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A kind of enrichment method of polyunsaturated fatty acid in oil

A technology for unsaturated fatty acids and oils, applied in the field of enrichment of polyunsaturated fatty acids, can solve the problems of complex steps and high cost of enzyme preparations, and achieve the effects of mild conditions and low energy consumption

Active Publication Date: 2022-03-15
青岛斯八达分析测试有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patents 201710621797.0 and 201710667021.2 respectively disclose the method of enriching polyunsaturated fatty acids from vegetable oils by using urea embedding method. Patent 201210247842.8 also discloses a similar method. Using urea embedding method can obtain DHA and other polyunsaturated fatty acids with a purity of 90%. Fatty acid, but the steps are relatively complicated, and attention should also be paid to the residue of urea in the product; 201510757500.4 discloses a method for enriching n3 polyunsaturated fatty acids from fish oil by enzymatic method using lipase, and patents 201310161447.2 and 201210134054.8 also disclose similar methods , the enzymatic method avoids the use of chemical reagents, but the cost of the enzyme preparation is relatively high; 201510196920.X proposed a method of enriching polyunsaturated fatty acids by using acetonitrile as a solvent and using multiple crystallization methods. Content increased by 50-90%, but the product needs to be handled carefully to avoid toxic acetonitrile residues

Method used

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  • A kind of enrichment method of polyunsaturated fatty acid in oil
  • A kind of enrichment method of polyunsaturated fatty acid in oil
  • A kind of enrichment method of polyunsaturated fatty acid in oil

Examples

Experimental program
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Effect test

Embodiment 1

[0042] Embodiment 1: Preparation of Fe-MOF74 particles

[0043] (1) 288 grams of Fe(NO 3 ) 2 .6H 2O and 553 grams of 2,5-dimethylolterephthalic acid were dissolved in 5 L of solvent prepared from ethanol, water and N,N dimethylformamide (DMF) in a volume ratio of 1:2:2 It is formed, bubbled with argon for 15 minutes to remove the air in the solution, then sealed the solution and heated at 100°C for 24 hours, cooled to room temperature, filtered, and the solid powder product was repeatedly soaked and extracted with methanol 4 times, each time using 5L Soak in methanol for 12 hours, then dry the solid powder product at 150°C for 6 hours, and finally obtain 602.5 grams of the product, and use a pulverizer to crush it to 50 meshes to obtain an iron-terephthalic acid organometallic framework compound (Fe-MOF74). The pore size is about 1.46nm, and the specific surface area is 1020m 2 / g.

[0044] (2) Take 500 grams of Fe-MOF74 powder and add it to the swing granulator. After op...

Embodiment 2

[0048] Embodiment 2: Preparation of Zn-MOF74 particles

[0049] (1) 299 grams of Zn(NO 3 ) 2 .6H 2 O and 594 grams of 2,5-dihydroxybutyl terephthalic acid were dissolved in 6 L of solvent prepared from ethanol, water and N,N dimethylformamide (DMF) in a volume ratio of 1:1:1 It is formed, bubbled with argon for 15 minutes to remove the air in the solution, then sealed and placed at 120 ° C for 12 hours, cooled to room temperature, filtered, and the solid powder product was repeatedly soaked and extracted with methanol twice, each soaked in 8L of methanol 8h, then dry the solid powder product at 120°C for 12h, and finally obtain 704.6 grams of the product, use a pulverizer to crush it to 100 mesh, and obtain the zinc-terephthalic acid organometallic framework compound (Zn-MOF74), the pore size The size is about 1.42nm, and the specific surface area is 1130m 2 / g.

[0050] (2) Take 500 grams of Zn-MOF74 powder, add it to the swing granulator, and slowly spray 150 mL of sodi...

Embodiment 3

[0053] Example 3 Enrichment of DHA in Schizochytrium algae oil

[0054] Get 500 grams of Fe-MOF74 particles prepared in Example 1 and fill them into a glass tube for column chromatography with a diameter of 60 mm, then slowly add 250 mL of Schizochytrium algae oil (containing DHA 40%) from the mouth of the tube, fill the glass tube and After immersing the Fe-MOF74 particles, let it stand for 2 hours, then release the adsorbed oil, collect the Fe-MOF74 adsorption material, put the adsorption material in a high-speed centrifuge for centrifugation at a speed of 8000r / min, and centrifuge for 10 minutes to collect and enrich DHA The Schizochytrium algae oil was 200mL with a DHA content of 50%. The DHA content in the oil was tested according to the national standard GB5009.168; the enrichment operation was repeated three times to obtain 85mL of the Schizochytrium algae oil rich in DHA with a DHA content of 75%.

[0055] After centrifugation, the Fe-MOF74 adsorption material can be r...

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Abstract

The invention discloses a method for enriching polyunsaturated fatty acids in oil, which comprises the following steps: 1) preparation of organometallic framework compound (MOF); 2) preparation of MOF particles: pulverize the prepared MOF, and then add viscose The mixture is granulated to obtain MOF particles; 3) Enrichment of polyunsaturated fatty acids in oil: fill the MOF particles prepared in step 2) into the adsorption column, add the oil to be separated into the adsorption column, and after standing Collect MOF particles of the adsorption material and centrifuge to obtain oil rich in polyunsaturated fatty acids; repeat this step at least three times to obtain oil rich in polyunsaturated fatty acids. The present invention adopts the method of MOF adsorption for the first time to enrich the polyunsaturated fatty acid in the oil, and can obtain the oil with various enrichment degrees. The invention has mild conditions, the MOF adsorption material can be reused, the energy consumption is low, and the problem of chemical reagent residue does not exist.

Description

technical field [0001] The invention relates to a method for enriching polyunsaturated fatty acids, in particular to a method for enriching polyunsaturated fatty acids in oil. Background technique [0002] Polyunsaturated fatty acids usually refer to a class of fatty acids containing two or more conjugated or non-conjugated double bonds, mainly in the form of triglycerides in fats from animals, plants and microorganisms. Polyunsaturated fatty acids are It is considered to have an important relationship with the normal metabolism of the human body, and has specific physiological regulatory functions such as anti-inflammatory response, anti-oxidation and lowering high-density lipoprotein. [0003] Typical polyunsaturated fatty acids can be divided into n3, n6 and n9 according to the position of their double bonds. Linolenic acid belonging to n3 type is one of the two essential fatty acids for human body; it is added to infant milk powder as a nutritional enhancer DHA (docosah...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30C11C1/02B01D15/08
CPCB01J20/226C11C1/02B01D15/08
Inventor 赵澎韩香莲张璟吕海金
Owner 青岛斯八达分析测试有限公司
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