CN1810841A - Chrysanthemum polysaccharide extracting process - Google Patents
Chrysanthemum polysaccharide extracting process Download PDFInfo
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- CN1810841A CN1810841A CN 200510019403 CN200510019403A CN1810841A CN 1810841 A CN1810841 A CN 1810841A CN 200510019403 CN200510019403 CN 200510019403 CN 200510019403 A CN200510019403 A CN 200510019403A CN 1810841 A CN1810841 A CN 1810841A
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Abstract
The chrysanthemum polysaccharide extracting process includes the following steps: water extraction of coarse polysaccharide from the medicine material; eliminating liposoluble impurities with chloroform, petroleum ether, etc; alcohol precipitation to separate precipitate as the chrysanthemum polysaccharide from water extracted matter, and final drying to obtain solid chrysanthemum polysaccharide. The chrysanthemum polysaccharide extracting process is fast, simple, low in cost, high in yield, and is favorable to the medical application of chrysanthemum polysaccharide.
Description
Technical field
The invention belongs to the extracting method of Chinese medicine active ingredient, more particularly it relates to a kind of extracting method of chrysanthemum polysaccharide.
Background technology
Polysaccharide is the polarity macromolecular cpd.Generally (plant, microorganism, marine alga etc.) extract from natural product.Up to the present, existing nearly hundred kinds of polysaccharide compounds are extracted out. and many experiments prove that all polysaccharide and infection, tumour, inflammation and some autoimmune disorders have substantial connection.Therefore STUDY ON POLYSACHAROSE and exploitation are more and more caused people's extensive concern.The bioactive research of polyose medicament be the most active in the polyose research also be to make progress the fastest field.Carbohydrate is found in the immunity system and plays a key role in recent years, and is especially true in the defence process of human body to the virus-type bacteria attack.The modern medicine study card: chrysanthemum has remarkable coronary artery dilator, strengthens the effect of coronary artery blood flow, can suppress the katabolism of the synthetic and increased excretions of cholesterol of cholesterol in the liver, and the effect of anti-inflammatory refrigerant is arranged, and informal dress can be promoted longevity.So far yet there are no the relevant report of chrysanthemum polysaccharide extracting method.
Summary of the invention
The objective of the invention is to propose a kind of extracting method of chrysanthemum polysaccharide.The present invention adopts pure bleed formulation with polysaccharide in the orthogonal experiment method optimization chrysanthemum, with chrysanthemum polysaccharide extraction productive rate and content is index, to the flooding time in the leaching process, extraction temperature, the extraction effect of three levels of three factors of the alcohol concn that precipitating is used is analysed in depth, determine to extract the optimum extraction condition of chrysanthemum polysaccharide at last, for the development and use of chrysanthemum polysaccharide provide test basis.
The objective of the invention is to reach by following measure: the extraction of chrysanthemum polysaccharide is adopted water to carry ethanol and is separated out the precipitator method, its principle is soluble in water according to chrysanthemum polysaccharide, be insoluble in ethanol, sherwood oil, the character of chloroform equal solvent, used water extracts Crude polysaccharides earlier from former herbal medicine, with weeding of grease solubility impurities such as chloroform, sherwood oils, with ethanol it is precipitated from aqueous extract at last and separate out, thereby isolate chrysanthemum polysaccharide, drying promptly obtains the solid chrysanthemum polysaccharide.
More particularly it in turn includes the following steps:
1.. get a certain amount of chrysanthemum and add 30 times of water termostats immersions, extraction time is 1-3 hour, and lixiviate constant temperature filters in 80-100 ℃ of scope, gets extracting solution;
2.. the chrysanthemum residue that will soak adds 15-20 times of water again to be continued constant temperature and soaked 30 minutes, filter extracting solution; The chrysanthemum residue that will soak for the third time adds 15-20 times of water to be continued constant temperature and soaked 30 minutes, filter extracting solution; Merge No. three times extracting solution;
3.. place rotatory evaporator to be concentrated into 3 times of quantity of fluid of quantitative chrysanthemum extracting solution, centrifugal collection supernatant liquor removes albumen 2 times with sevag reagent method, extracts the weeding of grease solubility impurity 1-3 time, the water intaking layer with chloroform or 2 times of amounts of ethyl acetate;
4.. add ethanol in water layer, collecting the alcohol concn scope is the precipitation that 70-90% separates out, and precipitation is washed respectively 2 times with acetone and ether, and drying promptly gets the solid chrysanthemum polysaccharide.
In technique scheme, described soak time is that 2 hours, extraction temperature are that 100 ℃, precipitation are 80% with alcohol concn.
In technique scheme, described soak time is that 3 hours, extraction temperature are that 100 ℃, precipitation are 80% with alcohol concn.
The present invention is a kind of method of extracting chrysanthemum polysaccharide, has filled up the blank of chrysanthemum polysaccharide extracting method, and present method is extracted chrysanthemum polysaccharide and had advantage quick, easy, that cost is low, yield is high.Help further studying the application of chrysanthemum polysaccharide in medical treatment.
Description of drawings
Fig. 1 influences the factor comparison diagram of chrysanthemum polysaccharide productive rate for orthogonal test of the present invention;
Fig. 2 influences the factor comparison diagram of chrysanthemum polysaccharide content for orthogonal test of the present invention.
Embodiment
Describe performance of the present invention in detail below in conjunction with accompanying drawing: (notes X-coordinate in Fig. 1, Fig. 2 is an influence factor, and ordinate zou is the K value, and the difference of same factor MAX and MIN is extreme value R)
1, the extracting method of chrysanthemum polysaccharide: 1.. the chrysanthemum of getting 50g adds 30 times of water 1500ml constant temperature and soaks, and extraction time is 1-3 hour, and lixiviate constant temperature filters in 80-100 ℃ of scope, gets extracting solution;
2.. the chrysanthemum that soaks is added 900ml water again continues constant temperature and soaked 30 minutes, filter extracting solution; Again the chrysanthemum that soaks is added 900ml water and continues constant temperature and soaked 30 minutes, filter extracting solution; Merge No. three times extracting solution;
3.. place rotatory evaporator to be concentrated into 150ml extracting solution, centrifugal collection supernatant liquor removes albumen 2 times with sevag reagent method, extracts the weeding of grease solubility impurity 1-3 time with chloroform or ethyl acetate 100ml, the water intaking layer;
4.. add ethanol in water layer, collecting alcohol concn is the precipitation that 70-90% separates out, and precipitation is washed respectively 2 times with acetone and ether, and drying promptly gets the solid chrysanthemum polysaccharide.
2. chrysanthemum polysaccharide Determination on content method:
2.1 measuring method: the absorbancy of measuring different concns glucose with the phenolsulfuric acid method is formulated concentration-absorbancy typical curve, the chrysanthemum polysaccharide sample is made into certain density solution again and operates its absorbancy of survey down by the typical curve item, substitution concentration-absorbancy typical curve equation calculates the gained polysaccharide content.
2.2 the preparation precision of typical curve takes by weighing the glucose reference substance 10.2mg that is dried to constant weight, puts in the 100ml measuring bottle, is dissolved in water and is diluted to scale, shakes up, and promptly gets glucose reference substance storing solution.Accurately measure above-mentioned reference substance solution 1.0,2.0,3.0,4.0,5.0ml, put respectively in the 10ml measuring bottle, respectively get 0.5ml more respectively and add vitriol oil 7.5ml and 5% phenol 1.5ml, in 40 ℃ of insulations 30 minutes, measure optical density at 490nm wavelength place, get regression equation C=132.57A-20.67, r=0.9971.The result shows, at 10.2～51.0 μ gml
-1Concentration range in have good linear relationship.
2.3 orthogonal experimental design is according to the extraction process of above-mentioned test, through single-factor simultaneous test repeatedly, the factor of orthogonal experimental design is: 3 factors such as flooding time, extraction temperature, sedimentary alcohol concn, every factor 3 levels (seeing Table 1), productive rate and content with chrysanthemum polysaccharide serve as to investigate index, with L9 (3
4) orthogonal table arrangement test.
Table 1 factor and water-glass
| Level | A extraction time (h) | The B extraction temperature (℃) | C alcohol concn (%) | The |
| 1 | 1 | 80 | 70 | |
| 2 | 2 | 90 | 80 | |
| 3 | 3 | 100 | 90 |
(annotate: other conditionally complete is identical during test)
3. result: extract chrysanthemum polysaccharide by orthogonal experiment design, yield and content results see Table 2.
Table 2 chrysanthemum polysaccharide extracts orthogonal experiment plan and takes into account the result
| A | B | C | Error | Productive rate (%) | Content (%) | ||
| | 1 | 1 | 1 | 1 | 3.68 | 33.03 | |
| | 1 | 2 | 2 | 2 | 2.46 | 30.32 | |
| | 1 | 3 | 3 | 3 | 4.37 | 44.12 | |
| Embodiment 4 | 2 | 1 | 2 | 3 | 3.62 | 51.31 | |
| | 2 | 2 | 3 | 1 | 5.12 | 64.34 | |
| | 2 | 3 | 1 | 2 | 4.37 | 40.34 | |
| Embodiment 7 | 3 | 1 | 3 | 2 | 3.03 | 40.16 | |
| Embodiment 8 | 3 | 2 | 1 | 3 | 2.38 | 54.00 | |
| Embodiment 9 | 3 | 3 | 2 | 1 | 6.69 | 80.45 | |
| Productive rate | k1 | 10.51 | 10.329 | 10.42 | |||
| k2 | 13.09 | 9.942 | 12.77 | ||||
| k3 | 12.09 | 15.432 | 12.51 | ||||
| R | 0.86 | 1.830 | 0.78 | ||||
| Content | k1 | 107.47 | 124.49 | 127.38 | |||
| k2 | 155.99 | 148.67 | 162.08 | ||||
| k3 | 174.61 | 164.91 | 148.61 | ||||
| R | 22.38 | 13.47 | 11.57 |
(annotate: other conditionally complete is identical during test)
3.1 determining of the processing condition of optimum extraction chrysanthemum polysaccharide productive rate: can draw each factor each horizontal sum K1, K2, K3 through computing.By the peak value of the R value of productive rate in the table 2 and Fig. 1 as can be seen, the factor ordering that productive rate is extracted in influence is B＞A＞C, and B has the greatest impact, and C is then minimum.Comprehensive each factor K value and direct visual comparison, drawing in theory, the processing condition of optimum extraction productive rate are A2B3C2.So determine its optimum extraction productive rate processing condition be: extraction time is 2h, and extraction temperature is 100 ℃, and the precipitating alcohol concn is 80%.
3.2 determining of the processing condition of optimum extraction chrysanthemum polysaccharide content: in addition, analyzed by R value and the Fig. 2 of content in the table 2, the factor that influences its content sorts and is: A＞B＞C.The influence of A is more remarkable.Illustrate in the leaching process that extraction time is maximum to the content influence of chrysanthemum polysaccharide, time lengthening helps improving the content of chrysanthemum polysaccharide; Alcohol concn, extraction temperature are also bigger to the influence of chrysanthemum polysaccharide content, and by finding out in the table that precipitation is 80% with alcohol concn, content was higher when extraction temperature was 100 ℃.See that from K1, K2, the K3 of its content the processing condition of gained chrysanthemum polysaccharide content the best are A3B3C2.To sum up stating the optimum process condition that extracts chrysanthemum polysaccharide is preferably: extraction time is 3h, and extraction temperature is 100 ℃, and the alcohol concn that precipitating is used is 80%.
3.3 confirmatory experiment: be the checking optimised process, take by weighing chrysanthemum 50g, promptly add 30 times of water gagings extractions 3 times according to optimizing back gained optimum extraction process, extraction time is 3h, extraction temperature is 100 ℃, the alcohol concn that precipitating is used is 80% to extract, and the gained polysaccharide is weighed and carried out assay.The result shows that polysaccharide yield is 6.25%, and the relative percentage composition of chrysanthemum polysaccharide is 78.30%, and is consistent with the optimum level in the orthogonal table as can be known, illustrates that the determined technology of the present invention is reasonable.
Need to prove: to those of ordinary skill in the art, can also make some changes or distortion to the present invention under the prerequisite that does not change the principle of the invention, this belongs to protection scope of the present invention equally.
Claims (3)
1, a kind of extracting method of chrysanthemum polysaccharide is characterized in that it in turn includes the following steps:
1.. get a certain amount of chrysanthemum and add 30 times of water termostats immersions, extraction time is 1-3 hour, and lixiviate constant temperature filters in 80-100 ℃ of scope, gets extracting solution;
2.. the chrysanthemum residue that will soak adds 15-20 times of water again to be continued constant temperature and soaked 30 minutes, filter extracting solution; The chrysanthemum residue that will soak for the third time adds 15-20 times of water to be continued constant temperature and soaked 30 minutes, filter extracting solution; Merge No. three times extracting solution;
3.. place rotatory evaporator to be concentrated into 3 times of quantity of fluid of quantitative chrysanthemum extracting solution, centrifugal collection supernatant liquor removes albumen 2 times with sevag reagent method, extracts the weeding of grease solubility impurity 1-3 time, the water intaking layer with chloroform or 2 times of amounts of ethyl acetate;
4.. add ethanol in water layer, collecting the alcohol concn scope is the precipitation that 70-90% separates out, and precipitation is washed respectively 2 times with acetone and ether, and drying promptly gets the solid chrysanthemum polysaccharide.
2, the extracting method of a kind of chrysanthemum polysaccharide according to claim 1 is characterized in that described soak time is that 2 hours, extraction temperature are that 100 ℃, precipitation alcohol concn are 80%.
3, the method for extracting the Japanese Honeysuckle polysaccharide from Japanese Honeysuckle according to claim 1 is characterized in that described soak time is that 3 hours, extraction temperature are that 100 ℃, precipitation alcohol concn are 80%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101869588A (en) * | 2010-06-29 | 2010-10-27 | 浙江大学 | Preparation method and application of effective component of chrysanthemum |
| CN102188469A (en) * | 2011-05-27 | 2011-09-21 | 河南大学 | Chrysanthemum morifolium extractive with live protection function, extraction method and applications thereof |
| CN101659708B (en) * | 2009-08-27 | 2012-05-30 | 昆明理工大学 | Method for extracting and purifying medical polysaccharide of large leaf moss |
| CN103554284A (en) * | 2013-10-11 | 2014-02-05 | 青岛农业大学 | Extraction and separation process for peony stamen polysaccharide |
| CN103788221A (en) * | 2013-10-11 | 2014-05-14 | 青岛农业大学 | Araban in peony stamens and extraction separation method thereof |
| CN104292350A (en) * | 2014-09-17 | 2015-01-21 | 上海交通大学 | Extraction process and application of chrysanthemum polysaccharide |
| CN110463807A (en) * | 2019-07-15 | 2019-11-19 | 合肥工业大学 | A kind of auxiliary reducing blood lipid soft sweets and preparation method thereof rich in emperor's chrysanthemum polysaccharide |
| CN112279933A (en) * | 2020-11-30 | 2021-01-29 | 河南大学 | Chrysanthemum polysaccharide, extraction method and application thereof in preparing medicine for treating functional constipation |
-
2005
- 2005-09-08 CN CN 200510019403 patent/CN1810841A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101659708B (en) * | 2009-08-27 | 2012-05-30 | 昆明理工大学 | Method for extracting and purifying medical polysaccharide of large leaf moss |
| CN101869588A (en) * | 2010-06-29 | 2010-10-27 | 浙江大学 | Preparation method and application of effective component of chrysanthemum |
| CN101869588B (en) * | 2010-06-29 | 2012-05-02 | 浙江大学 | Preparation method and application of effective component of chrysanthemum |
| CN102188469A (en) * | 2011-05-27 | 2011-09-21 | 河南大学 | Chrysanthemum morifolium extractive with live protection function, extraction method and applications thereof |
| CN103554284A (en) * | 2013-10-11 | 2014-02-05 | 青岛农业大学 | Extraction and separation process for peony stamen polysaccharide |
| CN103788221A (en) * | 2013-10-11 | 2014-05-14 | 青岛农业大学 | Araban in peony stamens and extraction separation method thereof |
| CN103788221B (en) * | 2013-10-11 | 2016-06-08 | 青岛农业大学 | Arabinan and extraction and separation method thereof in a kind of tree peony stamen |
| CN104292350A (en) * | 2014-09-17 | 2015-01-21 | 上海交通大学 | Extraction process and application of chrysanthemum polysaccharide |
| CN104292350B (en) * | 2014-09-17 | 2017-05-24 | 上海交通大学 | Extraction process and application of chrysanthemum polysaccharide |
| CN110463807A (en) * | 2019-07-15 | 2019-11-19 | 合肥工业大学 | A kind of auxiliary reducing blood lipid soft sweets and preparation method thereof rich in emperor's chrysanthemum polysaccharide |
| CN112279933A (en) * | 2020-11-30 | 2021-01-29 | 河南大学 | Chrysanthemum polysaccharide, extraction method and application thereof in preparing medicine for treating functional constipation |
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