CN101580551B - Method for extracting polygonatum odoratum polysaccharide - Google Patents
Method for extracting polygonatum odoratum polysaccharide Download PDFInfo
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- CN101580551B CN101580551B CN2009100121857A CN200910012185A CN101580551B CN 101580551 B CN101580551 B CN 101580551B CN 2009100121857 A CN2009100121857 A CN 2009100121857A CN 200910012185 A CN200910012185 A CN 200910012185A CN 101580551 B CN101580551 B CN 101580551B
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Abstract
The invention provides a method for extracting polygonatum odoratum polysaccharide. The method comprises that: polygonatum odoratum crude drug powder is extracted by ultrasonic; water is used as an extracting agent; the extracting temperature is between 20 and 80 DEG C; the ultrasonic frequency is between 30 and 100kHz; the powder is filtered after extracting; the extract is decompressed and concentrated; absolute ethanol is added into the extract to separate precipitate; and the precipitate is washed by acetone, frozen, dried and crushed. Ultrasonic extraction is adopted, so the extract has small dosage, the quantity of polysaccharide dissolved in the extract is reduced, the yield of the polysaccharide is improved, the extracting temperature is reduced by 10 to 20 DEG C compared with the prior method, and low temperature extraction is favorable for protecting effective ingredients. Meanwhile, the extracting time is shortened by over 1 hour. Compared with conventional methods, such as the decocting method, the immersion method, the percolation method and the like, the ultrasonic extraction method has the advantages of time conservation, energy conservation, high extracting efficiency and the like.
Description
Technical field
The present invention relates to a kind of vegetable polysaccharides class material extracting method, relate to the extraction of fragrant solomonseal rhizome polyoses specifically.
Background technology
In recent years, along with the progress of phylactic agent, microbial film and multiple biologically active substance shows, carbohydrate function in vivo is not limited to provide energy and participation structure, also has diversified biological function simultaneously, in vital movement, participated in the comings and goings of cell, especially STUDY ON POLYSACHAROSE has become the focus that people pay close attention to, the various countries scholar seeks with the research of extracting the polysaccharide component with certain physiologically active very active from various biomaterials, thereby makes the research of polyose that the trend that unprecedentedly develops rapidly arranged.Along with to the understanding in depth of active polysaccharide, and people are to the high praise of various natural medicines, whole food, and polysaccharide is nontoxic with it, have no side effect, and be nutrition, the effective constituent of functional health product such as medical assistance, paid attention to by the world today.Constitute the polyose of one of base substance of life,, extensively be present in animal cell membrane, plant and the microorganism wall with its diversified form.
Along with deepening continuously of Celluar and Molecular Biology research, the biological activity of polyose is more and more paid attention to by people, and especially it more makes it become one of focus of current drug research to immune two-ways regulation function.People can trace back to the discovery of Shear in 1936 to the polysaccharide anti-tumor activity to the preliminary research of polysaccharide.To the fifties, find that successively some fungus polysaccharides and higher plant polysaccharide have tangible antitumor activity.Since the seventies, scientists finds that polysaccharide and saccharide complex participate in and mediated the adjusting of the various biological phenomenas of cell, the particularly adjusting of immunologic function, polysaccharide especially herbal polysaccharide because of having enhancing body immunologic function and pharmacological action such as antitumor, and almost do not have toxicity and can control its quality by chemical means, more and more cause domestic and international pharmacologist, biologist and chemists' interest, become current research focus.The sugar chain of finding polysaccharide the eighties again has decisive action in molecular biology, can control cell fission and differentiation, regulates the growth and the aging of cell.
Discovering of nearest three more than ten years, polysaccharide and saccharide complex have participated in the adjusting of the various biological phenomenas of cell.Polysaccharide compound is a kind of immunomodulator, and its energy immune cell activated improves body's immunological function, and normal cell is not had toxic side effect.Up to the present, existing more than 300 kind of polysaccharide compound separated extracting from natural product, wherein from plant, the water-soluble polysaccharide that especially extracts from Chinese medicine is the most important, has found that the polysaccharide compound in 100 plurality of Chinese has immunologic enhancement.
At present, the radix polygonati officinalis of China is sold to home and overseas market mainly as starting material, vast countries and regions such as main exit Korea S, Japan, South East Asia, America, European Union.Radix polygonati officinalis can be used as resources of medicinal plant and carries out research and development, as the representative plant radix polygonati officinalis of Polygonatum, all produce in most of area in the whole nation, especially with the output maximum of northeast and Hunan area radix polygonati officinalis, be two big major production areas of Chinese radix polygonati officinalis supply, so the title of " Hunan radix polygonati officinalis " and " closing radix polygonati officinalis " is also arranged on commodity.The Hunan radix polygonati officinalis is bigger because of flavour of a drug, mainly as the medicine resource exploitation, closes radix polygonati officinalis because of its free from extraneous odour, and the sugar degree height mainly can be used as the protective foods exploitation.The radix polygonati officinalis extracting method of existing report is decocting method, reflux extraction, percolation etc. mostly, it is long to have an extraction time, there is the certain waste phenomenon in characteristics such as the extraction solvent load is more in large-scale production process, but do not see the relevant report of domestic pass radix polygonati officinalis at present.
Summary of the invention
At the defective that existing polygonatum odoratum polysaccharide extracting method exists, the present invention proposes a kind of easy and simple to handle, extracting method that extraction yield is high.
Finishing the concrete technical measures that the foregoing invention purpose taked is: a kind of extracting method of polygonatum odoratum polysaccharide is characterized in that: extraction process is divided into supersound extraction and refinement treatment, and concrete grammar is as follows:
Supersound extraction: close the radix polygonati officinalis crude drug and crush and screen, get undersize powder and carry out supersound extraction, water is for extracting solvent, solid-liquid ratio 1: 15～40, extracting temperature is 20～80 ℃, ultrasonic frequency is 30～100kHz, extraction time 0.5～3h extracts after-filtration, and filter residue repeats to extract;
Refinement treatment: with the extracting solution concentrating under reduced pressure, put, add anhydrous alcohol solution, shake up, leave standstill, filter to room temperature, sediment separate out, the throw out washing with acetone discards washings, and throw out lyophilize, pulverizing get white powder.
Close the radix polygonati officinalis crude drug and crush and screen, sieved 60 mesh sieves.
The supersound extraction number of times is 1～3 time.
Extracting solution concentrating under reduced pressure, pressure are 0.008～0.05MPa, 25 ℃ of temperature, and being concentrated into the concentrated solution relative density is 1.25～1.36.
The anhydrous alcohol solution consumption is 2～4 times of concentrated solution quality, leaves standstill 12～36h.
Washing with acetone, acetone consumption are 0.5～3 times of throw out quality, washing with acetone 1～3 time.
The fragrant solomonseal rhizome polyoses assay:
The drafting of typical curve: the standardized solution of configuration different concns, measure optical density at the wavelength place of 490nm, be ordinate zou with the optical density, concentration is X-coordinate, the drawing standard curve.With concentration is X-coordinate, and absorbance is that ordinate zou carries out linear regression, gets regression equation to be: A=0.0113C+0.0022, r=0.9991.Linearity range: 12.28～42.98mg/ml.
Samples contg is measured: the accurate 2ml sample solution of drawing in the 100ml concentrated solution, add water to 100ml, therefrom get 2ml again and add 10ml ethanol, stir, 5000 leave heart 10min, get and be precipitated to the 100ml measuring bottle, get 2ml and add 1ml 4% phenol, add 7ml 98% vitriol oil, 40 ℃ of water-bath 30min, frozen water 5min, 490nm measures, by polysaccharide yield in the regression equation calculation sample solution.The quality of polysaccharide in polysaccharide yield=liquid to be measured/pass radix polygonati officinalis quality.
Beneficial effect of the present invention: the present invention is owing to take ultrasonic extraction, and the extracting solution consumption is few, reduces the polysaccharide amount of dissolving in the extracting solution, improves the polysaccharide yield, and extracts temperature and reduce by 10～20 ℃ than existing method, and the time shortens more than 1 hour.With traditional methods such as decocting method, pickling process, percolation relatively, ultrasonic extraction have save time, energy-conservation, extraction efficiency advantages of higher.The ultrasonic disruption process is a physical process, does not have chemical reaction in the leaching process, is remained unchanged at short notice by the biologically active substance of lixiviate, has shortened the broken time.Utilize judder that ultrasonic wave produces, high acceleration, intensive cavitation effect, stirring action etc. all can quicken effective ingredient and enter solvent; thereby improved extraction efficiency; shortened extraction time, saved solvent, extract at low temperature helps the protection of effective constituent.
Embodiment
Embodiment 1: closes the radix polygonati officinalis crude drug powder and crosses 60 mesh sieves, get undersize powder 100g, add entry 1500g, and under 20 ℃, KQ-100DV type numerical control supersonic cleanser (Kunshan Ultrasonic Instruments Co., Ltd.), ultrasonic frequency 30kHz, extraction time 0.5h.Extraction time 3 times filters, and No. three extracting solutions are merged, at vacuum pressure 0.08MPa, under 25 ℃ of the temperature, be evaporated to relative density 1.36, put to room temperature, add 3 times of anhydrous alcohol solution, shake up, leave standstill 12h, filter sediment separate out, with 0.5 times of washing with acetone 3 times, discard washings, throw out gets the 19.96g white powder according to a conventional method in-50 ℃ of following lyophilizes, pulverizing.The polysaccharide yield is 8.79% after measured.
Embodiment 2: close the radix polygonati officinalis crude drug powder and cross 60 mesh sieves, get undersize powder 100g, add entry 3000g, extracting temperature is 50 ℃, ultrasonic frequency 80kHz, extraction time 2h.Extraction time 2 times filters, and extracting solution is merged, be evaporated to relative density 1.18, put, add 4 times of anhydrous alcohol solution to room temperature, shake up, leave standstill 24h, filter sediment separate out, with 1.5 times of washing with acetones 2 times, discard washings, throw out gets the 20.32g white powder according to a conventional method in-50 ℃ of following lyophilizes, pulverizing.The polysaccharide yield is 8.97% after measured.
Embodiment 3: close the radix polygonati officinalis crude drug powder and cross 60 mesh sieves, get undersize powder 100g, add entry 4000g, extracting temperature is 80 ℃, ultrasonic frequency 100kHz, 2 hours extraction times.Extraction time 1 time filters, and extracting solution is evaporated to relative density 1.29, put to room temperature, add 3 times of anhydrous alcohol solution, shake up, left standstill 36 hours, filter, sediment separate out with 3 times of washing with acetones 1 time, discards washings, throw out gets the 22.15g white powder according to a conventional method in-50 ℃ of following lyophilizes, pulverizing.The polysaccharide yield is 9.36% after measured.
Reference examples: the radix polygonati officinalis crude drug powder is crossed 60 mesh sieves, refluxing extraction, water is for extracting solution, and solid-liquid ratio 1: 60 extracts 90～95 ℃ of temperature, and refluxing extraction 4h extracts 3 times, filters, merging filtrate, concentrated, in concentrated solution: dehydrated alcohol=1: 3 ratio, alcohol precipitation 36h.Filter, sediment separate out with 3 times of washing with acetones 3 times, discards washings, and throw out lyophilize, pulverizing must the 22.69g white powders.The polysaccharide yield is 9.56% after measured.
Can find out that from the foregoing description the polysaccharide yield improves with extracting temperature and ultrasonic frequency, example 3 shows that extracting temperature be 80 ℃, and ultrasonic frequency 100kHz extracts once its polysaccharide yield near reference examples, but extraction time only is the sixth of reference examples.
Claims (5)
1. the extracting method of a polygonatum odoratum polysaccharide, it is characterized in that: supersound extraction: close the radix polygonati officinalis crude drug and crush and screen, get undersize powder and carry out supersound extraction, water is the extraction solvent, solid-liquid ratio 1: 40, and extracting temperature is 80 ℃, ultrasonic frequency is 100kHz, extraction time 2h extracts after-filtration, and filter residue repeats to extract;
Refinement treatment: with the extracting solution concentrating under reduced pressure, put, add anhydrous alcohol solution, shake up, leave standstill, filter to room temperature, sediment separate out, the throw out washing with acetone discards washings, and the throw out lyophilize is pulverized, and gets white powder.
2. according to the extracting method of the described polygonatum odoratum polysaccharide of claim 1, it is characterized in that: close the radix polygonati officinalis crude drug and crush and screen, sieved 60 mesh sieves.
3. according to the extracting method of the described polygonatum odoratum polysaccharide of claim 1, it is characterized in that: extracting solution concentrating under reduced pressure, pressure are 0.008～0.05Mpa, and temperature is 25 ℃, and being concentrated into the concentrated solution relative density is 1.25～1.36.
4. according to the extracting method of the described polygonatum odoratum polysaccharide of claim 1, it is characterized in that: the anhydrous alcohol solution consumption is 2～4 times of concentrated solution quality, leaves standstill 12～36h.
5. according to the extracting method of the described polygonatum odoratum polysaccharide of claim 1, it is characterized in that: washing with acetone, acetone consumption are 0.5～3 times of throw out, washing with acetone 1～3 time.
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| CN105535033A (en) * | 2016-03-02 | 2016-05-04 | 云南圣草峰生物科技有限公司 | Method for extracting truffle polysaccharides from truffles |
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| CN105194319A (en) * | 2015-11-08 | 2015-12-30 | 长沙佰顺生物科技有限公司 | Preparation method of polygonatum odoratum polysaccharide medicine composition |
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| CN116675782A (en) * | 2023-05-17 | 2023-09-01 | 宁波大学科学技术学院 | Method for extracting polygonatum odoratum polysaccharide and determination method thereof |
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