CN106317241B - The isolation and purification method and products thereof of polysaccharide in a kind of Gorgon euryale pericarp - Google Patents
The isolation and purification method and products thereof of polysaccharide in a kind of Gorgon euryale pericarp Download PDFInfo
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- CN106317241B CN106317241B CN201610725273.1A CN201610725273A CN106317241B CN 106317241 B CN106317241 B CN 106317241B CN 201610725273 A CN201610725273 A CN 201610725273A CN 106317241 B CN106317241 B CN 106317241B
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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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- 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
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
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- Polysaccharides And Polysaccharide Derivatives (AREA)
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Abstract
The invention discloses a kind of isolation and purification methods and products thereof of polysaccharide in Gorgon euryale pericarp, select fresh, nothing to rot, the Gorgon fruit pericarp of no disease and pests harm, remove the solid impurity in Gorgon euryale pericarp, the silt on cleaning removal Gorgon euryale pericarp；The water of 10 20 times of amounts is added in the Gorgon euryale pericarp cleaned out（v/w）, it is homogenized and obtains homogenate；Through filter cloth, press filtration detaches step by step, removes residue, collects filtrate；Selective retention molecular weight filtrate collected by the ultrafiltration membrance filter of 3000Da or more, takes retention part on film, you can obtains Gorgon euryale pericarp polysaccharide concentrate；It is freeze-dried to obtain Gorgon euryale pericarp polyose；Purity of polysaccharide is creamy white powdered 90% or more in the product.Purity of polysaccharide shows high water imbibition 90% or more in gained Gorgon euryale pericarp polysaccharide sample（51.30 g/g）, oil absorption（1.14 g/g）And stronger anti-oxidation characteristics.
Description
Technical field
The present invention relates to field of food, and in particular to the isolation and purification method and products thereof of polysaccharide in a kind of Gorgon euryale pericarp.
Background technology
Gorgon fruit is a kind of mature seed kernel of water plant Gorgon euryale, is commonly called as " Gorgon fruit ", is one of China's traditional Chinese medicine, and
One of " dietotherapeutic " material that the Ministry of Public Health of China promulgates in the first batch.Gorgon fruit has a plurality of health care functions, such as " Gorgon euryale can quench the thirst kidney-nourishing,
It controls under urinary incontinence, seminal emission, gonorrhoea, band "（《Compendium of Materia Medica》）, Gorgon fruit has effects that " tonifying spleen, is reinforced the kidney at dampness removing "（《Book on Chinese herbal medicine is asked
Very》）.Gorgon fruit plant is very large, and main edible part is Gorgon fruit benevolence, and benevolence is coated in fruit.Its fruit divides spinosity（North
Gorgon euryale, wild species）With it is stingless（Gordon euryale seed or Soviet Union Gorgon euryale）Two types generally comprise dozens of to hundreds of Gorgon fruit kinds in each fruit
Son.Wherein Soviet Union's Gorgon euryale fruit is very big, after taking seed, will produce the by-products such as a large amount of pericarp and its internal spongioplasm diaphragm.
In Gorgon fruit producing region, these by-products are generally discarded, untapped utilization.
Currently, the processing and utilization to Gorgon fruit resource is also limited only to Gorgon fruit benevolence.Annual country's Gorgon fruit kernel yield is about
Ten thousand tons of 8-10, wherein 10%-15% is used as Chinese medicine, remaining is for nourishing food materials.Relative to Gorgon fruit benevolence, including Gorgon fruit kind
The yield of the by-products such as shell, tender stem, pericarp is far above Gorgon euryale benevolence.But this part resource is not all utilized substantially at present, such as
Gorgon euryale pericarp, yield are 2-3 times of Gorgon euryale benevolence quantity, are enriched the study found that containing in Gorgon fruit pericarp this Research Team early period
Polysaccharide.The polysaccharide is a kind of non-starch polysaccharide, water-soluble high, shows multiple functions characteristic, great developing and utilizingpotentiality.
End on July 9th, 2016, from Chinese scientific journal database（CNKI）In retrieve the text in relation to Gorgon fruit polysaccharide altogether
Offer totally 16（Table 1）, the Gorgon fruit polysaccharide in document in table 1 extracts from Semen Euryales without exception, is related to non-starch
Polysaccharide or starch-polysaccharides, and extracting method is mostly the method for water extract-alcohol precipitation.Gorgon euryale pericarp is the Main By product in Gorgon fruit production,
It not yet utilizes at present.
The Gorgon fruit polysaccharide pertinent literature that table 1 is collected from CNKI databases
.Invention content
The technical issues of solution：Present invention aims at Gorgon fruit comprehensive resource utilization rate is improved, a kind of water extraction knot is provided
The Gorgon euryale pericarp separation of polysaccharides purification process of membrane filtration is closed, and the functional character of the polysaccharide is further analyzed, is developed a kind of new
Gorgon euryale pericarp polyose, the polyose have high water imbibition（51.30 g/g）, oil absorption（1.14 g/g）And it is total
Reducing power（Fig. 1）.Sample extraction rate is in 1 documents 8 of table 4% or more（0.62 mg/g）Nearly 100 times.
To achieve the goals above, the technical solution that the present invention takes is：
The isolation and purification method of polysaccharide, preparation process include in a kind of Gorgon euryale pericarp：The cleaning of Gorgon fruit pericarp plus water are even
Slurry, slag liquid 5 process procedures such as press filtration separation, membrane filtration, freeze-drying step by step.
It is as follows：
（1）The cleaning of Gorgon fruit pericarp：Fresh, nothing is selected to rot, the Gorgon fruit pericarp of no disease and pests harm, manual cleaning removed before this
Solid impurity in Gorgon euryale pericarp, then with clean water, the silt on cleaning removal Gorgon euryale pericarp；
（2）Water is added to be homogenized：The Gorgon euryale pericarp cleaned out is taken, is put into refiner, is added what 10-20 times of Gorgon euryale pericarp quality was measured
Water（g/mL）, homogenate；
（3）Press filtration detaches slag liquid step by step：It will（2）Gained homogenate, removes residue, collects final filtrate step by step in step, this
For Gorgon euryale pericarp polysaccharide extraction liquid；
（4）Membrane filtration：Ultrafiltration membrance filter of the selective retention molecular weight in 3000Da or more（3）In collected filtrate, take
Retention part on film, you can obtain Gorgon euryale pericarp polysaccharide concentrate；
（5）Freeze-drying：It will（4）Middle gained Gorgon euryale pericarp polysaccharide concentrate is freeze-dried to obtain the production of Gorgon euryale pericarp polysaccharide
Product, purity of polysaccharide is creamy white powdered 90% or more in the product, free from extraneous odour.
As preferably, step（2）It is middle to use Y18 type high-speed homogenizations machine interval, multiple homogenized, 1- per treatment
2min（15000r/min）, interval 1-2min, continuous homogenized 3-4 times.
As preferably, step（3）Described in step by step press filtration separation be that homogenate is passed sequentially through into the mesh filter of 100 mesh ~ 500
Cloth press filtration detaches.Such as it can make to use 100 mesh, 200 mesh, 300 mesh, 500 mesh filter cloth press filtrations successively.
As preferably, step（4）Selective retention molecular weight is in the ultrafiltration membrane of 3000Da or more, wheel speed 600-
800 r/min, operating pressure 0.06-1.0Mpa.
The polysaccharide extraction liquid in Gorgon euryale pericarp can be obtained by " adding water homogenate, slag liquid, press filtration detaches step by step "；By " film mistake
Filter " link, can be obtained Gorgon euryale pericarp polysaccharide purification liquid, and polysaccharide concentration is improved 2-4 times, improve Polyose extraction efficiency, saving at
This.
Using above-mentioned technique, polyose can be extracted from fresh Gorgon euryale pericarp, in the product purity of polysaccharide 90% with
On, it is creamy white powdered, free from extraneous odour.Sample yield is 4% or more.Gained polysaccharide sample is analyzed through gel column chromatography, the polysaccharide
Average molecular weight is in 3700-12500, and structural unit is based on galactolipin and glucose.
There are following differences for the Gorgon fruit polysaccharide that the present invention extracts and these documents enumerated in table 1：（1）Source is not
Together, districts and cities extract from Semen Euryales without exception for Gorgon fruit polysaccharide in the document in table 1, are related to non-starch polysaccharide or starch
Polysaccharide.And described Gorgon fruit polysaccharide is extracted from the pericarp of Gorgon euryale fruit in the present invention, pericarp is the main pair in Gorgon fruit production
Product not yet utilizes at present.（2）Characteristic is different, and the recovery rate of the carried Gorgon fruit polysaccharide of 1 Literature of table is very low, only 0.62 mg/g
（Zhao Xuan etc.）, and not about the water imbibition of Gorgon fruit polysaccharide, oil absorption data in contrast material, only antioxidant properties and anti-tired
The characteristics such as labor.The recovery rate of the extracted Gorgon fruit polysaccharide of this patent is 4% or more（It is equivalent to 40mg/g or more）, far above comparison material
Material, in addition, Gorgon fruit polysaccharide obtained by this patent has high water imbibition（51.30 g/g）, oil absorption（1.14 g/g）And compared with
Strong anti-oxidation characteristics（Light absorption value when 0.4mg/ml under 700nm wavelength is 1.2）（Fig. 1）, far above contrast material in table 1
10（Li Xiangli etc.）In total reducing power（Light absorption value when 0.4mg/ml is about 0.2）.（3）Extracting method is different.This patent Gorgon euryale
Real polysaccharide, which is adopted, to be extracted with water in conjunction with membrane filtering method, and the method that contrast material mostly uses greatly water extract-alcohol precipitation in table 1.
Therefore, this patent method extraction gained Gorgon euryale pericarp polysaccharide is totally different from all Gorgon fruit polysaccharide in table 1, is a kind of
Novel polysaccharide.
Advantageous effect：
The present invention from Gorgon euryale pericarp largely discarded in Gorgon fruit production and processing cleaned, homogenate, slag liquid step by step press filtration separation,
The techniques such as membrane filtration and freeze-drying extract a kind of novel Gorgon euryale pericarp polysaccharide, and sample yield is in 4%-12%.The technological process is simple,
It is perfect, be easy to industrialization processing.
Gained Gorgon euryale pericarp purity of polysaccharide is creamy white powdered 90% or more, free from extraneous odour.It is analyzed through gel column chromatography, it should
Polysaccharide average molecular weight is in 3700-12500, and structural unit is based on galactolipin and glucose.Antioxidation in vitro property analysis knot
Fruit shows that the polysaccharide has very strong antioxidation activity in vitro（Fig. 1, using potassium ferricyanide colorimetric method, wavelength 700nm）With it is high
Water imbibition（51.30 g/g adsorb centrifugal process）, oil absorption（1.14 g/g adsorb centrifugal process）, other functional character analyses
It need to be furtherd investigate.
Description of the drawings
Fig. 1 is the total reducing power of Gorgon euryale pericarp polysaccharide of the present invention；
Fig. 2 is that Gorgon euryale pericarp separation of polysaccharides of the present invention purifies flow chart.
Specific implementation mode
Following embodiment is technique in order to preferably explain the present invention, is not intended as the limitation to present invention process.
Ultrafiltration membrane
Embodiment 1
The isolation and purification method of polysaccharide, includes the following steps in a kind of Gorgon euryale pericarp：
（1）The cleaning of Gorgon fruit pericarp：Fresh, nothing is selected to rot, the Gorgon fruit pericarp of no disease and pests harm, manual cleaning removed before this
Solid impurity in Gorgon euryale pericarp, then with clean water, the silt on cleaning removal Gorgon euryale pericarp；
（2）Water is added to be homogenized：The Gorgon euryale pericarp that 500 g are cleaned out is taken, refiner is put into（Y18 types, Shanghai wing Simple-minded）It is interior, add 5
L deionized waters are homogenized 1min（15000 r/min）, 1 min of interval, continuous homogenized 3 times；
（3）Press filtration detaches slag liquid step by step：It will（2）Gained homogenate in step, uses 100 mesh, 200 mesh, 300 mesh, 500 successively
Mesh filter cloth press filtration（Pressure）, residue is removed step by step, collects final filtrate, this is Gorgon euryale pericarp polysaccharide extraction liquid；
（4）Membrane filtration：Selective retention molecular weight is in 5000 Da ultrafiltration membrance filters（3）In collected filtrate, take on film cut
Stay part（600 r/min of wheel speed, 0.08 Mpa of operating pressure）, you can obtain 1.2 L of Gorgon euryale pericarp polysaccharide concentrate；
（5）Freeze-drying：It will（4）1.2 L Gorgon euryale pericarp polysaccharide concentrates of middle gained are freeze-dried（- 55 DEG C, 32 h）
Obtaining 25.8 g of Gorgon euryale pericarp polyose, recovery rate 5.16%, purity of polysaccharide is creamy white powdered 91.21% in the product,
Free from extraneous odour.
The Gorgon euryale pericarp polysaccharide of gained is analyzed, polysaccharide sample is analyzed through gel column chromatography, the polysaccharide average molecular weight
Between 6800-9680, using sour water solution combination high performance liquid chromatography（HPLC）Its structural unit is analyzed with galactolipin and grape
Based on sugar.Use its total reducing power of potassium ferricyanide colorimetric method for determining for 1.24（0.4 mg/ml, 700 nm of wavelength）, have high
Water imbibition（52.32 g/g）And oil absorption（1.18 g/g）.
Embodiment 2
The isolation and purification method of polysaccharide, includes the following steps in a kind of Gorgon euryale pericarp：
（1）The cleaning of Gorgon fruit pericarp：Fresh, nothing is selected to rot, the Gorgon fruit pericarp of no disease and pests harm, manual cleaning removed before this
Solid impurity in Gorgon euryale pericarp, then with clean water, the silt on cleaning removal Gorgon euryale pericarp；
（2）Water is added to be homogenized：The Gorgon euryale pericarp that 1000 g are cleaned out is taken, refiner is put into（Y18 types, Shanghai wing Simple-minded）It is interior, add
12 L deionized waters are homogenized 1min（15000 r/min）, 1 min of interval, continuous homogenized 3 times；
（3）Press filtration detaches slag liquid step by step：It will（2）Gained homogenate in step, uses 100 mesh, 200 mesh, 300 mesh, 500 successively
Mesh filter cloth press filtration（Pressure）, residue is removed step by step, collects final filtrate, this is Gorgon euryale pericarp polysaccharide extraction liquid；
（4）Membrane filtration：Selective retention molecular weight is in 8000 Da ultrafiltration membrance filters（3）In collected filtrate, take on film cut
Stay part（800 r/min of wheel speed, 0.1 Mpa of operating pressure）, you can obtain 2.5 L of Gorgon euryale pericarp polysaccharide concentrate；
（5）Freeze-drying：It will（4）2.5 L Gorgon euryale pericarp polysaccharide concentrates of middle gained are freeze-dried（- 55 DEG C, 40 h）
Obtain 48.72 g of Gorgon euryale pericarp polyose, recovery rate 4.87%, purity of polysaccharide is 93.63% in the product, and be creamy white powder
Shape, free from extraneous odour.
The Gorgon euryale pericarp polysaccharide of gained is analyzed, polysaccharide sample is analyzed through gel column chromatography, the polysaccharide average molecular weight
Between 7800-1030, using sour water solution combination high performance liquid chromatography（HPLC）Its structural unit is analyzed with galactolipin and grape
Based on sugar.Use its total reducing power of potassium ferricyanide colorimetric method for determining for 1.54（0.4mg/ml, wavelength 700nm）, have high
Water imbibition（58.14 g/g）And oil absorption（1.72 g/g）.
Claims (7)
1. the isolation and purification method of polysaccharide in a kind of Gorgon euryale pericarp, which is characterized in that include the following steps：
1）The cleaning of Gorgon fruit pericarp：Fresh, nothing is selected to rot, the Gorgon fruit pericarp of no disease and pests harm, the solid removed in Gorgon euryale pericarp is miscellaneous
Matter, cleaning remove the silt on Gorgon euryale pericarp；
2）Water is added to be homogenized：Take step 1）The Gorgon euryale pericarp cleaned out, is added Gorgon euryale 10-20 times of water measured of pericarp quality, and homogenate obtains
Homogenate；
3）Press filtration detaches slag liquid step by step：By step 2）Middle gained homogenate, through filter cloth, press filtration detaches step by step, removes residue, collects
Filtrate；
4）Membrane filtration：Ultrafiltration membrance filter step 3 of the selective retention molecular weight in 3000Da or more）Collected filtrate, takes on film
Retention part, you can obtain Gorgon euryale pericarp polysaccharide concentrate；
5）Freeze-drying：By step 4）Middle gained Gorgon euryale pericarp polysaccharide concentrate is freeze-dried to obtain Gorgon euryale pericarp polyose；
Purity of polysaccharide is creamy white powdered 90% or more in the product.
2. the isolation and purification method of polysaccharide in a kind of Gorgon euryale pericarp according to claim 1, it is characterised in that：Step 2）Using
High-speed homogenization machine interval, multiple homogenized, 1-2min per treatment, rotating speed 15000r/min, interval 1-2min are continuous to be homogenized
Processing 3-4 times.
3. the isolation and purification method of polysaccharide in a kind of Gorgon euryale pericarp according to claim 1, it is characterised in that：Step 3）Middle institute
It is that homogenate is passed sequentially through the mesh filter cloth press filtration separation of 100 mesh ~ 500 to state the separation of press filtration step by step.
4. the isolation and purification method of polysaccharide in a kind of Gorgon euryale pericarp according to claim 1, it is characterised in that：Step 4）In,
Selective retention molecular weight is in the ultrafiltration membrane of 3000Da or more, wheel speed 600-800 r/min, operating pressure 0.06-1.0Mpa.
5. the isolation and purification method of polysaccharide in a kind of Gorgon euryale pericarp according to claim 1, it is characterised in that：Step 5）In it is cold
Dry use vacuum freeze drier is lyophilized and is first freeze-dried 24-36 h at -55 DEG C.
6. a kind of Gorgon euryale pericarp polysaccharide is isolated using any one of claim 1 ~ 5 isolation and purification method.
7. Gorgon euryale pericarp polysaccharide according to claim 6, it is characterised in that：90% or more, average molecular weight exists purity of polysaccharide
3700-12500, structural unit is based on galactolipin and glucose.
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Citations (3)
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|---|---|---|---|---|
| CN1916029A (en) * | 2006-08-22 | 2007-02-21 | 西南大学 | Method for purifying concentrated polysaccharide of male agaric by using isolation technique of composition filmes |
| CN102783694A (en) * | 2011-06-24 | 2012-11-21 | 滁州学院 | Method for extracting antioxidation active components from euryale seed shell |
| CN103275236A (en) * | 2013-05-31 | 2013-09-04 | 上海师范大学 | Preparation method of gorgon fruit polysaccharide extractive, and application thereof |
-
2016
- 2016-08-26 CN CN201610725273.1A patent/CN106317241B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1916029A (en) * | 2006-08-22 | 2007-02-21 | 西南大学 | Method for purifying concentrated polysaccharide of male agaric by using isolation technique of composition filmes |
| CN102783694A (en) * | 2011-06-24 | 2012-11-21 | 滁州学院 | Method for extracting antioxidation active components from euryale seed shell |
| CN103275236A (en) * | 2013-05-31 | 2013-09-04 | 上海师范大学 | Preparation method of gorgon fruit polysaccharide extractive, and application thereof |
Non-Patent Citations (2)
| Title |
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| In vitro Antioxidant Properties of Euryale ferox Seed Shell Extracts and their Preservation Effects on Pork Sausages;Cuan Zhang;《Journal of Food Processing and Preservation》;20140815;全文 * |
| 芡实的化学成分、药理作用及临床应用研究进展;刘琳 等;《中华中医药杂志》;20150228;第30卷(第2期);全文 * |
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