CN101830995B - Method for extracting polysaccharide by adopting decompressing inner ebullition - Google Patents
Method for extracting polysaccharide by adopting decompressing inner ebullition Download PDFInfo
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Abstract
The invention relates to an extracting method of polysaccharide, which is characterized by comprising the following steps of: firstly, taking low-concentration ethanol as a solvent to extract and separate out micromolecule components by adopting a decompressing inner ebullition; then taking water as a solvent to extract polysaccharide from materials to be extracted by adopting the decompressing inner ebullition. Since the extracting temperature is low and the extracting time is short, starch can not be pasted and the swelling of the materials is small, the diffusion of the micromolecules of the polysaccharide is not influenced, and impurities of an extracting solution are less and the filtration is easy. Compared with the traditional polysaccharide extracting and separating technology, the consumption level of the ethanol of the extracting method of polysaccharide is reduced by more than 1 time, the speed of the extracting process is increased by 10-20 times, and the yield and the purity of the polysaccharide are respectively increased by 10-50 percent and 10-40 percent.
Description
Technical field
The present invention relates to the polysaccharide extraction and separation technology, particularly adopt decompressing inner ebullition to extract the method for polysaccharide.
Background technology
Polysaccharide has multiple biological activity, is the polymer that aldose or ketose link together through glycosidic bond, by more than 20 to up to ten thousand monose molecular compositions, mainly is present in plant and the mikrobe with unbound state or combination.It has multiple pharmacological effect, more and more receives publicity.Polysaccharide is the polarity macromolecular cpd; With also have macromolecular substance such as soluble small molecular material such as monose, amino acid and starch, protein in the material of polysaccharide coexistence; Therefore; The extraction of polysaccharide adopts the alcohol reflux pre-treatment to isolate small molecular weight impurity mostly earlier, adopts hot water to make to extract solvent then and extracts, and take the alcohol precipitation operation that polysaccharide is carried out roughing out.Process for extracting like the disclosed a kind of Auricularia polysaccharide of Chinese patent [application number 200410020591]; Earlier with ethanol in the raw material after the pulverizing is carried out pre-treatment; Remove impurity such as pigment, monose; And then with microwave or UW and combine the combined-enzyme method enzymolysis, the polysaccharide material in the auricularia auriculajudae fully is dissolved out.The Study on extraction of the ganoderma active polysaccharide of delivering just like " ACAD J GCP " (2009 the 4th phase 348-351 pages or leaves); With 10 times of amount ethanol, 70 ℃ of water-bath backflow 30min do pre-treatment, filter; Filter residue added 15 times of water gaging ultrasonic times 20 minutes, again 80 ℃ of following water extraction 2 hours.These process for extracting solvent consumption when the pre-treatment of raw material metamorphosis many, material are big, influence follow-up polysaccharide stripping; When hot water extraction, the extraction high time of temperature is long, and impurity strippings such as starch and protein are many, and starch pasting can cause filtration difficulty and yield to descend.
" Guangxi science " (2006 the 1st phase 43-45 pages or leaves) proposes the decompressing inner ebullition process for extracting of effective ingredients in plant, and is used for the extraction of the chlorogenicacid of Japanese Honeysuckle, obtained effect preferably.But also report does not adopt the extraction of decompressing inner ebullition extraction method to the biomacromolecule polysaccharide.
Summary of the invention
The purpose of this invention is to provide a kind of extraction method of polysaccharides that solvent consumption is few, the time is short and yield is high that extracts; It is characterized in that being earlier that solvent adopts decompressing inner ebullition method extraction separation to go out the small molecules composition with the low-concentration ethanol; And then be that solvent adopts decompressing inner ebullition to extract polysaccharide with water, extracted polysaccharide from carrying the plant.
Performing step of the present invention and condition are following:
1, uses that to be carried 0.5～2 times of quality of material, mass concentration be 45～75% the wetting material powder of being carried of aqueous ethanolic solution; Adding consumption then is that 35～60 ℃, mass concentration are 5～20% aqueous ethanolic solution for carrying 6～12 times of quality of material, temperature; And reduce to 0.02～0.03MPa to pressure; Extracted 1～4 minute, and shed the pressure after-filtration, obtain the good wet cake of pre-treatment;
2, adding consumption toward wet cake is 50～70 ℃ hot water for carrying 8～20 times of quality of material, temperature, and reduces to 0.025～0.04MPa to pressure, extracts 3～10 minutes, sheds the pressure after-filtration, obtains polysaccharide and filtrates;
3, be concentrated into 1/5～1/15 of stoste volume to polysaccharide filtrating, adding volume then is that 2～3 times of liquid concentrator volumes, mass concentration are 95% ethanol, leaves standstill 2～10 hours, filters, and the wet cake drying obtains polysaccharide product.
Principle of the present invention is; When adopting for the first time the low-concentration ethanol decompressing inner ebullition to extract, because the temperature of extracting is low and the time is short, the swelling of material is very little; Can not influence the diffusion of subsequent extracted polysaccharide macro-molecular, polysaccharide is because alcoholic acid exists the little also loss of solubleness few; When adopting for the second time the water decompressing inner ebullition to extract; Since extract for the first time material inside residual certain density ethanol arranged; So need not to use alcohol desorption, and the extraction temperature that adopts is below starch gelatinization temperature, the same variation of the form of material does not help the diffusion of polysaccharide again very much; Extracting solution impurity is few, filters easily.
The present invention extracts with existing polysaccharide and stripping technique is compared, and its outstanding substantive distinguishing features and obvious improvement is:
During (1) owing to pre-treatment, alcohol concn is low, and consumption of ethanol reduces more than 1～4 times.
(2) leaching process speed is fast 4～10 times, has suffered the extraction separation process efficiency and is enhanced about more than once.
(3) yield of polysaccharide and purity improve 10～50% and 10～40% respectively.
Embodiment
Embodiment one: Radix Notoginseng polysaccharide extracts
It is 55% the wetting Notoginseng Root of aqueous ethanolic solution that 0.8 times of quality of material, mass concentration are carried in use; Adding consumption then is 45 ℃ 5% aqueous ethanolic solution for carrying 8 times of quality of material, temperature; And reduce to 0.026MPa to pressure; Pre-treatment was extracted 2 minutes, shed the pressure after-filtration, obtained the well wet Radix Notoginseng powder of pre-treatment; Adding consumption toward wet Radix Notoginseng powder is that 15 times of pseudo-ginseng quality, temperature are 60 ℃ hot water, and reduces to 0.028MPa to pressure, extracts 8 minutes, sheds the pressure after-filtration, obtains polysaccharide filtrating; Polysaccharide filtrating is concentrated into 1/10 of stoste, and adding volume then is that 2.5 times of liquid concentrator volumes, mass concentration are 95% ethanol, places 5 hours, filters, and the wet cake drying obtains Radix Notoginseng polysaccharide.Compare with traditional extraction using alcohol pre-treatment, amount of ethanol reduces 3 times; 15 times of the leaching process time decreased of polysaccharide, polysaccharide yield and purity improve 40% and 15% respectively.
Embodiment two: lentinan extracts
It is 60% the wetting mushroom powder of aqueous ethanolic solution that 1.2 times of quality of material, mass concentration are carried in use; Adding consumption then is 45 ℃ 15% aqueous ethanolic solution for carrying 8 times of quality of material, temperature; And reduce to 0.028MPa to pressure; Extracted 2 minutes, and shed the pressure after-filtration, obtain the well wet material of being carried of pre-treatment; Adding consumption is that 15 times of mushroom quality, temperature are 55 ℃ hot water, and reduces to 0.026MPa to pressure, extracts 6 minutes, sheds the pressure after-filtration, obtains polysaccharide extraction liquid; Polysaccharide extraction liquid is concentrated into 1/10 of stoste, and adding volume then is that 2.5 times of liquid concentrator volumes, mass concentration are 95% ethanol, places 5 hours, filters, and the wet cake drying obtains lentinan.Compare with traditional extraction using alcohol pre-treatment, amount of ethanol reduces 2 times; 20 times of the leaching process time decreased of polysaccharide, polysaccharide yield and purity improve 35% and 20% respectively.
Embodiment three: LBP extracts
It is 60% the wetting matrimony vine powder of aqueous ethanolic solution that 1 times of quality of material, mass concentration are carried in use; Adding consumption then is 45 ℃ 10% aqueous ethanolic solution for carrying 10 times of quality of material, temperature; And reduce to 0.028MPa to pressure; Extracted 3 minutes, and shed the pressure after-filtration, obtain the well wet material of being carried of pre-treatment; Adding consumption is that 15 times of matrimony vine quality, temperature are 55 ℃ hot water, and reduces to 0.025MPa to pressure, extracts 6 minutes, sheds the pressure after-filtration, obtains polysaccharide extraction liquid; Polysaccharide extraction liquid is concentrated into 1/8 of stoste, and adding volume then is that 2.3 times of liquid concentrator volumes, mass concentration are 95% ethanol, places 8 hours, filters, and the wet cake drying obtains LBP.Compare with traditional extraction using alcohol pre-treatment, amount of ethanol reduces 2 times; 20 times of the leaching process time decreased of polysaccharide, polysaccharide yield and purity improve 45% and 25% respectively.
Embodiment four: ganoderan extracts
It is 65% the wetting REISH of aqueous ethanolic solution that 2 times of quality of material, mass concentration are carried in use; Adding consumption then is 35 ℃ 15% aqueous ethanolic solution for carrying 6 times of quality of material, temperature; And reduce to 0.023MPa to pressure; Extracted 2 minutes, and shed the pressure after-filtration, obtain the well wet material of being carried of pre-treatment; Adding consumption is that 15 times of glossy ganoderma quality, temperature are 65 ℃ hot water, and reduces to 0.032MPa to pressure, extracts 6 minutes, sheds the pressure after-filtration, obtains polysaccharide extraction liquid; Polysaccharide extraction liquid is concentrated into 1/10 of stoste, and adding volume then is that 2.5 times of liquid concentrator volumes, mass concentration are 95% ethanol, places 5 hours, filters, and the wet cake drying obtains ganoderan.Compare with traditional extraction using alcohol pre-treatment, amount of ethanol reduces 2 times; The leaching process of polysaccharide, 20 times of time decreased, polysaccharide yield and purity improve 35% and 20% respectively.
Embodiment five: the Largeleaf Gymnema polysaccharide extracts
It is 65% the wetting Largeleaf Gymnema powder of aqueous ethanolic solution that 1.5 times of quality of material, mass concentration are carried in use; Adding consumption then is 45 ℃ 20% aqueous ethanolic solution for carrying 8 times of quality of material, temperature; And reduce to 0.03MPa to pressure; Extracted 3 minutes, and shed the pressure after-filtration, obtain the well wet material of being carried of pre-treatment; Adding consumption is that 15 times of Largeleaf Gymnema quality, temperature are 55 ℃ hot water, and reduces to 0.024MPa to pressure, extracts 6 minutes, sheds the pressure after-filtration, obtains polysaccharide extraction liquid; Polysaccharide extraction liquid is concentrated into 1/10 of stoste, and adding volume then is that 2.5 times of liquid concentrator volumes, mass concentration are 95% ethanol, places 5 hours, filters, and the wet cake drying obtains the Largeleaf Gymnema polysaccharide.Compare with traditional extraction using alcohol pre-treatment, amount of ethanol reduces 2 times; 20 times of the leaching process time decreased of polysaccharide, polysaccharide yield and purity improve 15% and 15% respectively.
Claims (1)
1. an extraction method of polysaccharides is characterized in that being earlier that solvent adopts the decompressing inner ebullition method to carry out pre-treatment with ethanol, and then is solvent employing decompressing inner ebullition extraction polysaccharide with water, and concrete steps are following:
(1) uses that to be carried 0.5～2 times of quality of material, mass concentration be 45～75% the wetting material powder of being carried of aqueous ethanolic solution; It is that Notoginseng Root, mushroom powder, REISH, Largeleaf Gymnema powder are wherein a kind of that the quilt is here carried material; Adding consumption then is that 35～60 ℃, mass concentration are 5～20% aqueous ethanolic solution for carrying 6～12 times of quality of material, temperature, and reduces to 0.02～0.03MPa to pressure, extracts 1～4 minute; Shed the pressure after-filtration, obtain the good wet cake of pre-treatment;
(2) adding consumption toward wet cake is 50～70 ℃ hot water for carrying 8～20 times of quality of material, temperature, and reduces to 0.025～0.04MPa to pressure, extracts 3～10 minutes, sheds the pressure after-filtration, obtains polysaccharide extraction liquid;
(3) be concentrated into 1/5～1/15 of stoste volume to polysaccharide extraction liquid, adding volume then is that 2～3 times of liquid concentrator volumes, mass concentration are 95% ethanol, leaves standstill 2～10 hours, filters, and the wet cake drying obtains polysaccharide product.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105294869A (en) * | 2014-07-11 | 2016-02-03 | 杨平 | Preparation method for extracting water-soluble polyose from black pine needles according to decompression inner-boiling method |
| CN104946454B (en) * | 2015-06-08 | 2017-07-04 | 齐鲁工业大学 | A kind of preparation method of pine needle medlar yellow wine |
| CN105777929A (en) * | 2016-05-19 | 2016-07-20 | 福建省农业科学院农业工程技术研究所 | Extracting method for pleurotus eryngii polysaccharide |
| CN106832040B (en) * | 2017-04-01 | 2019-08-13 | 河南夕阳蓝食品科技有限公司 | A kind of extracting method of lentinan |
| CN110003352A (en) * | 2019-04-12 | 2019-07-12 | 北部湾大学 | A kind of extracting method that moringa seeds selenium active constituent is effectively kept |
| CN110092846A (en) * | 2019-05-30 | 2019-08-06 | 遵义医科大学 | A method of extracting Dendrobium officinale polysaccharide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1679801A (en) * | 2005-01-12 | 2005-10-12 | 广西大学 | Pressure-released internal vaporizing extraction of plant effective component |
| CN1879662A (en) * | 2006-05-12 | 2006-12-20 | 广西大学 | Method for extracting plant effective component by interior evaporation and diacolation |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1679801A (en) * | 2005-01-12 | 2005-10-12 | 广西大学 | Pressure-released internal vaporizing extraction of plant effective component |
| CN1879662A (en) * | 2006-05-12 | 2006-12-20 | 广西大学 | Method for extracting plant effective component by interior evaporation and diacolation |
Non-Patent Citations (1)
| Title |
|---|
| 李春玲，等.三七总皂苷的减压内部沸腾提取及树脂吸附分离.《时珍国医国药》.2009,第20卷(第2期), * |
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