CN1361423A - Identification and test method of antilipemic medicine giant knotwood tablet - Google Patents
Identification and test method of antilipemic medicine giant knotwood tablet Download PDFInfo
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- CN1361423A CN1361423A CN 00120628 CN00120628A CN1361423A CN 1361423 A CN1361423 A CN 1361423A CN 00120628 CN00120628 CN 00120628 CN 00120628 A CN00120628 A CN 00120628A CN 1361423 A CN1361423 A CN 1361423A
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Abstract
The identification and test method of antilipemic medicine giant knotwood tablet includes the steps of: crushing coating-less tested medicine tablet, chloroform water bath heating reflux extraction in a Soxhlet extractor until on chloroform yellow, separating chloroform extractive liquid; further reflux extraction of the residue with 95% concentration ethanol water bath in a Soxhlet extractor for 3 hr, concentrating ethanol extractive liquid and constant volume diluting with ethanol, measuring the absorbance of the chloroform extractive liquid and the ethanol constant volume diluted liquid at 520 nm and 306 nm separately by means of spectrophotometric process; and comparing with the standard absorbance of emodin and veratryl alcohol glycoside to obtain corresponding contents.
Description
What the present invention relates to is discriminating detection method to hypolipemic giant knotweed rhizome tablet, specifically is by the archen in the giant knotweed rhizome tablet and resveratrol salidroside content are detected the method for discriminating with spectrophotometric method.
Giant knotweed rhizome tablet is to be prepared from by the giant knotweed extract powder, is used to the medicine that hyperlipemia is treated because of having reduction cholesterol and triglyceride function.Present detection to its effective ingredient, what adopt is after adding ethyl acetate and shake with the water liquid behind the chloroform extraction, the blue-fluorescence that its ethyl acetate extract is shown under ultraviolet lamp with extracted by ether and with the ethanolic solution behind the dissolve with ethanol again is with colourimetry respectively, and adds in above-mentioned water layer that chromogenic reaction behind the ferric trichloride carries out.From the methodology angle, the specificity of colourimetry and development process and sensitivity are all lower, and are subject to the interference of other composition of external environment and existence, and particularly when detection by quantitative was differentiated, the situation of its sum of errors mistake was difficult to avoid especially.
Given this, the objective of the invention is to provide a kind of detection to differentiate the more desirable method aspect specificity and accuracy when particularly carrying out the detection by quantitative discriminating to hypolipemic giant knotweed rhizome tablet for addressing the above problem.
The said discriminating detection method of the present invention to hypolipemic giant knotweed rhizome tablet, be after the giant knotweed tablet to be measured of no sugar-coat is pulverized, put in the cable type extractor according, end when under the water-bath reflux, being extracted into chloroform and not having yellow with chloroform, separate the chloroform extracted solution usefulness of purchasing in addition, residue after the extraction is at least 95% ethanol with content to be continued to reflux 3 hours with cable type extractor according water-bath heating, ethanol extract is concentrated into 100 milliliters to dilute with 95% ethanol constant volume after interior, differentiates detection by following operation respectively with spectrophotometric method then:
(1) precision is measured different volumes but is derived from the archen chloroform that is become with the chloroform preparation with the archen once precision weighing and contrasts with two parts of solution, and the medicine chloroform extracted solution to be measured of the above-mentioned usefulness of purchasing in addition, eliminate chloroform respectively, each residue adds respectively after 2% ammonia solution and 5% (being weight %) sodium hydroxide solution by the preparation of the precision of equivalent mixes the solution dissolving that become, with this mixed solution is blank, measure its absorbance log respectively at 520 nano wave length places, with two reference substances is reference, calculates the emodin content in the medicine to be measured;
(2) piceid of the contrast usefulness of precision weighing is mixed with the reference substance test solution with known content gradient with 95% ethanol constant volume after, make its standard absorption line of writing music with 95% alcohol solvent as blank at 306 nano wave length places, be under the condition of blank with the solvent with above-mentioned drug solution to be measured after the dilution of 95% ethanol constant volume then, measure it after the absorbance log at 306 nano wave length places, by this standard absorption line its content that converts of writing music.
In said method, during said preparation archen reference substance, can make precision weighing and the reference substance solution that is mixed with chloroform in emodin content be 100 mcg/ml; Take from the also accurate two parts of different volumes reference substance solution of measuring of this same reference substance solution and can be respectively 2 milliliters and 3 milliliters.During detection, said giant knotweed rhizome tablet drug dose to be measured generally can be for by 20, and taken by weighing 300 milligrams by it by precision in the medicine after pulverizing and place cable type extractor according, with 130 milliliters of chloroform extraction.Precision is measured and is detected after 10 milliliters of these extracts are handled by said method again, and the consumption by the equivalent 2% ammonia solution solution that mixing is become with 5% NaOH used when wherein dissolving is 20 milliliters.
The consumption of the piceid of the said usefulness of product in contrast generally can be 10 milligrams in the said method, after being settled to 50 milliliters with 95% ethanol, after precision is measured respectively by the gradient of 0.5 milliliter, 1.0 milliliters, 2.0 milliliters, 3.0 milliliters, 4.0 milliliters, 5.0 milliliters, 6.0 milliliters and 7.0 milliliters again, be diluted to 50 milliliters with the equal separately constant volume of 95% ethanol respectively again, be used for measuring and production standard absorbance log curve.When 20 used amount of drug to be measured match during with above-mentioned detection archen, residue behind its chloroform extraction is used alcohol extract again, this ethanol extract concentrates and available 95% ethanol constant volume is diluted to 100 milliliters, measure 1 milliliter and 2 milliliters of this drug solution to be measured then, after being diluted to 25 milliliters with 95% ethanol constant volume again, measure its absorbance log at 306 nano wave length places by said method.
Be appreciated that thus, said method of the present invention is by adopting spectrophotometer, archen in the giant knotweed rhizome tablet medicine and piceid are determined as foundation at the characteristic ultraviolet absorptivity of certain wave strong point, and by converting and realize with the absorbance log of corresponding reference substance or by the standard absorption that it the is depicted as line of writing music.Test findings shows, the inventive method and the aforesaid detection of carrying out with colourimetry and development process are at present differentiated, can realize similar detection discriminating purpose, but detect on the effect that its specificity, specificity and the each side such as accuracy that detect thereof all greatly improve.Particularly when the detection of carrying out quantitative property was differentiated, it detects the result who differentiates can more infallible assurance.
Below by specific embodiment foregoing of the present invention is described in further detail, but this should be interpreted as that the scope of the above-mentioned theme of the present invention is confined to following example.
20 in giant knotweed tablet after getting no sugar-coat to be detected or divesting sugar-coat, porphyrize, precision takes by weighing 300 milligrams and puts in the cable type extractor according, with 130 milliliters of chloroforms, under the water-bath reflux, be extracted into chloroform and do not end (about 3 hours) during displaing yellow, separate the chloroform extracted solution usefulness of purchasing in addition, as for detecting the test solution A to be detected that archen is used.Residue behind the chloroform extraction is with 130 milliliters of 95% ethanol or absolute ethyl alcohols, puts to bathe heating in the cable type extractor according again and continue down to reflux about 3 hours.Ethanol extract evaporation and concentration to 100 milliliter with after interior, is diluted to 100 milliliters with 95% ethanol constant volume, as measuring the test solution B to be detected that piceid is used.
Precision takes by weighing 10 milligrams of archen reference substances, is settled to 100 milliliters with chloroform, becomes the reference substance solution that emodin content is 100 mcg/ml.Precision is measured 2 milliliters of this reference substance solution and 3 milliliters of each portions respectively, and accurate test solution A10 milliliter above-mentioned to be detected of measuring, and eliminates its chloroform respectively, each part residue
After respectively accurate separately 2% ammonia solution and 5% (the being weight %) sodium hydroxide solution that adds by equivalent mixes the solution dissolving that become, with this mixed solution is blank, measure its absorbance log respectively at 520 nano wave length places, and be reference with two reference substances, calculate the emodin content in the medicine to be measured;
10 milligrams of the piceids of precision weighing contrast usefulness, after being mixed with 50 milliliters with 95% ethanol constant volume, precision is measured 0.5 milliliter, 1.0 milliliters, 2.0 milliliters, 3.0 milliliters, 4.0 milliliters, 5.0 milliliters, 6.0 milliliters and 7.0 milliliters respectively, be diluted to 50 milliliters with 95% ethanol constant volume again, reference substance test fluid as the known content gradient, make blank with 95% alcohol solvent, make its standard absorption line of writing music at 306 nano wave length places.Measure 1 milliliter or 2 milliliters of above-mentioned test solution B to be detected, be diluted to 25 milliliters with 95% ethanol constant volume after, be blank with the solvent, measure the absorbance log at its 306 nano wave length place, by above-mentioned contrast with the standard absorption of piceid line its content that converts of writing music.
Claims (5)
1. the discriminating detection method of hypolipemic giant knotweed rhizome tablet, after it is characterized in that giant knotweed tablet pulverizing to be measured with no sugar-coat, put in the cable type extractor according, end when under the water-bath reflux, being extracted into chloroform and not having yellow with chloroform, separate the chloroform extracted solution usefulness of purchasing in addition, residue after the extraction is at least 95% ethanol with content to be continued to reflux 3 hours with cable type extractor according water-bath heating, ethanol extract is concentrated into 100 milliliters with after interior, with the dilution of 95% ethanol constant volume, differentiate detection by following operation respectively with spectrophotometric method then:
(1) precision is measured different volumes but is derived from the archen chloroform that is become with the chloroform preparation with the archen once precision weighing and contrasts with two parts of solution, and the medicine chloroform extracted solution to be measured of the above-mentioned usefulness of purchasing in addition, eliminate chloroform respectively, after adding the 2% ammonia solution solution dissolving that mixing is become with 5% sodium hydroxide solution of preparing in each residue respectively by the precision of equivalent, with this mixed solution is blank, measure its absorbance log respectively at 520 nano wave length places, with two reference substances is reference, calculates the emodin content in the giant knotweed rhizome tablet medicine to be measured;
(2) contrast of precision weighing is mixed with the reference substance test solution with known content gradient with piceid with 95% ethanol constant volume after, make its standard absorption line of writing music with 95% alcohol solvent as blank at 306 nano wave length places, be under the condition of blank with the solvent with above-mentioned drug solution to be measured after the dilution of 95% ethanol constant volume then, measure it after the absorbance log at 306 nano wave length places, by this standard absorption line its content that converts of writing music.
2. the discriminating detection method of hypolipemic giant knotweed rhizome tablet as claimed in claim 1, emodin content in the archen chloroformic solution reference substance that it is characterized in that said precision weighing and become with chloroform preparation is 100 mcg/ml, takes from two parts of different volumes reference substances that this reference substance solution precision measures and is respectively 2 milliliters and 3 milliliters.
3. the discriminating detection method of hypolipemic giant knotweed rhizome tablet as claimed in claim 1 or 2, it is characterized in that said giant knotweed rhizome tablet amount of drug to be measured is for being taken by weighing 300 milligrams by 20 by precision in the medicine after pulverizing, put in the cable type extractor according with 130 milliliters of chloroform extraction, precision is measured and is detected after 10 milliliters of these extracts are handled by said method, and the consumption by the equivalent 2% ammonia solution solution that mixing is become with 5% NaOH used when wherein dissolving is 20 milliliters.
4. the discriminating detection method of hypolipemic giant knotweed rhizome tablet as claimed in claim 1, the consumption that it is characterized in that the piceid of said contrast usefulness is 10 milligrams, after being dissolved as 50 milliliters with 95% ethanol constant volume, by the gradient of 0.5 milliliter, 1.0 milliliters, 2.0 milliliters, 3.0 milliliters, 4.0 milliliters, 5.0 milliliters, 6.0 milliliters and 7.0 milliliters respectively precision measure, and after being diluted to 50 milliliters with 95% ethanol constant volume more respectively, be used for measuring and production standard absorbance log curve.
5. the discriminating detection method of hypolipemic giant knotweed rhizome tablet as claimed in claim 4, it is characterized in that said drug dose to be measured is 20, the concentrated back of its ethanol extract is 100 milliliters with the constant volume of the drug solution body to be measured of 95% ethanol dilution, measure 1 milliliter or 2 milliliters of the constant volume solution of this medicine to be measured, after being diluted to 25 milliliters with 95% ethanol constant volume again, measure its absorbance log at 306 nano wave length places by said method.
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| CN 00120628 CN1361423A (en) | 2000-12-26 | 2000-12-26 | Identification and test method of antilipemic medicine giant knotwood tablet |
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| CN 00120628 CN1361423A (en) | 2000-12-26 | 2000-12-26 | Identification and test method of antilipemic medicine giant knotwood tablet |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102596211B (en) * | 2009-12-29 | 2015-06-24 | 韩国韩医学研究院 | Compositions and functional foods for treating and preventing obesity using polygonum cuspidatum butanol fraction and ethyl acetate fraction |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102596211B (en) * | 2009-12-29 | 2015-06-24 | 韩国韩医学研究院 | Compositions and functional foods for treating and preventing obesity using polygonum cuspidatum butanol fraction and ethyl acetate fraction |
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