CN102051268A - Method for preparing fish oil PUFA ethyl ester - Google Patents
Method for preparing fish oil PUFA ethyl ester Download PDFInfo
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- CN102051268A CN102051268A CN2009102296517A CN200910229651A CN102051268A CN 102051268 A CN102051268 A CN 102051268A CN 2009102296517 A CN2009102296517 A CN 2009102296517A CN 200910229651 A CN200910229651 A CN 200910229651A CN 102051268 A CN102051268 A CN 102051268A
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- fish oil
- ethyl ester
- hexanaphthene
- added
- ethanol
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for preparing fish oil PUFA (polyunsaturated fatty acid) ethyl ester. The method comprises the following steps: (1) fish oil and ethanol with a certain proportion are added into a closed retort, a proper amount of sulfuric acid is added to serve as catalyst, and under nitrogen protection, refluxing is carried out for 4 to 5 hours in the temperature of 75 to 80 DEG C; and (2) after reaction, substance in the closed retort is cooled down to the room temperature, water and cyclohexane are added into the closed retort, stirred for 20 to 30 minutes and then left to stand, water phase is abandoned, the cyclohexane layer is washed for 3 to 5 times to achieve neutrality, anhydrous calcium chloride is utilized for dehydration, and at last, cyclohexane is removed through vacuum evaporation to produce fish oil PUFA ethyl ester. In the method provided by the invention, fish oil and ethanol can directly carry out transesterification reaction, so that saponification reaction is omitted, and products with a higher purity can be produced with a lower cost.
Description
Technical field
The present invention relates to a kind of preparation of ester, particularly a kind of preparation method of fish oil PUFA ethyl ester.
Background technology
Fish oil is the general designation of the intravital whole oily substances of fish, and it comprises body oil, liver oil and cerebrol.Fish oil is the byproduct of fish meal processing, and fish and waste thereof obtain with separating through steaming, squeezing.Fish oil is rich in multiple polyunsaturated fatty acid, and (poly-unsaturated fatty acid, PUFA), it is the street cleaner of human vas, can also the prevention of arterial sclerosis, apoplexy and heart trouble.Fish oil is that disease patients such as hypertension, coronary heart disease, cerebral apoplexy, diabetes, rheumatic arthritis, cancer are first-selected healthcare products.Fish oil also has the effect that suppresses platelet aggregation.
PUFA mainly is present in the marine organisms with the form of triglyceride level, and commodity PUFA preparation generally is to extract fish oil earlier from ocean fish or its tankage at present, produces PUFA through separation and purification again, and it is made dripping pill or capsule and pill.Need first esterification in the purge processes such as PUFA distills, to increase volatility.Esterification method after the first saponification is adopted in the preparation of PUFA ethyl ester at present more, and this kind method cost is bigger, easily introduces impurity.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of fish oil PUFA ethyl ester.
The technical scheme that the present invention takes is:
A kind of preparation method of fish oil PUFA ethyl ester may further comprise the steps:
(1) a certain proportion of fish oil and ethanol are added in the airtight retort, add an amount of sulfuric acid as catalyzer, 75-80 ℃ of reflux 4-5h under nitrogen protection;
(2) reaction is chilled to room temperature after finishing, and adds entry and hexanaphthene and stirs 20-30min, leave standstill, and aqueous phase discarded, washing hexanaphthene layer 3-5 time is to neutral, and with the Calcium Chloride Powder Anhydrous dehydration, hexanaphthene is sloughed in vacuum-evaporation at last, makes fish oil PUFA ethyl ester.
The described fish oil of step (1), ethanol and vitriolic mass ratio are 40: 20: 1.
Described water of step (2) and hexanaphthene consumption are respectively 1.5-2 times and 1-1.3 times of fish oil quality.
The inventive method fish oil can directly carry out transesterification reaction with ethanol, has saved the saponification reaction step, and available less cost makes the higher product of purity.
Embodiment
Embodiment 1
A kind of preparation method of fish oil PUFA ethyl ester may further comprise the steps:
(1) 100g fish oil and 50g ethanol are added in the airtight retort, add 2.5g sulfuric acid as catalyzer, 75 ℃ of reflux 4h under nitrogen protection;
(2) be chilled to room temperature after reaction finishes, add 150g water and 100g hexanaphthene and stir 20min, leave standstill, aqueous phase discarded, washing hexanaphthene layer is to neutral, and with the Calcium Chloride Powder Anhydrous dehydration, hexanaphthene is sloughed in last vacuum-evaporation, makes fish oil PUFA ethyl ester.
Embodiment 2
A kind of preparation method of fish oil PUFA ethyl ester may further comprise the steps:
(1) 200g fish oil and 100g ethanol are added in the airtight retort, add 5g sulfuric acid as catalyzer, 80 ℃ of reflux 5h under nitrogen protection;
(2) be chilled to room temperature after reaction finishes, add 400g water and 260g hexanaphthene and stir 20min, leave standstill, aqueous phase discarded, washing hexanaphthene layer is to neutral, and with the Calcium Chloride Powder Anhydrous dehydration, hexanaphthene is sloughed in last vacuum-evaporation, makes fish oil PUFA ethyl ester.
Embodiment 3
A kind of preparation method of fish oil PUFA ethyl ester may further comprise the steps:
(1) 100g fish oil and 50g ethanol are added in the airtight retort, add 2.5g sulfuric acid as catalyzer, 80 ℃ of reflux 4h under nitrogen protection;
(2) reaction is chilled to room temperature after finishing, and adds 200g water and 100g hexanaphthene and stirs 30min, leave standstill, and aqueous phase discarded, washing hexanaphthene layer 3-5 time is to neutral, and with the Calcium Chloride Powder Anhydrous dehydration, hexanaphthene is sloughed in vacuum-evaporation at last, makes fish oil PUFA ethyl ester.
Embodiment 4
A kind of preparation method of fish oil PUFA ethyl ester may further comprise the steps:
(1) 200g fish oil and 100g ethanol are added in the airtight retort, add 5g sulfuric acid as catalyzer, 80 ℃ of reflux 4h under nitrogen protection;
(2) be chilled to room temperature after reaction finishes, add 350g water and 250g hexanaphthene and stir 30min, leave standstill, aqueous phase discarded, washing hexanaphthene layer is to neutral, and with the Calcium Chloride Powder Anhydrous dehydration, hexanaphthene is sloughed in last vacuum-evaporation, makes fish oil PUFA ethyl ester.
Claims (1)
1. the preparation method of a fish oil PUFA ethyl ester is characterized in that may further comprise the steps:
(1) a certain proportion of fish oil and ethanol are added in the airtight retort, add an amount of sulfuric acid as catalyzer, 75-80 ℃ of reflux 4-5h under nitrogen protection;
(2) reaction is chilled to room temperature after finishing, and adds entry and hexanaphthene and stirs 20-30min, leave standstill, and aqueous phase discarded, washing hexanaphthene layer 3-5 time is to neutral, and with the Calcium Chloride Powder Anhydrous dehydration, hexanaphthene is sloughed in vacuum-evaporation at last, makes fish oil PUFA ethyl ester.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102296517A CN102051268A (en) | 2009-10-30 | 2009-10-30 | Method for preparing fish oil PUFA ethyl ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102296517A CN102051268A (en) | 2009-10-30 | 2009-10-30 | Method for preparing fish oil PUFA ethyl ester |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102051268A true CN102051268A (en) | 2011-05-11 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102296517A Pending CN102051268A (en) | 2009-10-30 | 2009-10-30 | Method for preparing fish oil PUFA ethyl ester |
Country Status (1)
| Country | Link |
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| CN (1) | CN102051268A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087158A (en) * | 2015-09-16 | 2015-11-25 | 荣成爱尔斯海洋生物科技有限公司 | Method for lowering acid value in ethyl-ester-type fish oil refinement process |
| CN106675775A (en) * | 2016-12-29 | 2017-05-17 | 山东禹王制药有限公司 | Method for removing cholesterol in fish oil by subcritical extraction |
| CN106753817A (en) * | 2016-12-30 | 2017-05-31 | 山东禹王制药有限公司 | A kind of industrialized preparing process of highly unsaturated fatty acid fish oil |
-
2009
- 2009-10-30 CN CN2009102296517A patent/CN102051268A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105087158A (en) * | 2015-09-16 | 2015-11-25 | 荣成爱尔斯海洋生物科技有限公司 | Method for lowering acid value in ethyl-ester-type fish oil refinement process |
| CN106675775A (en) * | 2016-12-29 | 2017-05-17 | 山东禹王制药有限公司 | Method for removing cholesterol in fish oil by subcritical extraction |
| CN106753817A (en) * | 2016-12-30 | 2017-05-31 | 山东禹王制药有限公司 | A kind of industrialized preparing process of highly unsaturated fatty acid fish oil |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20110511 |