CN104448023B - A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae) - Google Patents

A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae) Download PDF

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CN104448023B
CN104448023B CN201410796637.6A CN201410796637A CN104448023B CN 104448023 B CN104448023 B CN 104448023B CN 201410796637 A CN201410796637 A CN 201410796637A CN 104448023 B CN104448023 B CN 104448023B
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thallus
thallus laminariae
thallus eckloniae
eckloniae
laminariae
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CN104448023A (en
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周冠旻
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GUILIN HEYINXIANG NEW MATERIALS Co Ltd
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GUILIN HEYINXIANG NEW MATERIALS Co Ltd
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Abstract

The invention discloses a kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae), comprise the steps: Feedstock treating, ultra high pressure treatment, ultrasonic Treatment, enzymolysis, purification, be drying to obtain finished product.The present invention, by using the combination of two kinds of extracting modes, on the one hand shortens extraction time, on the other hand improves product yield.

Description

A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae)
Technical field
The present invention relates to the extracting method of a kind of polysaccharide sulfate, be specifically related to a kind of extraction from Thallus Laminariae (Thallus Eckloniae) The method of polysaccharide sulfate.
Background technology
((Lam inaria Japonica Aresch) is Phaeophyta Laminariales Laminariaceae Larminaria to Thallus Laminariae (Thallus Eckloniae) Tangleweed.Kelp Rich composition Han several functions, has high edible and medical value.Many Saccharide compound is widely present in the cell wall of animal cell membrane and plant, microorganism, is by aldehyde radical With ketone group by the bonded high molecular polymer of glycoside, be also constitute life four big base substances it One.Over nearly 20 years, along with the i.e. analysis means that deepens continuously of Natural Medicine Chemistry, pharmacological research is dashed forward Flying the development pushed ahead vigorously, the research of polysaccharide causes the most much great interest of scholar.Research shows, Natural polysaccharide compounds has antitumor and immunological enhancement.Thus, immunity in natural animal-plant The important biomolecule effect of polysaccharide is the most increasingly subject to people's attention, and becomes the focus of current research. Found that laminarin had many biological activitys, such as immunomodulating, antitumor, anticoagulant in recent years Blood, blood fat reducing, blood sugar lowering, antioxidation etc..
Polysaccharide sulfate (sulfated polysaccharides, SPS) is also known as polysaccharide sulfate (PSS), It is that in polysaccharide macro-molecular chain, the hydroxyl on monosaccharide molecule is replaced by sulfate radical and formed natural or narrow The polysaccharide derivates become, is a water miscible acidic polysaccharose of class, for polyanionic compound, having Learn the features such as structure complexity, structure activity relationship distinctness, diverse biological activities.Such as red algae, Brown algae in Sargassum Deng all containing a large amount of polysaccharide sulfate.Many researchs in recent years find that polysaccharide sulfate has multiple physiology Activity, including regulation immunity, antioxidation, blood sugar lowering, blood fat reducing, protection kidney, anticoagulation, resists Tumor and antiviral etc..
Polysaccharide sulfate is mainly derived from natural extract or chemosynthesis.Extract the tradition of polysaccharide sulfate Common method mainly has acid to carry, alkali carries and carrying with water, wherein in the majority with hot water extraction, acid, alkaline extraction The structure of polysaccharide sulfate will be destroyed, the most also the content of sulfate radical can be produced impact;And hot water The extraction ratio of extraction is the most relatively low, it is difficult to meet Production requirement.
Summary of the invention
In order to overcome the deficiencies in the prior art, the invention provides a kind of extraction polysaccharide sulphuric acid from Thallus Laminariae (Thallus Eckloniae) The method of ester.
The present invention is achieved through the following technical solutions:
A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae), comprises the steps:
1) Feedstock treating: by Thallus Laminariae (Thallus Eckloniae), pulverizes or smashes;
2) ultra high pressure treatment: add the pure of 40-60 times of weight portion in the Thallus Laminariae (Thallus Eckloniae) after pulverizing or smashing Water, pressure 350MPa, operative temperature 70-85 DEG C, ultra high pressure treatment 2-5min, filter after completing, Collect filtrate;
3) ultrasonic Treatment: by step 2) obtain filtrate, ultrasonic Treatment 5-10min, action temperature Spending 70-85 DEG C, power is 300W, filters after completing, and collects filtrate;
4) enzymolysis: step 3) filtrate that obtains add after proteases for decomposing protein becomes aminoacid, First pass through the ultrafiltration membrance filter of molecular cut off 1000-3000, be concentrated into substance through NF membrane the most again Obtaining crude polysaccharides concentrated solution behind long-pending 1/5, wherein, the inventory of protease is Thallus Laminariae (Thallus Eckloniae) weight 0.8-1.0%, enzymolysis time is 6-8h;
5) adding ethanol to volume fraction in crude polysaccharides concentrated solution is 25-35%, static, centrifugal, from Heart liquid is concentrated into the 1/3-1/2 of original volume through NF membrane, and adding ethanol to volume fraction is 75-80%, Centrifugation, it is dried to obtain polysaccharide sulfate.
Thallus Laminariae (Thallus Eckloniae) of the present invention be fresh or drying after Thallus Laminariae (Thallus Eckloniae).
Compared with prior art, present invention have the advantage that
1, the present invention uses ultra high pressure treatment Thallus Laminariae (Thallus Eckloniae) raw material, keeps a period of time in predetermined pressure, makes former Material intraor extracellular pressure reaches to balance (effective ingredient reaches dissolution equilibrium) release rapidly afterwards, makes intracellular Exosmosis pressure differential increases suddenly, and through cell membrane, (structure of cell membrane exists intracellular effective ingredient Change under supertension), transfer in extracellular extracting solution, reach to extract the mesh of target component 's.Hyperpressure extraction avoid cause because of long-time high temperature the change of effective ingredient, loss and The reduction of physiologically active, simultaneously as supertension is carried out in the environment of airtight, does not has solvent Volatilization, will not be to environment.It it is a kind of method safely and effectively extracting active substance.
2, the present invention is after using ultra high pressure treatment raw material, uses ultrasonic extraction the most again, ultrasonic Ripple extraction and application is strong mechanical shearing effect, promotes the dissolution of polysaccharide sulfate, and the present invention is led to Cross the combination using two kinds of extracting modes, on the one hand shorten extraction time, on the other hand improve product Product yield, use the present invention method, polysaccharide sulfate content more than 98.5%, extraction ratio 75% with On.
Detailed description of the invention
With embodiment, the invention will be further described below, but the invention is not limited in that these are implemented Example.
Embodiment 1:
A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae), comprises the steps:
1) Feedstock treating: by the Thallus Laminariae (Thallus Eckloniae) 10kg after drying, pulverizes;
2) ultra high pressure treatment: add the pure water of 400kg in the Thallus Laminariae (Thallus Eckloniae) after pulverizing, pressure 350MPa, Operative temperature 85 DEG C, ultra high pressure treatment 4min, filters after completing, collects filtrate;
3) ultrasonic Treatment: by step 2) obtain filtrate, ultrasonic Treatment 10min, operative temperature 85 DEG C, power is 300W, filters after completing, and collects filtrate;
4) enzymolysis: step 3) filtrate that obtains add after proteases for decomposing protein becomes aminoacid, First pass through the ultrafiltration membrance filter of molecular cut off 1000-3000, be concentrated into substance through NF membrane the most again Obtaining crude polysaccharides concentrated solution behind long-pending 1/5, wherein, the inventory of protease is the 0.8% of Thallus Laminariae (Thallus Eckloniae) weight, Enzymolysis time is 6h;
5) adding ethanol to volume fraction in crude polysaccharides concentrated solution is 30%, static, centrifugal, centrifugal liquid Be concentrated into the 1/2 of original volume through NF membrane, adding ethanol to volume fraction is 75%, centrifugation, It is dried to obtain polysaccharide sulfate.
Embodiment 2:
A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae), comprises the steps:
1) Feedstock treating: by fresh Thallus Laminariae (Thallus Eckloniae) 10kg, smash;
2) ultra high pressure treatment: add the pure water of 600kg in the Thallus Laminariae (Thallus Eckloniae) after smashing, pressure 350MPa, Operative temperature 80 DEG C, ultra high pressure treatment 2min, filters after completing, collects filtrate;
3) ultrasonic Treatment: by step 2) obtain filtrate, ultrasonic Treatment 8min, operative temperature 80 DEG C, power is 300W, filters after completing, and collects filtrate;
4) enzymolysis: step 3) filtrate that obtains add after proteases for decomposing protein becomes aminoacid, First pass through the ultrafiltration membrance filter of molecular cut off 1000-3000, be concentrated into substance through NF membrane the most again Obtaining crude polysaccharides concentrated solution behind long-pending 1/5, wherein, the inventory of protease is the 1.0% of Thallus Laminariae (Thallus Eckloniae) weight, Enzymolysis time is 7h;
5) adding ethanol to volume fraction in crude polysaccharides concentrated solution is 35%, static, centrifugal, centrifugal liquid Be concentrated into the 1/3 of original volume through NF membrane, adding ethanol to volume fraction is 80%, centrifugation, It is dried to obtain polysaccharide sulfate.
Embodiment 3:
A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae), comprises the steps:
1) Feedstock treating: by the Thallus Laminariae (Thallus Eckloniae) 10kg after drying, pulverizes;
2) ultra high pressure treatment: add the pure water of 500kg in the Thallus Laminariae (Thallus Eckloniae) after pulverizing, pressure 350MPa, Operative temperature 70 DEG C, ultra high pressure treatment 5min, filters after completing, collects filtrate;
3) ultrasonic Treatment: by step 2) obtain filtrate, ultrasonic Treatment 5min, operative temperature 70 DEG C, power is 300W, filters after completing, and collects filtrate;
4) enzymolysis: step 3) filtrate that obtains add after proteases for decomposing protein becomes aminoacid, First pass through the ultrafiltration membrance filter of molecular cut off 1000-3000, be concentrated into substance through NF membrane the most again Obtaining crude polysaccharides concentrated solution behind long-pending 1/5, wherein, the inventory of protease is the 0.9% of Thallus Laminariae (Thallus Eckloniae) weight, Enzymolysis time is 8h;
5) adding ethanol to volume fraction in crude polysaccharides concentrated solution is 35%, static, centrifugal, centrifugal liquid Be concentrated into the 1/2 of original volume through NF membrane, adding ethanol to volume fraction is 80%, centrifugation, It is dried to obtain polysaccharide sulfate.
Result:

Claims (2)

1. the method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae), it is characterised in that include following step Rapid:
1) Feedstock treating: by Thallus Laminariae (Thallus Eckloniae), pulverizes or smashes;
2) ultra high pressure treatment: add the pure of 40-60 times of weight portion in the Thallus Laminariae (Thallus Eckloniae) after pulverizing or smashing Water, pressure 350MPa, operative temperature 70-85 DEG C, ultra high pressure treatment 2-5min, filter after completing, Collect filtrate;
3) ultrasonic Treatment: by step 2) obtain filtrate, ultrasonic Treatment 5-10min, action temperature Spending 70-85 DEG C, power is 300W, filters after completing, and collects filtrate;
4) enzymolysis: step 3) filtrate that obtains add after proteases for decomposing protein becomes aminoacid, First pass through the ultrafiltration membrance filter of molecular cut off 1000-3000, be concentrated into substance through NF membrane the most again Obtaining crude polysaccharides concentrated solution behind long-pending 1/5, wherein, the inventory of protease is Thallus Laminariae (Thallus Eckloniae) weight 0.8-1.0%, enzymolysis time is 6-8h;
5) adding ethanol to volume fraction in crude polysaccharides concentrated solution is 25-35%, static, centrifugal, from Heart liquid is concentrated into the 1/3-1/2 of original volume through NF membrane, and adding ethanol to volume fraction is 75-80%, Centrifugation, it is dried to obtain polysaccharide sulfate.
A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae) the most according to claim 1, its Be characterised by: described Thallus Laminariae (Thallus Eckloniae) be fresh or drying after Thallus Laminariae (Thallus Eckloniae).
CN201410796637.6A 2014-12-19 2014-12-19 A kind of method extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae) Expired - Fee Related CN104448023B (en)

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