CN103951556B - A kind of distil process being separated EPA, DPA and DHA from fish oil - Google Patents
A kind of distil process being separated EPA, DPA and DHA from fish oil Download PDFInfo
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- CN103951556B CN103951556B CN201410192466.6A CN201410192466A CN103951556B CN 103951556 B CN103951556 B CN 103951556B CN 201410192466 A CN201410192466 A CN 201410192466A CN 103951556 B CN103951556 B CN 103951556B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
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Abstract
The invention provides a kind of is raw material with fish oil, is separated the distil process of timnodonic acid (EPA), clupanodonic acid (DPA) and docosahexenoic acid (DHA).The method adopts three-stage distillation system to be separated fish oil, and its processing parameter is working pressure 0.01 ~ 100Pa, feeding rate 0.5 ~ 10kg/h, distillation temperature 200 ~ 400 DEG C, film forming rotating speed 100 ~ 350rpm.In products obtained therefrom, the total content of EPA, DPA and DHA reaches more than 50wt.%.This separating technology operates under the condition of high vacuum and relative low temperature, need not carry out esterification treatment, do not introduce any organic solvent to fish oil, protecting EPA, DPA and DHA bioactive while, significantly improves its content in fish oil.
Description
Technical field
The invention belongs to field of food, being specifically related to a kind of is raw material with fish oil, is separated the distil process of timnodonic acid (EPA), clupanodonic acid (DPA) and docosahexenoic acid (DHA).
Background technology
EPA, DPA and DHA etc. have vital role omega-3 polyunsaturated fatty acids to Human Physiology health is rich in fish oil, these nutritive ingredients effectively can promote human brain and neurally to grow, reduce the generation of cardiovascular and cerebrovascular diseases, and can body immunity be strengthened, there is the effects such as anticancer, anti-cancer simultaneously.With fish oil be the healthcare products of raw material at home and abroad go on the market existing for many years, along with people are to the attention increasingly of 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.
But the total content of EPA, DPA and DHA is only about 21wt.% in fish oil, and content is lower, do not reach the content requirement of field of medicaments, be necessary to carry out enriching and purifying to it.Be limited to the high boiling point of fish oil Pharmaceutical ingredients, thermo-sensitivity, oxidizable and there is the features such as biological activity, in addition product separation is used for medicine food industry, therefore selects operational condition safety, green, gentle molecular distillation technique as the purification process of EPA, DPA and DHA in fish oil.
Separating technology general is at present before molecular distillation, carries out ethyl esterified process to fish oil, then is separated through multistage distillation system, obtains the ethyl esterified product of highly purified EPA, DPA and DHA.Although this technique effectively can reduce the thermal destruction risk of material, obtain highly purified separated product, esterification treatment process can introduce organic solvent in product, and esterification can reduce the biological activity of EPA, DPA and DHA equally, affects its pharmaceutical use.Therefore molecular distillation technique is adopted; directly with nonesterified fish oil for raw material; do not introducing under the bioactive prerequisite of omega-3 polyunsaturated fatty acids such as organic solvent and protection EPA, the content improving EPA, DPA and DHA in fish oil has important research meaning.
Summary of the invention
The object of the present invention is to provide a kind of is raw material with fish oil, is separated the distil process of timnodonic acid (EPA), clupanodonic acid (DPA) and docosahexenoic acid (DHA).Operate under the condition of high vacuum and relative low temperature, esterification treatment need not be carried out to fish oil, not introduce any organic solvent, protecting EPA, DPA and DHA bioactive while, 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, pole light constituent is wherein removed through falling-film evaporator under 100 Pa, the product introduction inner-cooled luwa evaporator that falling-film evaporator obtains, secondary light constituent is wherein removed under 10 Pa, 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 be separated with DHA.Light constituent is heated from generating surface effusion and moves to condensing surface condensation, flows into collector form distillate along condensing wall; The difficult volatiles such as EPA, DPA and DHA then goes out to form rectificated remaining liquid along evaporation wall surface current, realizes the object of EPA, DPA and DHA in purifying fish oil.In products obtained therefrom, the total content of EPA, DPA and DHA can reach 50 more than wt.%.
Distillation temperature 200 ~ 400 DEG C, feeding rate 0.5 ~ 10 kg/h, film forming rotating speed 100 ~ 350 rpm.
Remarkable advantage of the present invention is:
(1) is directly raw material with fish oil, carries out fractionation by distillation operation, save material that esterification consumes, time and energy.
(2) under rational Processes and apparatus condition, after three-stage distillation system, in fish oil, the total content of EPA, DPA and DHA can reach 50 more than wt.%.
(3) sepn process can not introduce any separating agent, there is not 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 the 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 (pole light constituent); 4. inner-cooled luwa evaporator; 5. collector two (secondary light constituent); 6. inner-cooled wiped-film short-distance distillation plant; 7. distillate collector; 8. rectificated remaining liquid collector (fish oil after purifying).
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, and thickness of liquid film is 0.001 m.Be that raw material carries out distillation test separation with fish oil, in raw material, EPA content is 11.73wt.%, and DHA content is 6.50 wt.%, DPA content is 3.35 wt.%.Feeding rate is 0.6 L/h, pole light constituent is removed through falling-film evaporator under 100 Pa, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom carries out purifying through inner-cooled wiped-film short-distance distillation plant to omega-3 polyunsaturated fatty acidses such as EPA in fish oil, 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, and in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 more than wt.%.
Embodiment 2
The device using embodiment 1 used and raw material, feeding rate controls within 0.6 ~ 1.0 L/h scope, pole light constituent is removed through falling-film evaporator under 100 Pa, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom carries out purifying through inner-cooled wiped-film short-distance distillation plant to omega-3 polyunsaturated fatty acidses such as EPA in fish oil, 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, and in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 more than 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, and thickness of liquid film is 0.001 m.Be that raw material carries out distillation test separation with fish oil, 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, pole light constituent is removed through falling-film evaporator under 100 Pa, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom carries out purifying through inner-cooled wiped-film short-distance distillation plant to omega-3 polyunsaturated fatty acidses such as EPA in fish oil, working pressure is 0.1 Pa, distillation temperature is 290 ~ 320 DEG C, and film forming rotating speed is 220 rpm.Material is after three-stage distillation system, and in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 more than wt.%.
Embodiment 4
Use the equipment in embodiment 3 and raw material, feeding rate is 5.0 ~ 8.5 kg/h, pole light constituent is removed through falling-film evaporator under 100 Pa, products obtained therefrom removes time light constituent through inner-cooled luwa evaporator under 10 Pa, products obtained therefrom carries out purifying through inner-cooled wiped-film short-distance distillation plant to omega-3 polyunsaturated fatty acidses such as EPA in fish oil, working pressure is 0.1 Pa, and distillation temperature is 300 DEG C, and film forming rotating speed is 220 rpm.Material is after three-stage distillation system, and in rectificated remaining liquid, the total content of EPA, DPA and DHA can reach 50 more than wt.%.
The foregoing is only preferred embodiment of the present invention, all equalizations done 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)
1. one kind is separated the distil process of EPA, DPA and DHA from fish oil, it is characterized in that: the thick product of fish oil is from feeder charging, pole light constituent is wherein removed through falling-film evaporator under 100 Pa, enter inner-cooled luwa evaporator, secondary light constituent is wherein removed under 10 Pa, enter inner-cooled wiped-film short-distance distillation plant, under 0.1 Pa to fish oil in EPA, DPA be separated with DHA; Distillation temperature 200 ~ 400 DEG C, feeding rate 0.5 ~ 10 kg/h, film forming rotating speed 100 ~ 350 rpm; Fish oil is after three-stage distillation system, and in rectificated remaining liquid, the total content of EPA, DPA and DHA reaches more than 50wt.%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410192466.6A CN103951556B (en) | 2014-05-09 | 2014-05-09 | A kind of distil process being separated EPA, DPA and DHA from fish oil |
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| CN201410192466.6A CN103951556B (en) | 2014-05-09 | 2014-05-09 | A kind of distil process being separated EPA, DPA and DHA from fish oil |
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| CN103951556A CN103951556A (en) | 2014-07-30 |
| CN103951556B true CN103951556B (en) | 2015-09-09 |
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| AU2016336354B2 (en) * | 2015-10-05 | 2021-04-15 | Dsm Ip Assets B.V. | Oil compositions and methods of making |
| CN107216252B (en) * | 2016-03-22 | 2021-11-23 | 浙江医药股份有限公司新昌制药厂 | Preparation method of high-content Omega-3 fatty acid ethyl ester |
| CN112521270B (en) * | 2019-09-18 | 2022-09-23 | 浙江医药股份有限公司新昌制药厂 | Method for separating DHA (docosahexaenoic acid) and EPA (eicosapentaenoic acid) by high-vacuum continuous rectification method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101892124A (en) * | 2010-07-14 | 2010-11-24 | 广州市至润油脂食品工业有限公司 | Stink-free deep sea fish oil and preparation method and application thereof |
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| JPH09157685A (en) * | 1995-12-04 | 1997-06-17 | Ikeda Shiyokuken Kk | Concentration of docosahexaenoic acid-containing oil and fat |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101892124A (en) * | 2010-07-14 | 2010-11-24 | 广州市至润油脂食品工业有限公司 | Stink-free deep sea fish oil and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 分子蒸馏分离深海鱼油药用组分的研究;史晋辉等;《海峡药学》;20130915;第25卷(第9期);第69-71页 * |
| 分子蒸馏法制备鱼油多不饱和脂肪酸;傅红等;《无锡轻工大学学报》;20021130;第21卷(第6期);第617-621页 * |
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