CN105218696A - A kind of preparation method of high purity fucoidin - Google Patents

Abstract

The invention discloses a kind of preparation method of high purity fucoidin, belong to the preparing technical field of polyose.The present invention is directed to tradition at present extracts in the process of fucoidin, in vat liquor, impurity is many, at high temperature polysaccharide of making angry decomposes, and polysaccharide loss reaches more than 10% in preprocessing process, the invention provides a kind of preparation method of high purity fucoidin, first the present invention cultivates fresh sea grass, its fucoidin content is increased, re-use hydrochloric acid soln, lixiviate is carried out under microwave-assisted, the vat liquor of gained is decoloured, then by itself and sepiolite, sodium-acetate mixes, purifying under electrical condition, the refined solution of gained is mixed with trichoroacetic acid(TCA), remove albumen precipitation, finally purify purity 45 ~ 55% fucoidin.

Description

A kind of preparation method of high purity fucoidin

Technical field

The invention discloses a kind of preparation method of high purity fucoidin, belong to the preparing technical field of polyose.

Background technology

Fucoidin is algal polysaccharide again, is iuntercellular polysaccharide intrinsic in brown alga, is present in cell wall matrix.Its function may be have the moisture absorption to prevent the effect done in an atmosphere when time of low water frond exposes.Research shows that algal polysaccharide has certain lipidemia and the pharmaceutical activity of Tumor suppression, caused the concern of pharmacy research staff in recent years, product can produce natural radioactivity medicine that is antitumor, antiviral, reducing blood-fat, for the treatment of tumour, cardiovascular disease and renal function disease, the healthcare products of anti-oxidant, reducing blood-fat, raising body immunity also can be produced.

The existing method extracting fucoidin from marine alga of analysis and summary, mainly comprises water extraction and sour formulation two kinds.The present invention adopts the biologic enzymolysis method of high-efficiency cleaning to be extracted from marine alga by fucoidin, not only overcomes traditional water extraction and sour formulation and extracts fucoidin, and in its extract, effective constituent and structure are easily degraded the drawback destroyed; In addition, Enzymatic Extraction also has applied widely, fucoidin yield and the high feature of purity; It will be further appreciated that the fucoidin that Enzymatic Extraction obtains mostly is low-molecular-weight polysaccharide, be easier to absorption of human body and utilize.

At present, marine alga fragmentation is all Mechanical Crushing or enzymatic shell-broken, Extracting temperature is at 80 ~ 100 DEG C, extraction time is generally at 4 ~ 6 hours, extraction time, more than twice, adopts alkalescence, neutral or acidic solution soaks or stirring is extracted, and extracts yield 1% ~ 3%, but in vat liquor, the impurity such as protein is more, and high temperature also may cause polysaccharide to decompose.Although sodium hydroxide and formaldehyde method etc. can be adopted to carry out pre-treatment to frond or vat liquor reduce foreign matter content, pre-treatment often causes polysaccharide loss to reach more than 10%.

Summary of the invention

The technical problem that the present invention mainly solves: in the process for the fucoidin of tradition extraction at present, in vat liquor, impurity is many, at high temperature polysaccharide of making angry decomposes, and polysaccharide loss reaches more than 10% in preprocessing process, the invention provides a kind of preparation method of high purity fucoidin, first the present invention cultivates fresh sea grass, its fucoidin content is increased, re-use hydrochloric acid soln, lixiviate is carried out under microwave-assisted, the vat liquor of gained is decoloured, then by itself and sepiolite, sodium-acetate mixes, purifying under electrical condition, the refined solution of gained is mixed with trichoroacetic acid(TCA), remove albumen precipitation, finally purify purity 45 ~ 55% fucoidin.

In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is:

(1) get 1 ~ 3kg fresh sea grass and put into cultivation pool, seawater is added wherein by solid-to-liquid ratio 1:3, stir respectively to wherein adding 10 ~ 15g Sodium phosphate dibasic, 3 ~ 5g SODIUM PHOSPHATE, MONOBASIC, 100 ~ 200g ammonium nitrate and 280 ~ 380g calcium amino acid chelate again, then in cultivation pool, oxygen is filled with, ensure that the oxygen level in the solution in cultivation pool is 8.6 ~ 9.2mg/L, be 8000 ~ 9000Lux in intensity of illumination, temperature is at 30 ~ 38 DEG C, cultivates 2 ~ 4 days;

(2) sea grass is taken out after terminating by above-mentioned cultivation, distilled water is used to be cleaned on its surface, put it into again in refrigeration chamber, temperature is set as-15 ~-5 DEG C, after sea grass is hardening, taken out and put into pulverizer, be ground into 30 ~ 50 order particles, the particulate matter of gained is put into container, add 120 ~ 300g cellulose complex enzyme wherein, deionized water is used to soak particulate matter, then functional quality mark is the hydrochloric acid soln adjustment pH of 45% is 4 ~ 5, it is 50 ~ 60 DEG C in temperature, microwave is under 600 ~ 800MHz, slow stirring 2 ~ 4h, speed setting is 120 ~ 160r/min,

(3) filter after above-mentioned stirring terminates, the filtered liquid of gained is put into container, after adding 300 ~ 400g sodium chlorate stirring, 10 ~ 15min wherein, add wherein massfraction be 70% sodium hydroxide solution regulate pH be 8 ~ 9, then be poured in whizzer and carry out centrifugation, get supernatant liquor;

(4) supernatant liquor of above-mentioned gained is put into container, adding massfraction is wherein that the hydrogen peroxide of 25% is until produce without precipitation, and then add wherein and add 50 ~ 70g80 order sepiolite powder and 300 ~ 400g sodium-acetate respectively, stir, control current density 0.09 ~ 0.12A/cm ², after purifying 70 ~ 90min, filter through row;

(5) filtered liquid of above-mentioned gained is put into container, adding trichoroacetic acid(TCA) wherein makes its concentration in the solution be 3.0 ~ 3.5g/mL, leave standstill 20 ~ 24h, centrifugal segregation albumen precipitation, and then in supernatant liquor, add massfraction be 25% calcium oxide solution adjust ph be 7.5 ~ 8.0, adding dehydrated alcohol again makes the volume fraction of ethanol in its supernatant liquor be 25 ~ 30%, at temperature is 5 ~ 10 DEG C, leave standstill until produce without precipitation, carried out centrifugation again, collect centrifugal thing, centrifugal thing is put into air dryer to carry out air-dry, obtain high purity fucoidin.

Fucoidin biological activity obtained by the present invention is high, and maintains content and the ratio of natural constituents.

The invention has the beneficial effects as follows:

(1) purity of the fucoidin obtained by the present invention reaches 45 ~ 55%;

(2) the present invention is in preparation process, and the organic solvent of use is easy to reclaim, and in the product obtained, solvent residual amount is lower than 1%;

(3) cost of manufacture of the present invention is low, easy handling.

Claims (1)

1. a preparation method for high purity fucoidin, is characterized in that concrete preparation process is:

(1) get 1 ~ 3kg fresh sea grass and put into cultivation pool, seawater is added wherein by solid-to-liquid ratio 1:3, stir respectively to wherein adding 10 ~ 15g Sodium phosphate dibasic, 3 ~ 5g SODIUM PHOSPHATE, MONOBASIC, 100 ~ 200g ammonium nitrate and 280 ~ 380g calcium amino acid chelate again, then in cultivation pool, oxygen is filled with, ensure that the oxygen level in the solution in cultivation pool is 8.6 ~ 9.2mg/L, be 8000 ~ 9000Lux in intensity of illumination, temperature is at 30 ~ 38 DEG C, cultivates 2 ~ 4 days;

(2) sea grass is taken out after terminating by above-mentioned cultivation, distilled water is used to be cleaned on its surface, put it into again in refrigeration chamber, temperature is set as-15 ~-5 DEG C, after sea grass is hardening, taken out and put into pulverizer, be ground into 30 ~ 50 order particles, the particulate matter of gained is put into container, add 120 ~ 300g cellulose complex enzyme wherein, deionized water is used to soak particulate matter, then functional quality mark is the hydrochloric acid soln adjustment pH of 45% is 4 ~ 5, it is 50 ~ 60 DEG C in temperature, microwave is under 600 ~ 800MHz, slow stirring 2 ~ 4h, speed setting is 120 ~ 160r/min,

(3) filter after above-mentioned stirring terminates, the filtered liquid of gained is put into container, after adding 300 ~ 400g sodium chlorate stirring, 10 ~ 15min wherein, add wherein massfraction be 70% sodium hydroxide solution regulate pH be 8 ~ 9, then be poured in whizzer and carry out centrifugation, get supernatant liquor;

(4) supernatant liquor of above-mentioned gained is put into container, adding massfraction is wherein that the hydrogen peroxide of 25% is until produce without precipitation, and then add wherein and add 50 ~ 70g80 order sepiolite powder and 300 ~ 400g sodium-acetate respectively, stir, control current density 0.09 ~ 0.12A/cm ², after purifying 70 ~ 90min, filter through row;

(5) filtered liquid of above-mentioned gained is put into container, adding trichoroacetic acid(TCA) wherein makes its concentration in the solution be 3.0 ~ 3.5g/mL, leave standstill 20 ~ 24h, centrifugal segregation albumen precipitation, and then in supernatant liquor, add massfraction be 25% calcium oxide solution adjust ph be 7.5 ~ 8.0, adding dehydrated alcohol again makes the volume fraction of ethanol in its supernatant liquor be 25 ~ 30%, at temperature is 5 ~ 10 DEG C, leave standstill until produce without precipitation, carried out centrifugation again, collect centrifugal thing, centrifugal thing is put into air dryer to carry out air-dry, obtain high purity fucoidin.