CN101177649B - Method for enriching active ingredient of seal oil - Google Patents
Method for enriching active ingredient of seal oil Download PDFInfo
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- CN101177649B CN101177649B CN2006101546140A CN200610154614A CN101177649B CN 101177649 B CN101177649 B CN 101177649B CN 2006101546140 A CN2006101546140 A CN 2006101546140A CN 200610154614 A CN200610154614 A CN 200610154614A CN 101177649 B CN101177649 B CN 101177649B
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Abstract
The invention discloses a method for enriching active ingredient from sea beer coarse oil. A little organic solvent is contained in termination products produced by the existing method, thus greatly limiting the application of the sea beer oil in natural medicines and health products; the enriching method of the existing method comprises esterification and degreasing processes with a plurality of steps and complex technique. The invention takes the sea beer coarse oil as raw material, and sea beer refined oil can be obtained after the purification through modular distillation and the enrichment of the active ingredient of unsaturated fatty acid. The invention is characterized in that the following conditions are adopted when in modular distillation: the charging flow is 20 to 100 ml/ min, and the evaporation temperature is 290 to 330 DEG C; the invention has the advantages of simple technique, short detention time and pollution free, and no esterification process is needed when the flow and the distillation temperature are high; the enriched sea beer refined oil is particularly applicable in the natural medicines and the health products.
Description
Technical field
The present invention relates to a kind of from the thick oil of fur seal the method for active constituent-enriched omega-3 unsaturated fatty acid (3-PUFA).
Background technology
Fur seal is that a kind of whole body covers with bristle, live in the following marine mammal in high and cold waters, the arctic (40 ℃) all the year round, its body contains a large amount of unsaturated fatty acids-mainly comprise timnodonic acid (EPA), docosahexenoic acid (DHA) and clupanodonic acid (DPA).Patent reports such as CN1679626, CN1437955, CN1435186, CN1518990, CN1410076 and CN1410077 the application of Seal fat: be used for preparation control chemical damage healthcare products; Preparation prevents and treats the climacteric syndrome medicine; Preparation senile dementia prevention and cure medicine; The healthcare products of also available removal chloasma, comedo and pregnant occasion spot; Also has special efficacy at treatment hyperplasia of prostate and diabetes.In addition, because these unsaturated fatty acidss (3-PUFA) human body self can not produce, must absorb from the external world.If long-term lacking can cause multiple disease, as: children's intellectual education dysplasia, atherosclerosis, hyperlipidemia and psoriasis etc.
Do not reach medicinal requirements because the thick oily 3-PUFA content of Seal fat in the market is low excessively, must carry out purification enrichment crude oil.At present, the method for enrichment active ingredient of seal oil adopts high vacuum rectification method or molecular distillation method after mainly including machine solvent extration, high performance liquid chromatography, silver resin chromatography, esterification.Above-mentioned high vacuum rectification method or molecular distillation method, in order to reduce the raw material boiling point, carried out esterification, in this process, brought a small amount of organic solvent into, make and contain a small amount of organic solvent in the finished product, limit the application of Seal fat greatly as a kind of natural drug and healthcare products; Carry out molecular distillation or high vacuum rectification then and purify, active constituent-enriched unsaturated fatty acids takes off ester again and gets the fur seal essential oil, and enriching method need be through over-churning, take off the ester process, and step is many, complex process.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that above-mentioned prior art exists, a kind of enriching method that carries out the Seal fat effective ingredient under high flow capacity and high distillation temperature condition is provided, it need not esterification, still-process does not have any pollution, technology is simple, active constituent content height, effective in the fur seal essential oil product of gained.
The present invention is realized by following technical proposals: the enriching method of active ingredient of seal oil, with the thick oil of fur seal is raw material, carry out purifying by molecular distillation, active constituent-enriched unsaturated fatty acids, get the fur seal essential oil, adopt following condition to operate when it is characterized in that molecular distillation: feed rate is the 20-100 ml/min, and vaporization temperature is 290-330 ℃.The present invention adopts above-mentioned processing condition to carry out molecular distillation, be different from fully the existing processes condition (feed rate in the existing molecular distillation method be generally the 60-100 milliliter/hour, vaporization temperature is≤100 ℃), the present invention has broken through the restriction of processing condition conventional in the existing molecular distillation method, under the condition of high flow capacity, high distillation temperature, need not esterification, technology is simple, avoid introducing organic solvent, be particularly suitable for the application in natural drug and healthcare products; Under high flow capacity, the residence time is short, does not produce other high objectionable impurities of boiling, also not polymerization, environmentally safe.
The enriching method of described active ingredient of seal oil, the pressure during molecular distillation are 0.01-10Pa, reduce service temperature as far as possible.
The enriching method of described active ingredient of seal oil, the cooling temperature during molecular distillation is 30-80 ℃, guarantees that condensed fluid can unrestricted flow in condenser.
The enriching method of described active ingredient of seal oil, the stir speed (S.S.) during molecular distillation is 100-1000rpm, guarantees the material mass transfer and conducts heat abundant.
The enriching method of described active ingredient of seal oil, the device that molecular distillation adopts are that the spacing of generating surface and condensing surface is 2～15cm, evaporation area 0.5-1.5m
2Short-path evaporator, guarantee that material can be evaporated on the condensing surface and enough evaporation areas are arranged.
The enriching method of described active ingredient of seal oil, the temperature difference that keeps vaporizer and condenser in the short-path evaporator during distillation be more than 60 ℃, guarantees to steam the gas pipe seizure that can be condensed fully.
The present invention has following beneficial effect: under the condition of high flow capacity, high distillation temperature, need not esterification, and technology is simple, and the residence time is short, does not produce other high objectionable impurities of boiling, also not polymerization, environmentally safe; The present invention purifies, and to reach required concentration process be simple flash distillation process to the thick oil of fur seal, do not bring any organic solvent into, and the fur seal essential oil after the enrichment is particularly suitable for using in natural drug and healthcare products.
The present invention is further illustrated below in conjunction with embodiment.
Embodiment
Embodiment 1
(feeder volume 300ml, 1.2 square metres of evaporation areas add 1L Seal fat crude product in the feeder of blade applicator rotating speed 100～1000rpm), contain 3-PUFA17.4% at the self-control molecular distillation apparatus.Open raw material preheating device, be warmed up to 100 ℃.The open cold radiator cooler, (it is excessive that condensing temperature can not be crossed the low distillate viscosity that causes to keep cooling temperature to be 40 ℃, influence is flowed), in cold-trap, add liquid nitrogen, open rotary-vane vaccum pump, make the working pressure of system reach 1.5Pa, open oil diffusion pump after 20 minutes, system pressure reaches 0.6Pa.The exact constant temperature groove that unlatching evaporation material is used heats thermal oil, make temperature surely arrive first 180 ℃, temperature to 290 ℃ is set again, after reaching target temperature, begin charging, feeding rate is 20mL/min, and the rotating speed of blade applicator is 300rpm, after still-process finishes, get overhead product 389mL, last running 587mL; 3-PUFA content reaches 25.8% in the finished product.
Embodiment 2
In the feeder of self-control molecular distillation apparatus (the same), add 1L Seal fat crude product, contain 3-PUFA18.8%.Open raw material preheating device, be warmed up to 100 ℃.The open cold radiator cooler, keeping cooling temperature is 50 ℃, adds liquid nitrogen in cold-trap, opens rotary-vane vaccum pump, makes the working pressure of system reach 1.5Pa, opens oil diffusion pump after 20 minutes, system pressure reaches 0.8Pa.The exact constant temperature groove that unlatching evaporation material is used heats thermal oil, make temperature surely arrive first 180 ℃, temperature to 310 ℃ is set again, after reaching target temperature, begin charging, feeding rate is 60mL/min, and the rotating speed of blade applicator is 300rpm, after still-process finishes, get overhead product 486mL, last running 505mL; 3-PUFA content reaches 28.3% in the finished product.
Embodiment 3
In the feeder of self-control molecular distillation apparatus (the same), add 1L Seal fat crude product, contain 3-PUFA15.3%.Open raw material preheating device, be warmed up to 100 ℃.The open cold radiator cooler, keeping cooling temperature is 60 ℃, adds liquid nitrogen in cold-trap, opens rotary-vane vaccum pump, makes the working pressure of system reach 1.5Pa, opens oil diffusion pump after 20 minutes, system pressure reaches 0.1Pa.The exact constant temperature groove that unlatching evaporation material is used heats thermal oil, make temperature surely arrive first 180 ℃, temperature to 330 ℃ is set again, after reaching target temperature, begin charging, feeding rate is 80mL/min, and the rotating speed of blade applicator is 350rpm, after still-process finishes, get overhead product 484mL, last running 504mL; 3-PUFA content reaches 27.6% in the finished product.
Embodiment 4
In the feeder of self-control molecular distillation apparatus (the same), add 1L Seal fat crude product, contain 3-PUFA17.6%.Open raw material preheating device, be warmed up to 100 ℃.The open cold radiator cooler, (it is excessive that condensing temperature can not be crossed the low distillate viscosity that causes to keep cooling temperature to be 70 ℃, influence is flowed), in cold-trap, add liquid nitrogen, open rotary-vane vaccum pump, make the working pressure of system reach 1.5Pa, open oil diffusion pump after 20 minutes, system pressure reaches 0.1Pa.The exact constant temperature groove that unlatching evaporation material is used heats thermal oil, make temperature surely arrive first 180 ℃, temperature to 315 ℃ is set again, after reaching target temperature, begin charging, feeding rate is 100mL/min, and the rotating speed of blade applicator is 300rpm, after still-process finishes, get overhead product 495mL, last running 486mL; 3-PUFA content reaches 28.4% in the finished product.
Protection scope of the present invention is not limited to the foregoing description, and technical scheme all and of the present invention technology contents identical or that be equal to all falls within the scope of protection of the present invention.
Claims (4)
1. the enriching method of active ingredient of seal oil, with the thick oil of fur seal is raw material, carry out purifying by molecular distillation, active constituent-enriched unsaturated fatty acids, get the fur seal essential oil, adopt following condition to operate when it is characterized in that molecular distillation: feed rate is the 20-100 ml/min, and vaporization temperature is 290-330 ℃, pressure during molecular distillation is 0.1-0.8Pa, and the cooling temperature during molecular distillation is 30-80 ℃.
2. the enriching method of active ingredient of seal oil according to claim 1, the stir speed (S.S.) when it is characterized in that molecular distillation is 100-1000rpm.
3. the enriching method of active ingredient of seal oil according to claim 2 is characterized in that device that described molecular distillation adopts is that the spacing of generating surface and condensing surface is 2～15cm, evaporation area 0.5-1.5m
2Short-path evaporator.
4. the enriching method of active ingredient of seal oil according to claim 3, the temperature difference that keeps vaporizer in the short-path evaporator and condenser when it is characterized in that distilling is more than 60 ℃.
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| CN2006101546140A CN101177649B (en) | 2006-11-10 | 2006-11-10 | Method for enriching active ingredient of seal oil |
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| CN2006101546140A CN101177649B (en) | 2006-11-10 | 2006-11-10 | Method for enriching active ingredient of seal oil |
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| CN101177649B true CN101177649B (en) | 2010-08-11 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544557B (en) * | 2009-05-05 | 2012-11-14 | 天津大学 | Coupling rectification system and application thereof in purifying EPA, DPA, and DHA in seal oil |
| CN102551041A (en) * | 2010-12-08 | 2012-07-11 | 浙江金诺康生物制药有限公司 | Refined seal oil, seal oil soft capsules and application of seal oil soft capsules in preparing health products for improving chemical liver injury |
| CN102138936B (en) * | 2011-03-29 | 2013-03-13 | 江苏省中医院 | Yellow dog penis extractive with resistance to ovarian function progeria as well as preparation method and applications thereof |
| 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 |
| CN110129131A (en) * | 2019-05-06 | 2019-08-16 | 嘉必优生物技术（武汉）股份有限公司 | Reduce the device and method of low iodine number content of fatty acid in grease |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757395A (en) * | 2004-10-09 | 2006-04-12 | 中国药品生物制品检定所 | Pure ursine fat, and its prepn. method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1757395A (en) * | 2004-10-09 | 2006-04-12 | 中国药品生物制品检定所 | Pure ursine fat, and its prepn. method |
Non-Patent Citations (6)
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| 林兰等.海狗油多烯脂肪酸的开发利用.药学进展26 1.2002,26(1),30-32. |
| 林兰等.海狗油多烯脂肪酸的开发利用.药学进展26 1.2002,26(1),30-32. * |
| 肖红卫等.多价不饱和脂肪酸分离方法及在橡胶籽油中的应用.云南化工27 1.2000,27(1),26-28. |
| 肖红卫等.多价不饱和脂肪酸分离方法及在橡胶籽油中的应用.云南化工27 1.2000,27(1),26-28. * |
| 许松林等.分子蒸馏提纯α- 亚麻酸的研究.化学工业与工程21 1.2004,21(1),25-28. |
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