CN101524458B - Extract of smilax glabra saponins and flavonoid and preparation method thereof - Google Patents
Extract of smilax glabra saponins and flavonoid and preparation method thereof Download PDFInfo
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- CN101524458B CN101524458B CN2009100432362A CN200910043236A CN101524458B CN 101524458 B CN101524458 B CN 101524458B CN 2009100432362 A CN2009100432362 A CN 2009100432362A CN 200910043236 A CN200910043236 A CN 200910043236A CN 101524458 B CN101524458 B CN 101524458B
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Abstract
The invention discloses an extract of smilax glabra saponins and flavonoid and a preparation method thereof. The preparation method comprises the steps of (1) smilax glabra medical materials are dried in vacuum, crushed and hydrolyzed by enzyme; and (2) smilax glabra saponins and flavonoid compound are extracted with ethanol under the auxiliary function of ultrasonic in inverse flow and condensed; the condensed compound is degreased with petroleum ether and extracted with chloroform and ethyl acetate; after the solvent is recovered, the solvent is dried in vacuum to obtain the extract of smilax glabra saponins and flavonoid which contains 30-80 percent of flavonoid compound. The obtained smilax glabra saponins extract contains 20-70 percent of saponins compound. The method utilizes composite plant extracting enzyme to pretreat the smilax glabra medical materials and extract the smilax glabra saponins and flavonoid compound with ultrasonic auxiliary extract technology, has high utilization degree of the medical materials and high yield of product, consumes low energy and is convenient to operate. The extract of smilax glabra saponins and flavonoid is widely applied to the field of medical materials, midbody and health-care food and has wide market foreground.
Description
Technical field
The present invention relates to a kind of method for preparing of Chinese medicine extract, specifically refer to from Rhizoma Smilacis Glabrae, extract the method for preparing of Saponin and flavone compound.
Background technology
Rhizoma Smilacis Glabrae is the dry rhizome of liliaceous plant smilacis glabra Smilax glbra Roxb.; But the Rhizoma Smilacis Glabrae of indication of the present invention also comprises the hargil Poria, and promptly the dry rhizome of Xiao Rhizoma Smilacis Chinensis is a kind of Chinese herbal medicine commonly used; Ground such as be distributed on the south the Yangtze river basin, sweet in the mouth, property are flat.Rhizoma Smilacis Glabrae and extract thereof have dehumidifying, detoxifcation, and effects such as easing joint movement are mainly used in damp and hot pouring worm, carbuncle, limbs contracture, bones and muscles pain due to scabies and the mercurialism.
The main effective ingredient of Rhizoma Smilacis Glabrae and extract thereof is Saponin and flavone compound; Therefore, the extractive technique of exploitation smilax glabra saponins and flavone compound is for the availability that improves the Rhizoma Smilacis Glabrae raw medicinal herbs; Developing Rhizoma Smilacis Glabrae extract market promotes that modernization of industry of Chinese materia medica is significant.
Aspect Rhizoma Smilacis Glabrae extract; The paper of " plant research " 2006 26 the 3rd phases of volume " extracting the technical study of total flavones in the Rhizoma Smilacis Glabrae " discloses a kind of method of from Rhizoma Smilacis Glabrae, extracting total flavones; But this literary composition research level is more shallow; Only the influence of factor pair extraction ratios such as temperature, concentration of alcohol is inquired into, and yield is not high yet; Patent (" Rhizoma Smilacis Glabrae total glycosides extract " application number: 200510095149.3) disclose a kind of Rhizoma Smilacis Glabrae total glycosides extract; But this method is only studied total glycosides extractive; Yield is lower, can't adapt to the requirement of industrialization of Chinese medicine." the macroporous adsorbent resin separation and purification Rhizoma Smilacis Glabrae total flavones " that " research of enriching and purifying macroporous resin Rhizoma Smilacis Glabrae total flavones " and " CHINA JOURNAL OF CHINESE MATERIA MEDICA " of " pharmacy today " 2008 18 3 phases of volume rolled up for 10 phases in 2008 33 disclose respectively a kind of from the Rhizoma Smilacis Glabrae alcohol extract method of separation and purification total flavones; But these two kinds of methods all exist cost high, the problem that can't produce in enormous quantities.
On the other hand, enzyme preparation has been applied to the plant extract and the field of Chinese medicines (like Semen Ginkgo, Radix Ginseng etc.), aspect industrialization of Chinese medicine, has brought into play important function, but uses the single enzyme preparation mostly, and effect is also not fully up to expectations.
Summary of the invention
For solving the problem that the above-mentioned prior art of from Rhizoma Smilacis Glabrae, extracting Saponin and flavone compound exists; The inventor is through a large amount of production practices, invents out a kind of availability that improves raw medicinal material, low energy consumption is low-cost, easy and simple to handle and yield the is high production method of from Rhizoma Smilacis Glabrae, extracting Saponin and flavone compound simultaneously finally.
The present invention includes following step:
(1) processing of raw medicinal material comprises raw medicinal material is carried out vacuum drying, pulverizing and enzymolysis.With raw medicinal material vacuum drying to moisture is 5%-10%, and baking temperature 50-80 degree is crushed to the 10-20 order, adds enzymolysis solution that 3-12 doubly measures then under the temperature of 35-55 degree enzymolysis 3-10 hour.The enzymolysis solution method for preparing is: 1-15 is restrained plant extract enzyme (enzyme is lived and is 10000-30000 unit) be dissolved in the 500mlpH value for promptly getting in the buffer of 4-7.Plant extract enzyme wherein consists of cellulase content 30-50%, pectase content is 20-40%, protease content 5-20%, xylanase 5-25%.With the extraction ratio that can improve Saponin and flavone compound after the enzyme processing.
(2) extraction of smilax glabra saponins and flavone compound.With 5-12 doubly to Rhizoma Smilacis Glabrae weight; Concentration is that the ethanol of 60-95% carried out reflux, extract, 2.5-6 hour, and triplicate, merge extractive liquid, are condensed into paste; With combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
The Rhizoma Smilacis Glabrae flavone extract that utilizes the present invention to obtain wherein contains flavone compound 30-80%; The smilax glabra saponins extract that obtains wherein contains oside compound 20-70%, all by extract weight.Flavonoid and Saponin class extract are widely used in crude drug, intermediate and field of health care food, and market prospect is wide.
Method for preparing of the present invention is that compound enzymic preparation is applied to the Rhizoma Smilacis Glabrae extract field; Be equipped with ultrasound wave auxiliary extraction technology again,, not only improved the availability of raw medicinal material than existing direct extractive technique; Also improved the yield (more conventional extraction method improves 10-40%) of Saponin and flavone compound; Have the advantages that energy consumption is low, extraction conditions is gentle, also improved operability simultaneously greatly, the extracting solution after handling with enzyme has the characteristics of easy filtration; Reduce energy consumption, provided cost savings, guaranteed the better quality of extract.
The specific embodiment
Below the concrete method for preparing of smilax glabra saponins, flavone extract is elaborated.
Embodiment 1:
1, be 5.5% with Rhizoma Smilacis Glabrae raw medicinal material vacuum drying to moisture, baking temperature 50 degree is crushed to 10 orders, the enzymolysis solution that adds 3 times of amounts enzymolysis 9.5 hours under the temperature of 35 degree.The enzymolysis solution method for preparing is: it is 4.2 buffer that 1.5 gram plant extract enzymes (enzyme work is 19000 units) are dissolved in the 500mlpH value.Plant extract enzyme wherein consists of that cellulase content 30%, pectase content are 40%, protease content 10%, xylanase 20%.
2, with 5 times to Rhizoma Smilacis Glabrae weight, concentration is that 60% ethanol carried out reflux, extract, 3 hours, triplicate, merge extractive liquid, are condensed into paste, with combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
Rhizoma Smilacis Glabrae flavone extract through above-mentioned processing obtains contains flavone compound 34% by extract weight; The smilax glabra saponins extract that obtains contains oside compound 41% by extract weight.
Embodiment 2
1, be 7% with Rhizoma Smilacis Glabrae raw medicinal material vacuum drying to moisture, baking temperature 55 degree is crushed to 18 orders, the enzymolysis solution that adds 8 times of amounts enzymolysis 4.5 hours under the temperature of 45 degree.The enzymolysis solution method for preparing is: it is 5.0 buffer that 8 gram plant extract enzymes (enzyme work is 21000 units) are dissolved in the 500mlpH value.Plant extract enzyme wherein consists of that cellulase content 47%, pectase content are 21%, protease content 8%, xylanase 24%.
2, with 8 times to Rhizoma Smilacis Glabrae weight, concentration is that 85% ethanol carried out reflux, extract, 2.5 hours, triplicate, merge extractive liquid, are condensed into paste, with combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
Rhizoma Smilacis Glabrae flavone extract through above-mentioned processing obtains contains flavone compound 40% by extract weight; The smilax glabra saponins extract that obtains contains oside compound 36% by extract weight.
Embodiment 3
1, be 9% with Rhizoma Smilacis Glabrae raw medicinal material vacuum drying to moisture, baking temperature 65 degree is crushed to 11 orders, the enzymolysis solution that adds 10 times of amounts enzymolysis 5 hours under the temperature of 48 degree.The enzymolysis solution method for preparing is: it is 7 buffer that 3 gram plant extract enzymes (enzyme work is 30000 units) are dissolved in the 500mlpH value.Plant extract enzyme wherein consists of that cellulase content 48%, pectase content are 25%, protease content 17%, xylanase 10%.
2, with 5 times to Rhizoma Smilacis Glabrae weight; Concentration is that 78% ethanol carried out reflux, extract, 3.6 hours under ultrasound wave is auxiliary, and triplicate, merge extractive liquid, are condensed into paste; With combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
Rhizoma Smilacis Glabrae flavone extract through above-mentioned processing obtains contains flavone compound 51% by extract weight; The smilax glabra saponins extract that obtains contains oside compound 47% by extract weight.
Embodiment 4
1, be 7.5% with Rhizoma Smilacis Glabrae raw medicinal material vacuum drying to moisture, baking temperature 79 degree is crushed to 20 orders, the enzymolysis solution that adds 9 times of amounts enzymolysis 3 hours under the temperature of 50 degree.The enzymolysis solution method for preparing is: it is 6.6 buffer that 14 gram plant extract enzymes (enzyme work is 15000 units) are dissolved in the 500mlpH value.Plant extract enzyme wherein consists of that cellulase content 39%, pectase content are 37%, protease content 16%, xylanase 8%.
2, with 11 times to Rhizoma Smilacis Glabrae weight; Concentration is that 72% ethanol carried out reflux, extract, 4.1 hours under ultrasound wave is auxiliary, and triplicate, merge extractive liquid, are condensed into paste; With combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
Rhizoma Smilacis Glabrae flavone extract through above-mentioned processing obtains contains flavone compound 60% by extract weight; The smilax glabra saponins extract that obtains contains oside compound 54% by extract weight.
Embodiment 5
1, be 9.5% with Rhizoma Smilacis Glabrae raw medicinal material vacuum drying to moisture, baking temperature 75 degree is crushed to 15 orders, the enzymolysis solution that adds 12 times of amounts enzymolysis 6 hours under the temperature of 55 degree.The enzymolysis solution method for preparing is: it is 4.5 buffer that 11 gram plant extract enzymes (enzyme work is 19000 units) are dissolved in the 500mlpH value.Plant extract enzyme wherein consists of that cellulase content 33%, pectase content are 36%, protease content 20%, xylanase 6%.
2, with 12 times to Rhizoma Smilacis Glabrae weight; Concentration is that 90% ethanol carried out reflux, extract, 6 hours under ultrasound wave is auxiliary, and triplicate, merge extractive liquid, are condensed into paste; With combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
Rhizoma Smilacis Glabrae flavone extract through above-mentioned processing obtains contains flavone compound 68% by extract weight; The smilax glabra saponins extract that obtains contains oside compound 61% by extract weight.
Claims (3)
1. a method for preparing smilax glabra saponins, flavone extract is characterized in that, may further comprise the steps:
(1) processing of raw medicinal material; Comprise raw medicinal material is carried out vacuum drying, pulverizing and enzymolysis; With raw medicinal material vacuum drying to moisture is 5%-10%; Baking temperature 50-80 degree is crushed to the 10-20 order, adds enzymolysis solution that 3-12 doubly measures then under the temperature of 35-55 degree enzymolysis 3-10 hour; The method for preparing of used enzymolysis solution is: it is that the plant extract enzyme of 10000-30000 unit is dissolved in the buffer of 500ml that 1-15 is restrained enzyme activity;
Said plant extract enzyme consists of: cellulase content 30-50%, pectase content are 20-40%, protease content 5-20%, xylanase 5-25%; The pH value of buffer is 4-7;
(2) extraction of smilax glabra saponins and flavone compound: use 5-12 doubly to Rhizoma Smilacis Glabrae weight, concentration carried out reflux, extract, 2.5-6 hour as the ethanol of 60-95%; Triplicate, merge extractive liquid; Be condensed into paste; With combining extraction liquid behind the chloroform extraction 2 times, concentrate and vacuum drying gets flavone extract behind the defat with petroleum ether; Reuse ethyl acetate extraction 2 times and combining extraction liquid, concentrated vacuum drying gets Saponin class extract.
2. the method for preparing smilax glabra saponins, flavone extract according to claim 1 is characterized in that: in the leaching process of said smilax glabra saponins and flavone compound, use the auxiliary alcohol reflux that carries out of ultrasound wave.
3. the smilax glabra saponins and the flavone extract that make according to the said method of claim 1 is characterized in that: by extract obtained weight, contain oside compound 20-70% in the smilax glabra saponins extract; Contain flavone compound 30-80% in the Rhizoma Smilacis Glabrae flavone extract.
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| CN101993902A (en) * | 2010-10-27 | 2011-03-30 | 漳州职业技术学院 | Method for extracting flavonoids compounds from asparagus and leftovers thereof |
| CN102671066A (en) * | 2012-05-18 | 2012-09-19 | 江西农业大学 | Hangover-alleviating compound and preparation method thereof |
| CN104435021A (en) * | 2014-11-11 | 2015-03-25 | 青海康普生物科技股份有限公司 | Extraction method of sea buckthorn flavonoids |
| CN105056027B (en) * | 2015-08-05 | 2019-12-17 | 贵州中医药大学 | Effective part of glabrous greenbrier rhizome with red section and application thereof |
| CN105902695B (en) * | 2016-05-24 | 2020-06-19 | 河北天元药业有限公司 | Novel method for preparing Shuangding injection |
| CN109259027B (en) * | 2018-12-20 | 2019-04-12 | 烟台五神生物科技有限公司 | A kind of health beverages |
| CN115453035A (en) * | 2022-10-18 | 2022-12-09 | 湖南祥民制药有限公司 | Method for extracting high-content notoginsenoside R1 from panax notoginseng |
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| CN101129890A (en) * | 2007-08-20 | 2008-02-27 | 陈江 | Oral liquid of cicada shell and lightyellow sophora root |
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| CN101129890A (en) * | 2007-08-20 | 2008-02-27 | 陈江 | Oral liquid of cicada shell and lightyellow sophora root |
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| 陈红梅等.土茯苓的化学与药理研究进展.《中国民族医药杂志》.2008,(第11期),71-73. * |
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