CN103951556A

CN103951556A - Distillation process for separating EPA (eicosapentaenoic acid), DPA (docosapentaenoic acid) and DHA (docosahexaenoic acid) from deep sea fish oil

Info

Publication number: CN103951556A
Application number: CN201410192466.6A
Authority: CN
Inventors: 胡晖; 谷高阳; 张举斌
Original assignee: Fuzhou University
Current assignee: Fuzhou University
Priority date: 2014-05-09
Filing date: 2014-05-09
Publication date: 2014-07-30
Anticipated expiration: 2034-05-09
Also published as: CN103951556B

Abstract

The invention provides a distillation process for separating EPA (eicosapentaenoic acid), DPA (docosapentaenoic acid) and DHA (docosahexaenoic acid) by using deep sea fish oil as a raw material. In the distillation process, the deep sea fish oil is separated by adopting a three-stage distillation system; the process parameters are as follows: the operating pressure is 0.01-100Pa, the feed rate is 0.5-10kg/h, the distillation temperature is 200-400 DEG C, and the film forming speed is 100-350rpm. The total content of EPA, DPA and DHA in the obtained product is more than 50wt%. The separation process is operated under the conditions of high vacuum and relatively low temperature and dispenses with esterification treatment of the deep sea fish oil and introduction of any organic solvent, thus substantially increasing the contents of EPA, DPA and DHA in the deep sea fish oil while protecting the bioactivities of EPA, DPA and DHA.

Description

A kind of from fish oil the distil process of separated EPA, DPA and DHA

Technical field

The invention belongs to field of food, be specifically related to a kind ofly take fish oil as raw material, the distil process of separated timnodonic acid (EPA), clupanodonic acid (DPA) and docosahexenoic acid (DHA).

Background technology

In fish oil, be rich in EPA, DPA and DHA etc. and Human Physiology health there is to the omega-3 polyunsaturated fatty acids of vital role, these nutritive ingredients can effectively promote human brain and neural growing, reduce the generation of cardiovascular and cerebrovascular diseases, and can strengthen body immunity, there is the effects such as anticancer, anti-cancer simultaneously.The healthcare products that the fish oil of take is raw material at home and abroad go on the market and have for many years, and along with the increasingly attention of people to ω-3 polyunsaturated fatty acid, fish oil is as the important sources of pure natural omega-3 polyunsaturated fatty acids, and its application prospect will be considerable.

Yet the total content of EPA, DPA and DHA is only 21wt.% left and right in fish oil, content is lower, does not reach the content requirement of field of medicaments, is necessary it to carry out enriching and purifying.The high boiling point, thermo-sensitivity, oxidizable and there is the features such as biological activity that are limited to the medicinal component of fish oil, in addition product separation is for medicine food industry, therefore select safe, green, the gentle molecular distillation technique of operational condition as the purification process of EPA, DPA and DHA in fish oil.

General separating technology is before molecular distillation at present, fish oil is carried out to second esterification treatment, then carry out separation through multistage distillation system, obtains the second esterified prod of highly purified EPA, DPA and DHA.Although this technique can effectively reduce the thermal destruction risk of material, obtains highly purified separated product, esterification treatment process can be introduced organic solvent in product, and esterification can reduce the biological activity of EPA, DPA and DHA equally, affects its pharmaceutical use.Therefore adopt molecular distillation technique; directly take nonesterified fish oil as raw material; do not introducing under the bioactive prerequisites of omega-3 polyunsaturated fatty acids such as organic solvent and protection EPA, in raising fish oil, the content of EPA, DPA and DHA has important research meaning.

Summary of the invention

The object of the present invention is to provide and a kind ofly take fish oil as raw material, the distil process of separated timnodonic acid (EPA), clupanodonic acid (DPA) and docosahexenoic acid (DHA).Under the condition of high vacuum and relative low temperature, operate, need not carry out esterification treatment to fish oil, do not introduce any organic solvent, in protection EPA, DPA and bioactive while of DHA, significantly improve its content in fish oil.

For achieving the above object, the present invention adopts following technical scheme:

The thick product of fish oil is from feeder charging, under 100 Pa, through falling-film evaporator, remove utmost point light constituent wherein, the product introduction inner-cooled luwa evaporator that falling-film evaporator obtains, under 10 Pa, remove inferior light constituent wherein, the product introduction inner-cooled wiped-film short-distance distillation plant that inner-cooled luwa evaporator obtains, under the working pressure of 0.1 Pa to fish oil in EPA, DPA carry out separated with DHA.Light constituent is heated and overflows and to move to condensing surface and condense from generating surface, flows into collector form distillate along condensing wall; The difficult volatiless such as EPA, DPA and DHA go out to form rectificated remaining liquid along evaporation wall surface current, realize the object of EPA, DPA and DHA in purifying fish oil.More than in products obtained therefrom, the total content of EPA, DPA and DHA can reach 50 wt.%.

200 ~ 400 ℃ of distillation temperatures, feeding rate 0.5 ~ 10 kg/h, film forming rotating speed 100 ~ 350 rpm.

Remarkable advantage of the present invention is:

(1) directly take fish oil as raw material, carry out fractionation by distillation operation, saved the material that esterification consumes, time and energy.

(2) under rational Processes and apparatus condition, after three-stage distillation system, more than in fish oil, the total content of EPA, DPA and DHA can reach 50 wt.%.

(3) sepn process can not introduced any separating agent, does not have organic reagent residue problem.

(4) material is without esterification pre-treatment, and the biological activity of EPA, DPA and DHA can be protected, and does not affect the pharmaceutical use of product.

(5) technology of the present invention can be used for other high boiling points, thermo-sensitivity, oxidizable and have a Separation Research of bioactive natural product.

Accompanying drawing explanation

Fig. 1 is process flow sheet of the present invention.

1. feeder; 2. falling-film evaporator; 3. collector one (utmost point light constituent); 4. inner-cooled luwa evaporator; 5. collector two (inferior light constituent); 6. inner-cooled wiped-film short-distance distillation plant; 7. distillate collector; 8. rectificated remaining liquid collector (purifying after fish oil).

Embodiment

Embodiment 1

Inner-cooled wiped-film short-distance distillation plant adopts small testing device, high 0.230 m of evaporator wall, and evaporation radius is 0.070 m, thickness of liquid film is 0.001 m.The fish oil of take carries out distillation test separation as raw material, and in raw material, EPA content is 11.73wt.%, and DHA content is 6.50 wt.%, and DPA content is 3.35 wt.%.Feeding rate is 0.6 L/h, under 100 Pa, through falling-film evaporator, remove utmost point light constituent, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom through inner-cooled wiped-film short-distance distillation plant to fish oil in the omega-3 polyunsaturated fatty acids such as EPA carry out purifying, working pressure is 0.1 Pa, distillation temperature is 563 ~ 583 K, and film forming rotating speed is 300 rpm.Material is after three-stage distillation system, more than in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 wt.%.

Embodiment 2

Use embodiment 1 device and raw material used, within feeding rate is controlled at 0.6 ~ 1.0 L/h scope, under 100 Pa, through falling-film evaporator, remove utmost point light constituent, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom through inner-cooled wiped-film short-distance distillation plant to fish oil in the omega-3 polyunsaturated fatty acids such as EPA carry out purifying, working pressure is 0.1 Pa, and distillation temperature is set as 573 K, and film forming rotating speed is 300 rpm.Material is after three-stage distillation system, more than in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 wt.%.

Embodiment 3

Inner-cooled wiped-film short-distance distillation plant adopts pilot plant, high 0.850 m of evaporator wall, and evaporation radius is 0.140 m, thickness of liquid film is 0.001 m.The fish oil of take carries out distillation test separation as raw material, in raw material, EPA content is 12.03 wt.%, DHA content is 6.68 wt.%, DPA content is 3.31 wt.%, feeding rate is 8 kg/h, under 100 Pa, through falling-film evaporator, remove utmost point light constituent, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom through inner-cooled wiped-film short-distance distillation plant to fish oil in the omega-3 polyunsaturated fatty acids such as EPA carry out purifying, working pressure is 0.1 Pa, distillation temperature is 290 ~ 320 ℃, and film forming rotating speed is 220 rpm.Material is after three-stage distillation system, more than in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 wt.%.

Embodiment 4

Use equipment and raw material in embodiment 3, feeding rate is 5.0 ~ 8.5 kg/h, under 100 Pa, through falling-film evaporator, remove utmost point light constituent, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom through inner-cooled wiped-film short-distance distillation plant to fish oil in the omega-3 polyunsaturated fatty acids such as EPA carry out purifying, working pressure is 0.1 Pa, and distillation temperature is 300 ℃, and film forming rotating speed is 220 rpm.Material is after three-stage distillation system, more than in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 wt.%.

The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.

Claims

1. the distil process of separated EPA, DPA and DHA from a fish oil, it is characterized in that: the thick product of fish oil is from feeder charging, under 100 Pa, through falling-film evaporator, remove utmost point light constituent wherein, enter inner-cooled luwa evaporator, under 10 Pa, remove inferior light constituent wherein, enter inner-cooled wiped-film short-distance distillation plant, under 0.1 Pa to fish oil in EPA, DPA carry out separated with DHA.

According to claim 1 from fish oil the distil process of separated EPA, DPA and DHA, it is characterized in that: fish oil is after three-stage distillation system, more than in rectificated remaining liquid, the total content of EPA, DPA and DHA reaches 50wt.%.

According to claim 1 from fish oil the distil process of separated EPA, DPA and DHA, it is characterized in that: 200 ~ 400 ℃ of distillation temperatures, feeding rate 0.5 ~ 10 kg/h, film forming rotating speed 100 ~ 350 rpm.