Supercritical CO2 extraction separation purification method for silkworm chrysalis alpha-linolenic acid

A technology for separation and purification of linolenic acid, which is used in the separation/purification of carboxylic acid compounds, organic chemistry, fatty acid production, etc., can solve the problems of low extraction rate, high cost, and large degree of damage to α-linolenic acid, and achieve product quality. The effect of high purity, simple and convenient operation, and short extraction time

Inactive Publication Date: 2008-02-13
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The invention provides a method for separating and purifying α-linolenic acid from silkworm chrysalis, aiming to solve the disadvantages of low extraction rate, large degree of damage to α-linolenic acid, and high cost in traditional extraction and purification methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] a. Using natural biological silkworm chrysalis as raw material, take silkworm chrysalis and pulverize and dry to obtain dry powder, take 300g of dry powder and put it in a 1L extraction kettle, and use supercritical CO 2 As an extractant, extract for 2.5 hours at an extraction pressure of 25MPa and an extraction temperature of 55°C; analyze at an analysis pressure of 6.0MPa and an analysis temperature of 40°C to obtain pupal oil.

[0022] b. Take pupae oil and place it in a kettle, add a sodium hydroxide ethanol solution with a concentration of 3.5% (w / v), stir at 65°C for 2 hours, add water until the solution is clear, adjust the pH to 2.5, and extract the solution with n-hexane, The n-hexane layer was washed with water until neutral, and dried to obtain mixed fatty acids.

[0023] c. Add the mixed fatty acid into the methanol solution with a concentration of 30%wt urea according to the mass ratio of mixed fatty acid and urea of ​​1:3, stir and clathrate at -20°C for 2...

Embodiment 2

[0025] a. Using natural biological silkworm chrysalis as raw material, take silkworm chrysalis and pulverize and dry to obtain dry powder, take 300g of dry powder and put it in a 1L extraction kettle, and use supercritical CO 2 As an extractant, extract for 0.5h at an extraction pressure of 20MPa and an extraction temperature of 40°C; analyze at an analysis pressure of 4.0MPa and an analysis temperature of 30°C to obtain pupal oil.

[0026] b. Take pupae oil and place it in a kettle, add a sodium hydroxide ethanol solution with a concentration of 4.5% (w / v), stir at 30°C for 24 hours, add water until the solution is clear, adjust the pH to 1.0, and extract the solution with n-hexane, The n-hexane layer was washed with water until neutral, and dried to obtain mixed fatty acids.

[0027] c. Add the mixed fatty acid into the methanol solution with a concentration of 20%wt urea according to the mass ratio of the mixed fatty acid and urea of ​​1:1, stir and clathrate at -15°C for 3...

Embodiment 3

[0029] a. Using natural biological silkworm chrysalis as raw material, take silkworm chrysalis and pulverize and dry to obtain dry powder, take 300g of dry powder and put it in a 1L extraction kettle, and use supercritical CO 2 As an extractant, extract for 5.0 hours at an extraction pressure of 40MPa and an extraction temperature of 60°C; analyze at an analysis pressure of 12MPa and an analysis temperature of 60°C to obtain pupal oil.

[0030] b. Take pupae oil and put it in a kettle, add 6% (w / v) sodium hydroxide ethanol solution, stir at 75°C for 0.5h, add water until the solution is clear, adjust the pH to 5.0, and extract the solution with n-hexane , wash the n-hexane layer with water until neutral, and dry to obtain mixed fatty acids.

[0031] c. Add the mixed fatty acid into the methanol solution with a concentration of 55%wt urea according to the mass ratio of the mixed fatty acid and urea of ​​1:12, stir and clathrate at -40°C for 12h, filter, wash the filter residue ...

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Abstract

The invention relates to an extraction and purification method of the pupa alpha-linolenic acid with the supercritical CO2 technology. The natural biological pupa powder is used as the raw material; the supercritical CO2 is used as the extraction agent to get the pupa oil; the pupa oil is added into the sodium hydroxide alcohol solution, and then to be stired, water-added and clarified; besided, the pupa oil is extracted by the organic solvent; the mixed fatty acid and urea are put into the urea methanol solution; at minus 15 to minus 20 Celsius system, and then to be stired 12 to 36 hours, next to be filtered and washed with the methanol;finally, the product is dried and the product can be got. The invention can be operated at a low temperature, avoiding the damage to the polyunsaturated fatty acid; the purity of the product quality is high and the extraction time is short; the operation is simple and convenient; compared with the traditional solvent method and squeezing method, the collection rate is high and the efficiency is high; the CO2 can be reused; no solvent is left; the product quality is high; the invention can be used in the mass production of the industrial mechanization.

Description

Technical field: [0001] The invention relates to a method for extracting and purifying natural bioactive components, in particular to a silkworm chrysalis α-linolenic acid supercritical CO 2 Extraction, separation and purification method. Background technique: [0002] Physiological and pharmacological effects and applications of pure natural biological silkworm chrysalis α-linolenic acid. α-Linolenic acid (α-Linolenic acid, α-LNA) is the core substance of human life. It is an omega-3 series polyunsaturated fatty acid. Neurophospholipid transformation, the core substance of metabolic functions, is a good donor of omega-3 series polyene fatty acids EPA and DHA in the body. α-LNA cannot be synthesized in the human body and must be taken from the outside. In March 1990, at the International Conference on ω-3 Series Polyunsaturated Fatty Acids in Washington, DC, it was confirmed that α-LNA is an "essential fatty alcohol" that is very important to the human body. As early as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C57/12C07C51/42C11C1/00
CPCY02P20/54
Inventor 邓树海张四喜常建晖
Owner SHANDONG UNIV
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