CN102836190A - Preparation method and quality control method for schefflera kwangsiensis general flavone extract - Google Patents
Preparation method and quality control method for schefflera kwangsiensis general flavone extract Download PDFInfo
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- CN102836190A CN102836190A CN2012103608310A CN201210360831A CN102836190A CN 102836190 A CN102836190 A CN 102836190A CN 2012103608310 A CN2012103608310 A CN 2012103608310A CN 201210360831 A CN201210360831 A CN 201210360831A CN 102836190 A CN102836190 A CN 102836190A
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Abstract
The invention discloses a preparation method and a quality control method for schefflera kwangsiensis general flavone extract. The preparation technology for the extract comprises the steps as follows: soaking a schefflera kwangsiensis medicinal material for 0.5 h by adding 8 to 10 times of ethanol by weight, wherein the volume concentration of the ethanol is from 60% to 80%; refluxing and extracting for 2 to 3 times with each time of 1 to 3 h; filtering and mixing filtrate; and decompressing and concentrating the filtrate at the temperature of 75 to 85 DEG.C to the temperature of 60 DEG.C, so as to obtain the extract with relative density of 1.10 to 1.30. The product quality control method mainly adopts a high performance liquid chromatography to detect the content of rutin. The preparation technology provided by the invention has the advantages of stable process parameter, process condition and process technology, high rutin extracting yield and strong industrial applicability. The quality control method provided by the invention has the advantages of high degree of separation, good linear relation, convenience, rapidness, accuracy and stability. Therefore, the quality control method meets the requirements of industrial production, and effectively controls the quality of the schefflera kwangsiensis general flavone extract and a preparation thereof.
Description
Technical field
The present invention relates to a kind of method for preparing and product quality control method of Radix Schefflerae Arboricolae total flavonoids extract.
Background technology
Radix Schefflerae Arboricolae is tender stem and the leaf of Araliaceae schefflera platymiscium Radix Schfflerae kwangisensis (Schefflera kwangsiensis Merr.Ex L).Be distributed widely in areass to the south, the Changjiang river such as Guangxi, Guangdong, Fujian, Radix Schefflerae Arboricolae main chemical compositions and effective ingredient are total flavones, mainly contain Quercetin, rutin etc.Rapid-action, the persistent of oral formulations such as the tablet of processing with this total flavonoids extract, capsule, drop pill, granulation machine.
Radix Schefflerae Arboricolae sheet NF standard (2010 editions one one) has been put down in writing the preparation and the content assaying method of this total flavonoids extract; But this method for preparing technological parameter, process conditions and Technology are unreasonable; Extract yield is low; Its content assaying method adopts ultraviolet visible spectrophotometry to measure content of total flavone, and complex operation, poor stability, error are big.Therefore, existing preparation of Radix Schefflerae Arboricolae sheet and content control method can not adapt to the commercial production demand well, and product quality is difficult to be effectively controlled.
Summary of the invention
For solving the deficiency of above-mentioned prior art, the invention provides a kind of preparation and product quality control method of Radix Schefflerae Arboricolae total flavonoids extract, short to realize preparation time, extract yield is high; And the employing HPLC is easy, measure content of total flavone quickly and accurately.
The present invention solves the problems of the technologies described above with following technical scheme:
The method for preparing of Radix Schefflerae Arboricolae total flavonoids extract of the present invention, its operational approach is following:
Got volumetric concentration that the Radix Schefflerae Arboricolae medical material adds 8 ~ 10 times of weight and be 60% ~ 80% soak with ethanol 0.5 hour, reflux, extract, 2 ~ 3 times, each 1 ~ 3 hour; Filter; Merging filtrate, relative density is 1.10 ~ 1.30 extractum when under 75～85 ℃, being evaporated to 60 ℃, promptly gets.
The method of quality control of Radix Schefflerae Arboricolae total flavonoids extract of the present invention, its operational approach is following:
Chromatographic condition and system suitability: use octadecylsilane chemically bonded silica to be filler; With Jia Chun ︰ 0.4% phosphoric acid by volume=solution of 35:65 mixed preparing is mobile phase; The detection wavelength is 365nm.
The preparation of reference substance solution: it is an amount of to get anhydrous control substance of Rutin, and precision steelyard is fixed, adds methanol and processes the solution that 1ml contains anhydrous rutin 0.1mg, as reference substance solution;
The preparation of need testing solution: get Radix Schefflerae Arboricolae total flavonoids extract 50mg, precision steelyard is fixed, puts in the 25ml measuring bottle, and it is an amount of to add methanol; Supersound process (power 250W, frequency 33KHz) is diluted to the 25ml scale with methanol, shakes up; Filter, get this filtrating, as need testing solution.
Algoscopy: accurate respectively reference substance and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure according to HPLC (2010 editions one appendix VI D of Chinese Pharmacopoeia), promptly get.
Extract making method of the present invention has following advantage:
Preparation time is short, has shortened the production cycle; Extract yield is high, has reduced production cost; Ethanol is recyclable to be utilized again, has reduced energy waste.
The total flavonoid glycoside extractum that adopts the inventive method to process can be processed oral formulations such as tablet, capsule, drop pill, granulation machine.
The present invention adopts HPLC that the quality of Radix Schefflerae Arboricolae total flavonoids extract is controlled, and method is simple and efficient, accurately stable, can adapt to industrial needs, can control the quality of Radix Schefflerae Arboricolae total flavonoids extract and preparation thereof effectively.
The specific embodiment
Embodiment 1 (preparation of Radix Schefflerae Arboricolae total flavonoids extract):
Getting the volumetric concentration that the Radix Schefflerae Arboricolae medical material adds 8 times of weight is 60% soak with ethanol 0.5 hour, reflux, extract, 2 times, and each 2 hours, filter, merging filtrate, concentrating under reduced pressure (temperature is 85 ℃) to relative density is the extractum of 1.10 (60 ℃), promptly gets.
Embodiment 2 (preparation of Radix Schefflerae Arboricolae total flavonoids extract):
Getting the volumetric concentration that the Radix Schefflerae Arboricolae medical material adds 9 times of weight is 70% soak with ethanol 0.5 hour, reflux, extract, 2 times, 2.5 hours for the first time; 1.5 hours for the second time, filter merging filtrate; Concentrating under reduced pressure (temperature is 75 ℃) to relative density is the extractum of 1.10 (60 ℃), promptly gets.
Embodiment 3 (preparation of Radix Schefflerae Arboricolae total flavonoids extract):
Getting the volumetric concentration that the Radix Schefflerae Arboricolae medical material adds 9 times of weight is 60% soak with ethanol 0.5 hour, reflux, extract, 3 times, and each 2 hours, filter, merging filtrate, concentrating under reduced pressure (temperature is 80 ℃) to relative density is the extractum of 1.20 (60 ℃), promptly gets.
Embodiment 4 (preparation of Radix Schefflerae Arboricolae total flavonoids extract)
Getting the volumetric concentration that the Radix Schefflerae Arboricolae medical material adds 10 times of weight is 80% soak with ethanol 0.5 hour, reflux, extract, 2 times, 3 hours for the first time; 2 hours for the second time, filter merging filtrate; Concentrating under reduced pressure (temperature is 75 ℃) to relative density is the extractum of 1.30 (60 ℃), promptly gets.
Embodiment 5 (method of quality control of Radix Schefflerae Arboricolae total flavonoids extract):
Chromatographic condition and system suitability: use octadecylsilane chemically bonded silica to be filler; With Jia Chun ︰ 0.4% phosphoric acid by volume=solution of 35:65 mixed preparing is mobile phase; The detection wavelength is 365nm.(methanol is absolute methanol, and 0.4% phosphoric acid is volumetric concentration, 0.4V phosphoric acid, 99.6V water)
The preparation of reference substance solution: it is an amount of to get anhydrous control substance of Rutin, and precision steelyard is fixed, adds absolute methanol and processes the solution that 1ml contains anhydrous rutin 0.1mg, as reference substance solution.
The preparation of need testing solution: get Radix Schefflerae Arboricolae total flavonoids extract 50mg, precision steelyard is fixed, puts in the 25ml measuring bottle, and it is an amount of to add absolute methanol; Supersound process (power 250W, frequency 33KHz) is diluted to the 25ml scale with methanol, shakes up; Filter, get this filtrating, as need testing solution.
Algoscopy: accurate respectively reference substance and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph, measure according to HPLC (2010 editions appendix VID of Chinese Pharmacopoeia), promptly get.
Industrial applicibility is investigated
1, adopts the content of anhydrous rutin in the high effective liquid chromatography for measuring Radix Schefflerae Arboricolae total flavonoids extract according to the invention; Its result shows; Anhydrous rutin chromatographic peak area and solution concentration in 4.704～37.632 μ g/ml scopes are the good linear relation, and r is 0.9999; Separating degree is good, and theoretical cam curve is calculated as 3609 by anhydrous rutin peak; When signal to noise ratio was 2:1, sample minimum detectable concentration was 0.16 μ g/ml; It is stable in 10 hours to measure solution; It is 99.3% that anhydrous rutin content is measured average recovery rate, and RSD is 0.61%; Precision test RSD is 0.23%; Stability test RSD is 1.35%.
2, the foregoing description all adopts with a collection of Radix Schefflerae Arboricolae medical material; The content that detects the prepared anhydrous rutin of Radix Schefflerae Arboricolae total flavonoids extract of above embodiment 1 ~ embodiment 4 with HPLC of the present invention is respectively 5.62%, 6.37%, 5.83% and 5.96, and extract yield is respectively 72.3%, 83.6%, 75.2% and 76.8%.
In sum, method for preparing technological parameter, process conditions and the stable technology of Radix Schefflerae Arboricolae total flavonoids extract of the present invention, extract yield is high, and industrial applicibility is strong; The present invention controls the quality of Radix Schefflerae Arboricolae total flavonoids extract with HPLC, and this method is simple and efficient, accurately stable, can adapt to industrial needs, can control the quality of Radix Schefflerae Arboricolae total flavonoids extract and preparation thereof effectively.
Claims (2)
1. the method for preparing of a Radix Schefflerae Arboricolae total flavonoids extract is characterized in that, its operational approach is following:
Got volumetric concentration that the Radix Schefflerae Arboricolae medical material adds 8 ~ 10 times of weight and be 60% ~ 80% soak with ethanol 0.5 hour, reflux, extract, 2 ~ 3 times, each 1 ~ 3 hour; Filter; Merging filtrate, relative density is 1.10 ~ 1.30 extractum when under 75～85 ℃, being evaporated to 60 ℃, promptly gets.
2. the method for quality control of a Radix Schefflerae Arboricolae total flavonoids extract is characterized in that, its operational approach is following:
Chromatographic condition and system suitability: use octadecylsilane chemically bonded silica to be filler; With Jia Chun ︰ 0.4% phosphoric acid by volume=solution of 35:65 mixed preparing is mobile phase; The detection wavelength is 365nm;
The preparation of reference substance solution: it is an amount of to get anhydrous control substance of Rutin, and precision steelyard is fixed, adds methanol and processes the solution that 1ml contains anhydrous rutin 0.1mg, as reference substance solution;
The preparation of need testing solution: get Radix Schefflerae Arboricolae total flavonoids extract 50mg, precision steelyard is fixed, puts in the 25ml measuring bottle, and it is an amount of to add methanol, and supersound process is diluted to the 25ml scale with methanol, shakes up, and filters, and gets this filtrating, as need testing solution.
Algoscopy: accurate respectively reference substance and each 20 μ l of need testing solution of drawing, inject high performance liquid chromatograph, according to high effective liquid chromatography for measuring, promptly get.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083277A (en) * | 2017-12-29 | 2018-05-29 | 凤台县鼎足农业发展有限公司 | A kind of reutilization technology of Pleurotus eryngii mushroom bran |
| CN110279735A (en) * | 2019-08-09 | 2019-09-27 | 金鸿药业股份有限公司 | A kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component and preparation method thereof |
Citations (1)
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| CN1454631A (en) * | 2003-01-24 | 2003-11-12 | 贵州三力制药有限责任公司 | Schefflera (Hantaoye) soft capsule and preparing method thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1454631A (en) * | 2003-01-24 | 2003-11-12 | 贵州三力制药有限责任公司 | Schefflera (Hantaoye) soft capsule and preparing method thereof |
Non-Patent Citations (1)
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| 刘娴，等: "《汉桃叶抗炎镇痛作用有效部位的筛选》", 《安徽医药》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108083277A (en) * | 2017-12-29 | 2018-05-29 | 凤台县鼎足农业发展有限公司 | A kind of reutilization technology of Pleurotus eryngii mushroom bran |
| CN110279735A (en) * | 2019-08-09 | 2019-09-27 | 金鸿药业股份有限公司 | A kind of CAULIS SCHEFFLERAE KWANGSIENSIS active component and preparation method thereof |
| CN110279735B (en) * | 2019-08-09 | 2021-07-09 | 金鸿药业股份有限公司 | Effective part of Chinese walnut leaf and preparation method thereof |
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Application publication date: 20121226 |