CN1034730C - Method of dunaliella collecting and beta-carotene extracting - Google Patents

Abstract

A method for extracting salina beta-carotene. It is characterized in that the density of the solution is reduced by diluting the salina solution with water, and the salina is collected by static sedimentation or centrifugal sedimentation to concentrate the algae solution. The salt algae concentrate obtained is then hypotonically swollen with water to discharge the cell fluid. The obtained algae film preparation is suspended in water, and extracted with vegetable oil or organic solvent in a hypotonic state. The obtained extract can be used as the final product, and can also be precipitated or concentrated with lower alcohols to crystallize β-carotene for use in health care and food additives.

Description

Method of dunaliella collecting and beta-carotene extracting

The invention belongs to a kind of extracting method of salt algae β-Hu Luobusu.

Before the present invention realizes, add flocculation agent such as molysite, aluminium salt etc. in the salt algae liquid that people normally will gather, make described salt algae flocculation, make the floating collection of salt algae with the air supporting method again, obtain wet algae enriched material, use citric acid complex flocculation agent such as aluminium salt, molysite etc. then.The concentration method complex process of this salt algae, cost is higher.The method of extracting β-Hu Luobusu from the wet algae enriched material of collecting has: (1) directly adopts vegetable oil extraction β-Hu Luobusu wherein, but solid-liquid separation is difficult, and inconvenience preparation crystal; (2) will wet and extract after the algae enriched material drying, but increase drying plant, and easily cause the oxidational losses of β-Hu Luobusu; (3) the algae enriched material washing desalination of will wetting, the dehydration enrichment carries out freezing heat then and melts, make cell rupture discharge enchylema after, use solvent extraction again, melt equipment but increased freezing heat, time-consuming taking a lot of work; (4) in the extraction agent edible oil, add tensio-active agent so that membranolysis helps the extraction of β-Hu Luobusu, but increased cost, and the removal of tensio-active agent is relatively more difficult.

The objective of the invention is to overcome the problem that exists in the prior art, a kind of extracting method of simple and easy effective salt algae β-Hu Luobusu is provided.

The extracting method of salt algae β-Hu Luobusu of the present invention at first be the salt algae liquid of will gather in 1: (algae liquid: ratio water water) dilutes salt algae liquid (degree Beaume 15-28 °) to 1-10, carry out solid-liquid separation with subsider or commercially available whizzer then, obtain wet algae enriched material, algae liquid is concentrated, salinity reduces, smaller volume is in order to further pre-treatment.

With above-mentioned wet algae enriched material in 1: (algae liquid: ratio water) adds water to 1-10, thermal agitation in basin, make that the salt frustule is hypotonic to be burst, examine under a microscope almost all that the thin chests of algae break, discharge enchylema, carry out solid-liquid separation with subsider or whizzer then, obtain the thick film preparation of the cytolemma, thylakoid membrane etc. of salt algae, wash film again with water for several times, further remove water soluble component, gained algae film preparation is a red-purple, for further extraction usefulness.

With described algae film preparation in 1: (algae film preparation: water: ratio extraction agent) adds water and one or more extraction agents to 1-5: 1-10.The effect of water is to keep hypotonic condition makes frustule be in state of rupture, and helps mixing and fully contacting of algae film and extraction agent.Extraction can be carried out in common extractor, and the extraction liquid layer that the upper strata contains β-Hu Luobusu is collected in room temperature or heated and stirred extraction 10-120 minute, and lower floor's algae-residue and aqueous phase layer are abandoned it.

Described extraction agent mainly adopts the good salad oil of low temperature current downflow or other vegetables oil such as soya-bean oil, rape oil, cottonseed wet goods, also can adopt ether, sherwood oil, hexanaphthene, hexane, acetone, dithiocarbonic anhydride or their volatile organic solvents such as mixture.When using salad oil to make extraction agent, the collected salad oil reservoir that contains β-Hu Luobusu is a finished product, it is brown xanchromatic oily liquids, its content beta-carotene is less than 20%, and its composition comprises carotenoid, fat-soluble pigment, liposoluble vitamin (as vitamin A and vitamin-E) and other fat-soluble cpds.When with an organic solvent making extraction agent, after the extraction liquid heating evaporation can being concentrated, add or do not add ethanol or methyl alcohol, 0-10 ℃ leaves standstill and separates out the red-purple crystal, and content beta-carotene is greater than 90%; Also can directly in extraction liquid, add ethanol or methyl alcohol (extraction liquid: ethanol or methyl alcohol=1: 1-10), the β-Hu Luobusu precipitation is separated out, content beta-carotene is greater than 50%, its composition is β-Hu Luobusu stereoisomer mixture and a small amount of alpha-carotene etc., and product is red-purple ointment shape.

Because described salt algae liquid solution proportion through diluting after descends, the salt algae is very easily by sedimentation or centrifuging collection, can make that salt algae thickening equipment is corresponding to dwindle, simplify technology, reduces cost.Salt algae enriched material bursts through water is hypotonic, and after the washing for several times, resulting salt algae film preparation has been removed the enchylema composition, has saved drying or freeze thawing equipment, also needn't add tensio-active agent, helps later extraction and separating technology.Extraction process carries out under hypotonic condition, and extraction is abundant, convenient, solid-liquid separation is simple, can make more than the extraction rate reached to 90% of β-Hu Luobusu in the described salt algae.As≤the 3ppm of products obtained therefrom, Pb≤10ppm.

Embodiment 1: the salt algae is diluted mixing with isopyknic water in basin, separate solid-liquid with commercially available whizzer, obtain wet algae enriched material.Wet algae enriched material is burst with 10 times water is hypotonic, enchylema in the frustule is flowed out, centrifuge dehydration then, make the thylakoid membrane that is rich in β-Hu Luobusu of salt algae and cytolemma etc. be deposited in the bottom, get salt algae film preparation, (algae film: water: ratio sherwood oil) added entry and sherwood oil in 1: 5: 5 with described salt algae film preparation then, the stirring at room extraction is after 30 minutes, carrying out two in extractor is separated, the upper layer of extraction liquid layer adds 2 times of ethanol, carotene is separated out, then can obtain containing the brown xanchromatic ointment shape throw out of β-Hu Luobusu more than 50%.

Embodiment 2: the preparation of described salt algae film preparation such as embodiment 1, (algae film: water: ratio salad oil) added entry and salad oil in 1: 1: 2 then, in extractor, stir and extracted 2 hours, centrifugally then carry out two and be separated, then can obtain containing the pale brown look oily liquids of β-Hu Luobusu more than 1%.

Embodiment 3: salt algae liquid is diluted sedimentation in the rearmounted subsider with 10 times water, obtain wet algae enriched material.Press embodiment 1, water is hypotonic burst, wash after, the algae film preparation.Pack in the extractor, then in 1: 1: 1 (algae film: water: ratio adding sherwood oil sherwood oil), 50 ℃ were stirred after 30 minutes, leave standstill and carry out two and be separated, upper layer of extraction liquid is taken out rearmounted commercially available evaporator evaporation and is concentrated, put then under the 0-10 ℃ of condition and separate out the red-purple crystallization, contain β-Hu Luobusu more than 90%.

Claims (4)

1. The extraction method of salina β-carotene is characterized in that the raw material salina liquid is diluted with water in a ratio of 1: 1-10 (salina liquid: water), the density of the solution is reduced, and the liquid is settled by standing or centrifuging The method is to recover the salina, concentrate the algae liquid, reduce the salinity, and reduce the volume to obtain the salina concentrate. The salt algae concentrate is then hypotonically burst with water, that is, the salt algae concentrate and water are mixed in a ratio of 1:1-10 (salina concentrate: water), and vigorously shaken to rupture the salina cells. The cell fluid is discharged, and the red algae film preparation is obtained after washing with water. The algae film preparation needs to be suspended in water to maintain a low-osmotic bursting state, and is extracted with a common extraction agent. The obtained extract can be used as the final product or β-carotene can be precipitated by lower alcohol precipitation or crystallized after concentration. 2. The method according to claim 1, wherein when the algae film preparation is extracted with the extractant, water needs to exist to maintain the hypotonic condition so that the algae cells are in a ruptured state, according to 1: 1-5: 1- 10 (algae film preparation: water: extractant) mix the algae film with water and extractant, extract at room temperature or by heating. 3. The method according to claim 1, wherein the extractant used can be edible vegetable oils such as salad oil, soybean oil, rapeseed oil, cottonseed oil, or ether, sherwood oil, hexanaphthene, normal hexane, acetone, Organic solvents such as carbon disulfide may also be a mixture thereof. 4. method according to claim 1 is characterized in that when using vegetable oil as extraction agent, extract is the product containing less than 20% beta-carotene; when using organic solvent as extraction agent, can press 1: Add ethanol or methanol at a ratio of 1-10 (extractant: lower alcohol) to precipitate β-carotene in the form of purple ointment, and the content of β-carotene is greater than 50%; you can also directly evaporate and concentrate the extract, add Or do not add ethanol or methanol, crystallize carotene at 0-10°C, and the content of β-carotene is greater than 90%.