CN106046194A - Extraction method of dendrobium huoshanense polysaccharide - Google Patents
Extraction method of dendrobium huoshanense polysaccharide Download PDFInfo
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- CN106046194A CN106046194A CN201610611390.5A CN201610611390A CN106046194A CN 106046194 A CN106046194 A CN 106046194A CN 201610611390 A CN201610611390 A CN 201610611390A CN 106046194 A CN106046194 A CN 106046194A
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- herba dendrobii
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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Abstract
The invention provides an extraction method of dendrobium huoshanense polysaccharide, and in particular relates to a method for extracting dendrobium huoshanense polysaccharide by an ultrasonic wave assistance hot reflux extraction method. According to the extraction method, the extracted polysaccharide is subjected to content detection by a phenol-sulfuric acid method. After the primary impurity removal through diethyl ether addition into dendrobium huoshanense coarse powder, a proper amount of methyl alcohol is added; after ultrasonic wave assistance hot reflux extraction, filtering is performed when the liquid is still hot; washing is performed; filtering residues are put into a flask; a proper amount of water is added; then, ultrasonic wave assistance hot reflux extraction is performed again; filtering is performed when the liquid is still hot; the operations are repeated for four times; obtained filter liquid and washing liquid are merged; through rotary evaporation, a target product, namely the dendrobium huoshanense polysaccharide is obtained. The extraction method of the dendrobium huoshanense polysaccharide provided by the invention has the advantages that the content of the obtained polysaccharide is high; the extraction time is short; the extraction is thorough; the extraction method is suitable for industrial application.
Description
Technical field
The present invention relates to the extracting method of a kind of Herba Dendrobii polysaccharide.
Background technology
Herba Dendrobii is the orchid family Dendrobium Sw, is a kind of rare medicinal herbs in China's traditional medicine, and its effective ingredient is predominantly
Polysaccharide and alkaloid, wherein, it is how many that the quality of Herba Dendrobii depends greatly on the content of polysaccharide in Herba Dendrobii.And Herba Dendrobii
In the most famous with Herba Dendrobii, the pharmacological action of Herba Dendrobii polysaccharide is mainly manifested in immunity, strong, defying age, antitumor
Deng effect.Along with social development, people are more and more higher to healthy concern, and its demand also can be increasing, but tradition Huoshan
The extracting method of dendrobium polysaccharide is to extract gained with plants such as the root of Herba Dendrobii platymiscium, stem, leaves, this technique gained
Product can not meet the future market demand to Herba Dendrobii intensive processing.Although, along with the development of science and technology,
The processing method occurring in that many Herba Dendrobii, but have little effect, therefore research emphasis revert to again from Herba Dendrobii coarse powder
As much as possible polysaccharide component is extracted in this viewpoint.Therefore a kind of efficient, Herba Dendrobii polysaccharide of high yield is developed
Class extracting method is the most significant.
It is indefinite to there is material base in the research of dendrobium polysaccharide at present, the frauds such as quality is uncontrollable, and separation purifying technique is coarse
End.
A kind of Dendrobium nobile polysaccharide recorded by No. 200810162496.7 prospectus of Chinese invention patent application
The preparation method of extract, affiliated Dendrobium nobile polysaccharide extract through defat, extraction, precipitate with ethanol, removing protein, except monosaccharide and oligosaccharide,
The steps such as gel column purification realize, polyoses content more than 90% in gained polyoses extract, but the method operation complexity, technique
Various, the used time is longer, is not suitable for industrial applications.
A kind of hypoglycemic activity has been recorded in No. 200810162496.7 prospectus of Chinese invention patent application
Dendrobium polysaccharide and extracting method thereof, select the dry Herba Dendrobii pulverized, add the water of its 20 ~ 40 times of weight, cellulase addition
Being 10 ~ 20g/mg, enzymolysis PH is 4.5 ~ 5.5, first uses the collaborative extraction of ultrasound wave-enzymolysis, and hydrolysis temperature 45 ~ 55 DEG C, during extraction
Between obtain dendrobium polysaccharide extracting solution after 10 ~ 20min, then the enzyme denaturing that heats up, present invention process is simple, the used time is short, improves Herba Dendrobii many
The yield of sugar and purity, but used by the method, cellulose enzyme amount is more, and PH is 4.5 ~ 5.5 structures that can affect polysaccharide, is not suitable for
Industrial applications.
Summary of the invention
For defect of the prior art, it is an object of the invention to provide the extracting method of a kind of Herba Dendrobii polysaccharide, institute
Obtaining polyoses content high, extraction time is short, and extraction comparison is thorough, is suitable for industrial applications.
The present invention solves technical problem and adopts the following technical scheme that
The present invention relates to the extracting method of a kind of Herba Dendrobii polysaccharide, comprise the steps:
(1) in the flask that apparatus,Soxhlet's is connected, add 100mL ether, 5g Herba Dendrobii coarse powder is placed in apparatus,Soxhlet's, adds
Hot reflux 0.5 ~ 6h, takes out Herba Dendrobii coarse powder；
(2) above-mentioned Herba Dendrobii coarse powder is added in 500mL flask, adds methanol in right amount, by ultrasonic wave added circumfluence distillation 20 ~
100min, filtered while hot, washing；
(3) filtering residue is placed in flask, adds water appropriate, then through ultrasonic wave added circumfluence distillation 20 ~ 100min, filtered while hot, weight
Operation 4 times again, merge the filtrate obtained and washing liquid, through rotary evaporation, obtain target product Herba Dendrobii polysaccharide.
Preferably, described apparatus,Soxhlet's uses heating in water bath.
Preferably, described bath temperature controls at 70 ~ 80 DEG C, most preferably 72 ~ 75 DEG C.
Preferably, described heating in water bath 0.5 ~ 6h, most preferably 3 ~ 4h.
Preferably, the addition of described methanol is 50 ~ 150mL, most preferably 80 ~ 120mL.
Preferably, in described (2), ultrasonic wave added return time is 20 ~ 100min, most preferably 25 ~ 35min.
Preferably, described (2) reflux temperature is 60 ~ 80 DEG C, most preferably 65 ~ 70 DEG C.
Preferably, the addition of described water is 50 ~ 150mL, most preferably 80 ~ 120mL.
Preferably, in described (3), ultrasonic wave added return time is 20 ~ 100min, most preferably 25 ~ 35min.
Preferably, described (3) reflux temperature is 90 ~ 120 DEG C, most preferably 95 ~ 110 DEG C.
Compared with prior art, the present invention has a following beneficial effect:
The extracting method gained polyoses content of described Herba Dendrobii polysaccharide is high, and extraction time is short, and extraction comparison is thorough, is suitable for industry
Change application.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.These embodiments are merely to illustrate the present invention and need not
In limiting the scope of the present invention.
Embodiment 1:
Adding 100mL ether in the flask that apparatus,Soxhlet's is connected, be placed in apparatus,Soxhlet's by 5g Herba Dendrobii coarse powder, water-bath adds
Heat, controls temperature 72 ~ 75 DEG C, is heated to reflux 3h, takes out Herba Dendrobii coarse powder；Herba Dendrobii coarse powder is added in 500mL flask, add
100mL methanol, temperature controls at about 65 DEG C, ultrasonic wave added circumfluence distillation 25min, filtered while hot, and washs 2 with methanol
Secondary；Being placed in flask by filtering residue, add water 100mL, in about 100 DEG C through ultrasonic wave added circumfluence distillation 25min, and filtered while hot,
And repetitive operation 4 times, the filtrate obtained and washing liquid are merged, rotary evaporation goes out solvent, obtains target product Herba Dendrobii many
Sugar 1.022g, yield 20.44%.
Embodiment 2:
Adding 100mL ether in the flask that apparatus,Soxhlet's is connected, be placed in apparatus,Soxhlet's by 5g Herba Dendrobii coarse powder, water-bath adds
Heat, controls temperature 72 ~ 75 DEG C, is heated to reflux 1h, takes out Herba Dendrobii coarse powder；Herba Dendrobii coarse powder is added in 500mL flask, add
100mL methanol, temperature controls at about 65 DEG C, ultrasonic wave added circumfluence distillation 25min, filtered while hot, and washs 2 with methanol
Secondary；Being placed in flask by filtering residue, add water 100mL, in about 100 DEG C through ultrasonic wave added circumfluence distillation 25min, and filtered while hot,
Repetitive operation 4 times, merges the filtrate obtained and washing liquid, and rotary evaporation goes out solvent, obtains target product Herba Dendrobii polysaccharide
0.925g, yield 18.50%.
Embodiment 3:
Adding 100mL ether in the flask that apparatus,Soxhlet's is connected, be placed in apparatus,Soxhlet's by 5g Herba Dendrobii coarse powder, water-bath adds
Heat, controls temperature 72 ~ 75 DEG C, is heated to reflux 5h, takes out Herba Dendrobii coarse powder；Herba Dendrobii coarse powder is added in 500mL flask, add
100mL methanol, temperature controls at about 65 DEG C, ultrasonic wave added circumfluence distillation 25min, filtered while hot, and washs 2 with methanol
Secondary；Being placed in flask by filtering residue, add water 100mL, in about 100 DEG C through ultrasonic wave added circumfluence distillation 25min, and filtered while hot,
Repetitive operation 4 times, merges the filtrate obtained and washing liquid, and rotary evaporation goes out solvent, obtains target product Herba Dendrobii polysaccharide
1.026g, yield 20.52%.
Embodiment 4:
Adding 100mL ether in the flask that apparatus,Soxhlet's is connected, be placed in apparatus,Soxhlet's by 5g Herba Dendrobii coarse powder, water-bath adds
Heat, controls temperature 72 ~ 75 DEG C, is heated to reflux 3h, takes out Herba Dendrobii coarse powder；Herba Dendrobii coarse powder is added in 500mL flask, add 50mL
Methanol, temperature controls at about 65 DEG C, ultrasonic wave added circumfluence distillation 25min, filtered while hot, and washs 2 times with methanol；Will filter
Slag is placed in flask, and add water 100mL, in about 100 DEG C through ultrasonic wave added circumfluence distillation 25min, filtered while hot, repetitive operation
4 times, the filtrate obtained and washing liquid being merged, rotary evaporation goes out solvent, obtains target product Herba Dendrobii polysaccharide 0.935g, receives
Rate 18.70%
Embodiment 5:
Adding 100mL ether in the flask that apparatus,Soxhlet's is connected, be placed in apparatus,Soxhlet's by 5g Herba Dendrobii coarse powder, water-bath adds
Heat, controls temperature 72 ~ 75 DEG C, is heated to reflux 3h, takes out Herba Dendrobii coarse powder；Herba Dendrobii coarse powder is added in 500mL flask, add
150mL methanol, temperature controls at about 65 DEG C, ultrasonic wave added circumfluence distillation 25min, filtered while hot, and washs 2 with methanol
Secondary；Being placed in flask by filtering residue, add water 100mL, in about 100 DEG C through ultrasonic wave added circumfluence distillation 25min, and filtered while hot,
Repetitive operation 4 times, merges the filtrate obtained and washing liquid, and rotary evaporation goes out solvent, obtains target product Herba Dendrobii polysaccharide
0.993g, yield 19.86%
Embodiment 6:
Adding 100mL ether in the flask that apparatus,Soxhlet's is connected, be placed in apparatus,Soxhlet's by 5g Herba Dendrobii coarse powder, water-bath adds
Heat, controls temperature 72 ~ 75 DEG C, is heated to reflux 3h, takes out Herba Dendrobii coarse powder；Herba Dendrobii coarse powder is added in 500mL flask, add
100mL methanol, temperature controls at about 80 DEG C, ultrasonic wave added circumfluence distillation 25min, filtered while hot, and washs 2 with methanol
Secondary；Being placed in flask by filtering residue, add water 100mL, in about 100 DEG C through ultrasonic wave added circumfluence distillation 25min, and filtered while hot,
Repetitive operation 4 times, merges the filtrate obtained and washing liquid, and rotary evaporation goes out solvent, obtains target product Herba Dendrobii polysaccharide
0.985g, yield 19.71%.
Embodiment 7:
The preparation process of the present embodiment is with embodiment 1, and except for the difference that adding the reflux extracting time after methanol is 100min, separates
Obtain target product Herba Dendrobii polysaccharide 0.988g, yield 19.76%.
Embodiment 8:
The preparation process of the present embodiment is with embodiment 1, and except for the difference that the addition of water is 50mL, isolated target product Huoshan
Dendrobium polysaccharide 0.861g, yield 17.22%
Embodiment 9:
The preparation process of the present embodiment is with embodiment 1, and except for the difference that adding the reflux extracting time after water is 100min, separates
To target product Herba Dendrobii polysaccharide 0.945g, yield 18.91%
As same materials carried out separating-purifying according to conventional purification methods, its process is as follows:
Weighing dry Herba Dendrobii powder 5g and add the 75%(V/V of 4 times of quality) to extract 48 little for the stirring of ethanol water merceration
Time, recycle 45 micrometer Millipore filter membranes and gained Herba Dendrobii lixiviating solution is carried out sucking filtration, filtrate is carried out 8000rpm high speed centrifugation
30 minutes, it is thus achieved that supernatant and precipitation；Dissolve described precipitation adds 3 times amount distilled water, boil 10 minutes in 100 DEG C,
8000rpm high speed centrifugation 30 minutes after cooling, it is thus achieved that supernatant and precipitation；Further supernatant is carried out rotary evaporation concentration,
It is dried again to constant weight, it is thus achieved that solubility Herba Dendrobii polysaccharide powder.The weight weighing the Herba Dendrobii polysaccharide obtained is 0.828g, receives
Rate is 16.57%.
Being extracted by above-mentioned contrast, the judgement Herba Dendrobii of the present invention Polyose extraction method institute that can will be apparent from is much
Sugar yield can have preferable application prospect close to the extracting method of the most conventional Herba Dendrobii polysaccharide.
Above the specific embodiment of the present invention is described.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformation or amendment within the scope of the claims, this not shadow
Ring the flesh and blood of the present invention.
Claims (10)
1. the extracting method of a Herba Dendrobii polysaccharide, it is characterised in that: comprise the steps:
(1) adding Herba Dendrobii coarse powder and solvent in the flask that apparatus,Soxhlet's is connected, wherein both additional proportions are that Herba Dendrobii is thick
Powder: ether is 5g:100ml, is heated to reflux 0.5 ~ 6h, takes out Herba Dendrobii coarse powder；
(2) above-mentioned Herba Dendrobii coarse powder is added in flask, add methanol, by ultrasonic wave added circumfluence distillation 20 ~ 100min, take advantage of
Heat filtering, washing；
(3) filtering residue is placed in flask, adds water appropriate, then through ultrasonic wave added circumfluence distillation 20 ~ 100min, filtered while hot, weight
Operation 4 times again, merge the filtrate obtained and washing liquid, through rotary evaporation, obtain target product Herba Dendrobii polysaccharide.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (1), Soxhlet
Extractor uses heating in water bath, and described bath temperature controls at 70 ~ 80 DEG C, and it is 0.5 ~ 6 hour that described water-bath adds the time.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 2, it is characterised in that: described bath temperature controls
72~75℃。
The extracting method of Herba Dendrobii polysaccharide the most according to claim 2, it is characterised in that: the described heating in water bath time is
3 ~ 4 hours.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (2), methanol
The volume that adds be 10 ~ 30 times of Herba Dendrobii meal quality, most preferably 16 ~ 24 times.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (2), ultrasonic
The auxiliary reflux time is 25 ~ 35min.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (2), backflow
Temperature is 65 ~ 70 DEG C.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (3), water
Addition volume is 16 ~ 24 times of Herba Dendrobii meal quality.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (3), ultrasonic
The auxiliary reflux time is 25 ~ 35min.
The extracting method of Herba Dendrobii polysaccharide the most according to claim 1, it is characterised in that: in described step (3), return
Stream temperature is 95 ~ 110 DEG C.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632539A (en) * | 2016-11-03 | 2017-05-10 | 明光市大全甜叶菊专业合作社 | A stevia rebaudiana glucoside extracting method |
| CN108191990A (en) * | 2017-12-29 | 2018-06-22 | 贺州市星辉科技有限公司 | The method of ultrasonic extraction method Dendrobium officinale polysaccharide |
| CN108314744A (en) * | 2018-01-12 | 2018-07-24 | 浙江寿仙谷医药股份有限公司 | A kind of method of rapid extraction Dendrobium officinale polysaccharide |
| CN108341887A (en) * | 2018-03-14 | 2018-07-31 | 漯河中德双成功能食品研究院有限公司 | A kind of preparation method of Dendrobidium huoshanness polysaccharide |
| CN109393319A (en) * | 2018-11-29 | 2019-03-01 | 靖州康源苓业发展有限公司 | A kind of preparation method of tuckahoe health care niblet |
| CN111285940A (en) * | 2020-04-08 | 2020-06-16 | 安徽霍山麟鼎轩生物科技有限公司 | Method for extracting and purifying dendrobium huoshanense active polysaccharide |
| CN111690076A (en) * | 2020-06-22 | 2020-09-22 | 浙江亚林生物科技股份有限公司 | Dendrobium pectin extraction process method |
| CN115607628A (en) * | 2022-10-20 | 2023-01-17 | 浙江长典药物技术开发有限公司 | Dendrobium candicum fluid extract, preparation process and equipment thereof |
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2016
- 2016-07-30 CN CN201610611390.5A patent/CN106046194A/en not_active Withdrawn
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106632539A (en) * | 2016-11-03 | 2017-05-10 | 明光市大全甜叶菊专业合作社 | A stevia rebaudiana glucoside extracting method |
| CN108191990A (en) * | 2017-12-29 | 2018-06-22 | 贺州市星辉科技有限公司 | The method of ultrasonic extraction method Dendrobium officinale polysaccharide |
| CN108314744A (en) * | 2018-01-12 | 2018-07-24 | 浙江寿仙谷医药股份有限公司 | A kind of method of rapid extraction Dendrobium officinale polysaccharide |
| CN108314744B (en) * | 2018-01-12 | 2020-10-16 | 浙江寿仙谷医药股份有限公司 | Method for rapidly extracting dendrobium officinale polysaccharide |
| CN108341887A (en) * | 2018-03-14 | 2018-07-31 | 漯河中德双成功能食品研究院有限公司 | A kind of preparation method of Dendrobidium huoshanness polysaccharide |
| CN108341887B (en) * | 2018-03-14 | 2020-08-07 | 河南夕阳蓝食品科技有限公司 | Preparation method of dendrobium huoshanense polysaccharide |
| CN109393319A (en) * | 2018-11-29 | 2019-03-01 | 靖州康源苓业发展有限公司 | A kind of preparation method of tuckahoe health care niblet |
| CN111285940A (en) * | 2020-04-08 | 2020-06-16 | 安徽霍山麟鼎轩生物科技有限公司 | Method for extracting and purifying dendrobium huoshanense active polysaccharide |
| CN111690076A (en) * | 2020-06-22 | 2020-09-22 | 浙江亚林生物科技股份有限公司 | Dendrobium pectin extraction process method |
| CN115607628A (en) * | 2022-10-20 | 2023-01-17 | 浙江长典药物技术开发有限公司 | Dendrobium candicum fluid extract, preparation process and equipment thereof |
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Application publication date: 20161026 |