Method for extracting high-purity Alpha-ethyl linolenate from silkworm chrysalis oil

A technology of ethyl linolenate and silkworm chrysalis oil, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds. It can solve the problems of easy pollution, weakened selectivity, and reduced processing capacity, and reduce production costs. , improve stability, increase selectivity effect

Active Publication Date: 2010-01-13
ZHEJIANG UNIV OF TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

And for silkworm chrysalis oil, α-linolenic acid content is not high (only 20-30%), cuprous ion selectivity is low, easy to pollute, and the problem that adsorption capacity is little just highlights, so separation efficiency is not high, selectivity weakens, The p

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  • Method for extracting high-purity Alpha-ethyl linolenate from silkworm chrysalis oil
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  • Method for extracting high-purity Alpha-ethyl linolenate from silkworm chrysalis oil

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Experimental program
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Effect test

Embodiment 1-4

[0028] Solvent extraction and pretreatment of embodiment 1-4 silkworm chrysalis oil

[0029] Place the silkworm chrysalis at 85-90°C for 3 hours in vacuum, mechanically pulverize to 60-80 mesh, then accurately weigh 100g of dry silkworm chrysalis powder, according to the material-liquid ratio of silkworm chrysalis mass and solvent volume is 1:10g / ml, add solvent, ultrasonic Extract (45KHz) for 30 minutes, concentrate in vacuo, weigh and calculate silkworm chrysalis oil content (dry weight), and the reaction conditions and yields are shown in Table 1.

[0030] Table 1. Ultrasonic-assisted extraction of silkworm chrysalis oil by different solvents

[0031]

[0032] Ultrasonic-assisted extraction is carried out at room temperature, with mild conditions and good product quality. High extraction efficiency can significantly reduce extraction time. The effects of different solvents are quite different, and the extraction rate of chloroform / methanol is the highest, bu...

example 5-16

[0033] Example 5-16 Ultrasonic-assisted research on ethyl esterification of silkworm chrysalis oil

[0034] Prepare silkworm chrysalis oil according to the method of Example 3, then react with ethanol and catalyst sodium ethylate according to the reaction conditions in Table 2, after the reaction is finished, wash with water, leave to stand for layering, take the organic phase and distill under reduced pressure to remove the solvent, and obtain silkworm chrysalis Mix fatty acid ethyl esters; the added mass of sodium ethoxide is 2.15g. The reaction results are shown in Table 2.

[0035] Table 2 Ethyl esterification of silkworm chrysalis oil under different ultrasonic conditions

[0036]

[0037] Note: The molar ratio of ethanol / silkworm chrysalis oil is about 10:1, sodium ethoxide is the catalyst, and the amount added is 1% of the oil mass.

[0038] The data shows that ultrasonic waves are significantly better than traditional mechanical stirring, and the conve...

example 21-25

[0044] Example 21-25 Study on the separation of α-linolenic acid by silver tetrafluoroborate column chromatography

[0045] Silver ion silica gel is prepared as follows: 50g silica gel (100-120 mesh, surface area 127.85m 2 g -1 ) in ethanol (20mL, 10min), add 150mL silver tetrafluoroborate ethanol solution (5g silver tetrafluoroborate dissolved in 150mL70wt% ethanol aqueous solution) and stir continuously for 10min, and evaporate the ethanol to dryness in a water bath under the protection of nitrogen to obtain free-flowing adsorption Silica gel with silver ions, then dried overnight at 80°C, activated to obtain silica gel with silver ions. Cool and store in a brown bottle for dry storage. Wet column packing (glass chromatographic column 19mm x 30cm, packing height 5cm) was used to obtain a silver ion adsorption column.

[0046] Take 1.0 mL of silkworm chrysalis mixed fatty acid ethyl esters prepared above, dissolve in 5 mL of n-hexane, add silver ion adsorption colu...

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Abstract

The invention provides a method for extracting high-purity Alpha-ethyl linolenate from silkworm chrysalis oil, which realizes the separation of the high-purity Alpha-ethyl linolenate from mixed fatty acid by a complexing absorbing agent of metal ions and comprises the following steps: firstly, performing alcoholysis on the silkworm chrysalis oil under the help of ethanol ultrasonically to preparesilkworm chrysalis mixed ethyl fatty acid; secondly, passing the silkworm chrysalis mixed ethyl fatty acid through a pre-saturated complexing absorption column of metal ions of competitive absorbent,wherein saturated fatty acid and monounsaturated fatty acid freely pass, and polyunsaturated fatty acid and silver ions form a Pi compound; and thirdly, changing elution solvent for eluting. The purity of the obtained Alpha-ethyl linolenate is 95-99 percent.

Description

(1) Technical field [0001] The invention relates to a method for extracting high-purity alpha-linolenic acid ethyl ester from silkworm chrysalis oil. (two) background technology: [0002] α-linolenic acid, C18: 3 n-3, is an essential fatty acid for the human body, and it is also a precursor for the synthesis of DHA and EPA in the human body. It is a functional factor for both medicine and food, and is used in medicine, food, cosmetics and other fields. α-linolenic acid has a wide range of physiological functions, including: 1. Regulating "three highs" (hyperlipidemia, hypertension, hyperglycemia); 2. Improving liver function and restoring chemical liver damage; 3. Preventing cardiovascular and cerebrovascular diseases , Anti-platelet aggregation, prevent myocardial infarction and cerebral infarction, inhibit cerebral hemorrhage; 4. Resist HIV <hiv>5. Reduce the ability of germs to invade and effectively prevent prostatitis; 6. Improve various inflammations, prevent as...

Claims

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Application Information

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IPC IPC(8): C07C69/587C07C67/56
Inventor 孟祥河潘秋月孙培龙张安强
Owner ZHEJIANG UNIV OF TECH
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