CN102153669B

CN102153669B - Preparation method of low-molecule brown seaweed glucan

Info

Publication number: CN102153669B
Application number: CN 201010169739
Authority: CN
Inventors: 汤洁
Original assignee: BEIJING LEILI UNITED OCEAN BIOLOGICAL TECHNOLOGY CO LTD
Current assignee: BEIJING LEILI UNITED OCEAN BIOLOGICAL TECHNOLOGY CO LTD
Priority date: 2010-05-12
Filing date: 2010-05-12
Publication date: 2013-01-16
Anticipated expiration: 2030-05-12
Also published as: CN102153669A

Abstract

The invention belongs to a preparation method of low-molecule brown seaweed glucan. Alkali carbonate solution is used for breaking up seaweed tissue and cells, acid is used for adjusting a pH value to be proper, alginic acid, brown seaweed polysaccharide and brown seaweed starch are extracted from the seaweed tissue and the cells, and the starch is degraded with hydroxide to turn into the brown seaweed glucan with the average molecular weight being 800-1000 Dalton. As reported, the brown seaweed glucan with the low molecular weight can enhance the immunity of a human body and the stress resistance of plants.

Description

A kind of preparation method of low molecule brown seaweed glucan

Technical field

A kind of preparation method of Seaweed Extract.

Technical background

Marine alga is one of rich in natural resources in the world, and particularly the kelp such as sea-tangle, wakame has successfully been realized propagating artificially, and output increases greatly, and in the world sea-tangle output is above 200,000 tons according to estimates.China is world brown alga cultivation big country; estimate that annual production is above 80,000 tons; the industrial scale of the algin of China is very large at present; aspect food-processing, be used widely; the production of fucose is started late; but develop very soon, be applied to protective foods or medicine, laminaran does not then have large-scale production and application.It is reported, all contain laminaran in sea-tangle and the wakame, content and is that the glucose of β-1,3 structure consists of about 1%, also contains a small amount of β-1,6 structure and a small amount of seminose.It is reported that marine alga starch is the same with other Sargassum polysaccharides also to have certain physiological function, as has the activity of blood fat reducing and reducing cholesterol, low-molecular-weight brown seaweed glucan also can be used as plant-growth regulator, strengthens the resistance of plant.

Summary of the invention

The object of the invention is to invent and provide a kind of preparation method of low-molecular-weight brown seaweed glucan, better realizes the comprehensive utilization of brown alga resource.

For achieving the above object, the preparation technology of brown alga low molecular weight dextran is:

1. lixiviate

Get and be crushed to 0.1～5cm ²Brown alga (sea-tangle, wakame or Sargassum fusiforme), put in the aqueous solution that is dissolved with alkaline carbonate, 60 ℃～90 ℃ insulated and stirred lixiviates 2 hours, make marine alga tissue and cytoclasis, with the acid pH 2～5 that neutralizes, restir lixiviate 1～4 hour, centrifugal or solids removed by filtration bits obtain algae leaching liquor.

2. ultrafiltration and concentration

Vat liquor is 3000 daltonian ultra-filtration membranes or Hollow Fiber Ultrafiltration post ultrafiltration desalination and is concentrated to 1/10～1/40 of vat liquor volume through molecular weight cut-off, is concentrated solution.

3. ethanol precipitation

Add ethanol in the concentrated solution of step 2, make alcohol concn reach 20%～35% (v/v), at this moment alginic acid is out precipitated, and centrifugation goes out precipitation and dehydrates, and gets alginic acid; Continue to add ethanol in centrifugate, make alcohol concn reach 60%～70% (v/v), at this moment algin and fucoidin are out precipitated, and centrifugation goes out precipitation and dehydrates, and gets algin and algal polysaccharide; And then in centrifugate, add ethanol, and make alcohol concn reach 80%～85% (v/v), this moment, laminaran was out precipitated, namely got laminaran through dehydrating.

4. degraded

Laminaran is water-soluble, add an amount of hydrogen peroxide, insulated and stirred is 1～6 hour at a certain temperature, starch is degraded, adding a little Manganse Dioxide makes excessive hydrogen peroxide oxidation decomposite oxygen, then add a small amount of VC and remove residual hydrogen peroxide, in degradation solution, add ethanol dextran is settled out, namely get the low-molecular-weight algal dextran through dehydrating.

Embodiment

Example 1:

(1) preparation laminaran

Get 100g and be crushed to 1～5cm ²Sea-tangle, put in the solution that 2000mL is dissolved with 30g yellow soda ash, 80 ℃ of insulated and stirred 0.5 hour make tissue and the cytoclasis of sea-tangle, slowly drip the hydrochloric acid pH 4 that neutralizes, and extract 2 hours again; Centrifugal or filter, discard centrifugal slag or filter residue (can be used for the production seaweed fertilizer), clear liquid is 3000 daltonian ultra-filtration membranes or Hollow Fiber Ultrafiltration post by molecular weight cut-off, is concentrated to 220mL, adds the 100mL dehydrated alcohol, and Lalgine is precipitated out; Then in 300mL centrifugate, add the 250mL dehydrated alcohol, algin and fucoidin are precipitated out, the centrifugation precipitation, and dehydrate to get algin and fucoidin; Then continue to add dehydrated alcohol in 530mL centrifugate, make alcohol concn reach 85%, the centrifugation precipitation dehydrates to get laminaran 0.8g.

(2) preparation fucose dextran

Above-mentioned starch is dissolved in the 100mL water, add 30% superoxol 10mL, stir insulation degraded 2 hours in 60 ℃, add a little Manganse Dioxide particle, make hydrogen peroxide decomposition emit oxygen, until the rear adding 0.05g Vc of emerging without bubble, remove residual hydrogen peroxide, fully shut down degradation reaction, the centrifugal Manganse Dioxide of removing, obtain 95mL centrifugate, add therein dehydrated alcohol 538mL, dextran is separated out, centrifugal drying, obtain little yellow dextran powder 0.7g, molecular-weight average is 1000 dalton.

Example 2:

(1) preparation laminaran

Get and be crushed to 20 purpose wakame 200g, put in the solution that 5000mL is dissolved with 50g salt of wormwood, stir to extract 0.5 hour in 80 ℃, with the sulfuric acid pH 2 that neutralizes, continue to stir and extracted 4 hours, centrifugal or filter, discard centrifugal slag or filter residue (can be used for the production seaweed fertilizer), clear liquid is 3000 daltonian ultra-filtration membranes or Hollow Fiber Ultrafiltration post by molecular weight cut-off, is concentrated to 600mL, add the 250mL dehydrated alcohol, Lalgine is precipitated out; Then in 810mL centrifugate, add the 620mL dehydrated alcohol, algin and fucoidin are precipitated out, the centrifugation precipitation, and dehydrate to get algin and fucoidin; Then continue to add dehydrated alcohol in 1400mL centrifugate, make alcohol concn reach 80%, the centrifugation precipitation dehydrates to get laminaran 1.7g.

(2) preparation fucose dextran

Above-mentioned starch is dissolved in the 200mL water, add 30% superoxol 15mL, stir insulation degraded 2 hours in 60 ℃, add a little Manganse Dioxide particle, make hydrogen peroxide decomposition emit oxygen, until the rear adding 0.15g Vc of emerging without bubble, remove residual hydrogen peroxide, fully shut down degradation reaction, the centrifugal Manganse Dioxide of removing, obtain 170mL centrifugate, add therein dehydrated alcohol 960mL, dextran is separated out, centrifugal drying, obtain little yellow dextran powder 1.5g, molecular-weight average is 800 dalton.

Claims

1. the preparation method of a low-molecular-weight algal dextran is characterized in that, described low-molecular-weight algal dextran be molecular weight at 800～1000 daltonian low molecule brown seaweed glucans, and described preparation method comprises:

(1) with alkali-metal carbonate aqueous solution the brown alga cell or tissue is disintegrated, discharge Chemical Composition wherein, further arrive pH 2～5 with the acid neutralization, wherein the ratio of used alkaline solution and brown alga is 10:1～40:1, and under 80 ℃ condition stirring reaction 0.5 hour, stirring and leaching l～4 hour under the same conditions again after the acid neutralization, thus make the brown alga slurry; And wherein, used brown alga is sea-tangle, wakame, Sargassum fusiforme, and used acid is hydrochloric acid, sulfuric acid, nitric acid, citric acid, and used alkaline carbonate is yellow soda ash or salt of wormwood, and the concentration of used alkali metal soln is 0.1%～1%;

(2) continue to extract and concentrate with the ultrafiltration desalination, it comprises: the brown alga slurry is made the brown alga vat liquor through centrifugal or filter cleaner, the rotating speed that centrifugal employing is 3000 rev/mins, filter and then adopt diatomite filtration, the clear liquid of slagging-off is through ultra-filtration membrane or the ultrafiltration post is concentrated and desalination, the molecular weight cut-off of ultra-filtration membrane or ultrafiltration post is not more than 3000 dalton, and cycles of concentration is 1/10～1/40 of stoste;

(3) ethanol precipitation, thereby isolate laminaran, it comprises: the desalination concentrated solution of preparation contains algal polysaccharide and laminaran, to use ethanol precipitation, polysaccharide is separated with starch, adopt three grades of precipitations, be precipitated as for the first time and in concentrated solution, add ethanol and make ethanol content reach volume percent 20%～35%, this moment, alginic acid was separated out, precipitation is to go out alignic solution for continuous in centrifugation to add ethanol for the second time, makes alcohol concn reach volume percent 60%～70%, and this moment, fucose was separated out, precipitation is to go out the fucose solution for continuous in centrifugation to add ethanol for the third time, make alcohol concn reach volume percent 80%～85%, this moment, laminaran was separated out, and centrifugation goes out laminaran, and dehydrate, then make laminaran;

(4) this starch is prepared low-molecular-weight brown seaweed glucan through degraded again, it comprises: add superoxol in the aqueous solution of laminaran, 30 ℃～80 ℃ lower insulated and stirred 1～6 hour, laminaran just is degraded to molecular weight at 800～1000 daltonian low molecule brown seaweed glucans, this LMD is namely separated out under volume percent 80%～85% alcohol concn, just makes the alginate oligosaccharide powder through dehydrating.

2. preparation method according to claim 1 is characterized in that, the concentration of used alkali metal soln is 0.3%.

3. preparation method according to claim 1 is characterized in that, the add-on of hydrogen peroxide is 1%～5% of starch, and stops degraded and remove residual hydrogen peroxide with a small amount of Manganse Dioxide and Vc after 2 hours in degraded.

4. preparation method according to claim 3 is characterized in that, the add-on of hydrogen peroxide is 3% of starch.