, frequency 33kHz) processed 30 minutes, let cool, weighed weight again, adding concentration is the weight that 50% methyl alcohol is supplied minimizing.Shake up, filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Acteoside content in the callicarpa nudiflora particle of table 9
According to the result that table 9 is measured, consider the difference of the factors such as crude drug source, operating process, take 65% content limit as this product of above-mentioned average content, namely every bag in regulation sample contains callicarpa nudiflora with acteoside (C
29H
36O
15) meter, must not be less than 3.9mg.
Description of drawings
Fig. 1 is acteoside reference substance HPLC figure;
Fig. 2 is callicarpa nudiflora sample acteoside assay HPLC figure;
Fig. 3 is callicarpa nudiflora particle negative sample contrast HPLC figure.
Embodiment:
Embodiment one:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Yi Jing – 0.1% acetum (16:84) is mobile phase, and the detection wavelength is 332nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solutionGet 2 bags of callicarpa nudiflora particles, porphyrize is got 0.7g, and is weighed, puts in the 50ml tool plug triangular flask, adds 50% methyl alcohol 25ml, weighed weight, and ultrasonic (power 250w, frequency 33kHz) processed 30 minutes, let cool.Weighed weight adds the weight that 50% methyl alcohol is supplied minimizing again, shakes up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
Callicarpa nudiflora particle every bag (the 3g/ bag contains medicinal extract 0.8g) contains acteoside (C
29H
36O
15), must not be less than 3.9mg.
Embodiment two:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Jia Chun – 0.1% acetum (18:82) is mobile phase, and the detection wavelength is 322nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solutionGet 2 bags of callicarpa nudiflora particles, porphyrize is got 0.8g, and is weighed, puts in the 50ml tool plug triangular flask, adds 30% methyl alcohol 50ml, weighed weight, and ultrasonic (power 250w, frequency 33kHz) processed 45 minutes, let cool.Weighed weight adds the weight that 30% methyl alcohol is supplied minimizing again, shakes up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
Callicarpa nudiflora particle every bag (the 3g/ bag contains medicinal extract 0.8g) contains acteoside (C
29H
36O
15), must not be less than 3.9mg.
Embodiment three:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Yi Jing – 0.3% phosphoric acid solution (10:90) is mobile phase, and the detection wavelength is 345nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solutionGet callicarpa nudiflora 10, porphyrize is got 0.5g, and is weighed, puts in the 50ml tool plug triangular flask, adds 100% methyl alcohol 15ml, weighed weight, and ultrasonic (power 250w, frequency 33kHz) processed 15 minutes, let cool.Weighed weight adds the weight that 100% methyl alcohol is supplied minimizing again, shakes up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
Callicarpa nudiflora every (the 0.5g/ sheet contains medicinal extract 0.2g) contains acteoside (C
29H
36O
15), must not be less than 1.0mg.
Embodiment four:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Yi Jing – phosphoric acid solution (30:70) is mobile phase, and the detection wavelength is 332nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solution Get 10 of callicarpa nudiflora capsules, porphyrize is got 0.3g, and is weighed, puts in the 50ml tool plug triangular flask, adds 50% methyl alcohol 25ml, weighed weight, and ultrasonic (power 250w, frequency 33kHz) processed 30 minutes, let cool.Weighed weight adds the weight that 50% methyl alcohol is supplied minimizing again, shakes up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
Callicarpa nudiflora capsule every (the 0.3g/ grain contains medicinal extract 0.2g) contains acteoside (C
29H
36O
15), must not be less than 1.0mg.
Embodiment five:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Yi Jing – 0.1% acetum (18:82) is mobile phase, and the detection wavelength is 332nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solutionGet capsule (containing soft capsule) or tablet (containing dispersing tablet); porphyrize; get the weight that is equivalent to 1 or 1 (every contains dry extract 0.5g person, gets 0.5), weighed; put in the 50ml tool plug triangular flask; add 50% methyl alcohol 25ml, weighed weight, ultrasonic (power 250w; frequency 33kHz) processed 30 minutes, let cool.Weighed weight adds the weight that 50% methyl alcohol is supplied minimizing again, shakes up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
Every or every in callicarpa nudiflora capsule or tablet (containing dispersing tablet) contain dry extract 0.2g person, and every or every contains acteoside (C
29H
36O
15), must not be less than 0.8mg; Every contains dry extract 0.5g person, and every contains acteoside (C
29H
36O
15), must not be less than 2.0mg.
Embodiment six:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Yi Jing – 0.1% acetum (18:82) is mobile phase, and the detection wavelength is 332nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solutionGet suppository, chopping, mixing are got the weight that is equivalent to 1 suppository, and be weighed, puts in the 50ml tool plug triangular flask, adds 50% methyl alcohol 25ml, weighed weight, and ultrasonic (power 250w, frequency 33kHz) processed 30 minutes, let cool.Weighed weight adds the weight that 50% methyl alcohol is supplied minimizing again, shakes up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
Every of callicarpa nudiflora suppository contains acteoside (C
29H
36O
15), must not be less than 0.8mg.
Embodiment seven:
The assay method of acteoside content in the callicarpa nudiflora preparation adopts the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring.
Chromatographic condition and system suitabilityBe filling agent with octadecylsilane chemically bonded silica, Yi Jing – 0.1% acetum (18:82) is mobile phase, and the detection wavelength is 332nm, and number of theoretical plate calculates by the acteoside peak should be not less than 4000.
The preparation of reference substance solutionIt is an amount of to get the acteoside reference substance, weighed, adds 50% methyl alcohol and makes the solution that every 1ml contains 40mg, and get final product.
The preparation of need testing solutionGet mixture, the accurate 3ml that draws puts in the 25ml measuring bottle, adds methyl alcohol to nearly scale, and ultrasonic (power 250w, frequency 33kHz) processed 30 minutes, let cool.Add methyl alcohol to scale, shake up.Filter, get subsequent filtrate and filter with miillpore filter (0.45 μ m), get subsequent filtrate, and get final product.
Determination methodDraw respectively reference substance solution, each 10 μ l of need testing solution, the injection liquid chromatography is measured, and be get final product.
The every ml of callicarpa nudiflora mixture contains acteoside (C
29H
36O
15), must not be less than 0.5mg.
Claims (3)
1. the assay method of acteoside content in the callicarpa nudiflora preparation, adopt the acteoside content in the callicarpa nudiflora preparation need testing solution of high effective liquid chromatography for measuring, it is characterized in that: chromatographic condition and system suitability are: be that filling agent Yi Jing – acetum is mobile phase with octadecylsilane chemically bonded silica, the percentage by weight of acetonitrile is 16% in the mobile phase, the percentage by weight of acetum is 84%, and the concentration of acetum is 0.1%, and the detection wavelength is 332nm.
2. the assay method of acteoside content in the callicarpa nudiflora preparation according to claim 1, it is characterized in that: the preparation method of described callicarpa nudiflora preparation need testing solution is: get callicarpa nudiflora preparation, be equivalent to callicarpa nudiflora medicinal extract 0.05-1.5g, weighed, put in the tool plug triangular flask, adding concentration is 30-100% methyl alcohol 15-50ml, weighed weight, and ultrasonic processing is 15-45 minute under power 250w and frequency 33kHz, let cool, weighed weight again, adding concentration is the weight that 30-100% methyl alcohol is supplied minimizing, shakes up, filter, get subsequent filtrate and again filter with the miillpore filter of 0.45 μ m, get subsequent filtrate, and get final product.
3. the assay method of acteoside content in the callicarpa nudiflora preparation according to claim 1, it is characterized in that: the more excellent preparation method of described callicarpa nudiflora particle need testing solution is: get 2 bags of callicarpa nudiflora particles, porphyrize, get 0.7g, be equivalent to callicarpa nudiflora medicinal extract 0.187g, weighed, put in the tool plug triangular flask, adding concentration is 50% methyl alcohol 25ml, weighed weight, and ultrasonic processing is 30 minutes under power 250w and frequency 33kHz, let cool, weighed weight again, adding concentration is the weight that 50% methyl alcohol is supplied minimizing, shakes up, filter, get subsequent filtrate with the miillpore filter filtration of 0.45 μ m, get subsequent filtrate, and get final product.
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| CN106038828A (en) * | 2016-06-10 | 2016-10-26 | 普正药业股份有限公司 | Callicarpa nudiflora extract containing rich verbascoside and preparation method of callicarpa nudiflora extract |
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| CN104215698A (en) * | 2013-05-31 | 2014-12-17 | 九芝堂股份有限公司 | Callicarpa nudiflora medicine, intermediate and fingerprint detection method and standard fingerprint of preparation |
| CN104597139A (en) * | 2013-10-30 | 2015-05-06 | 九芝堂股份有限公司 | Method for simultaneously determining three kinds of phenylethanoid glycoside compositions in callicarpa nudiflora preparation through HPLC |
| CN104597139B (en) * | 2013-10-30 | 2017-05-17 | 九芝堂股份有限公司 | Method for simultaneously determining three kinds of phenylethanoid glycoside compositions in callicarpa nudiflora preparation through HPLC |
| WO2021109704A1 (en) * | 2019-12-06 | 2021-06-10 | 罗胥恩 | Chronic wound healing composition and application thereof |
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