KR900002920B1 - A process for the rebining of sundrops oil - Google Patents

Abstract

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Description

Method of Purifying Evening Primrose Oil

The present invention relates to a method for extracting and purifying evening primrose oil of high purity from a evening primrose seed in a more stable manner.

Evening primrose seeds, as known (JAOCS. Vol, 61, March 1984), contain about 15% protein, 43% cellulose and 24% oil, of which evening primrose oil contains 16 to 18 saturated and unsaturated carbon atoms. It is made up of fat. That is, almost all of them consist of unsaturated fats, such as linoleic acid (65-80%), gamma-linolenic acid (8-14%) and oleic acid (6-11%), and thus evening primrose oil containing these unsaturated fats ( Wol dog colostrum) is very difficult and difficult to purify the purification process by a conventionally known method has been developed a variety of refining techniques to solve this problem is poor quality or poor yield easily due to poor quality and stability of the product.

For example, JAOCS. Vol, 61, No. 3 March 1984 describes a method of crushing evening primrose seeds using a roller, immersing it in normal hexane, extracting oil, and washing it to remove gum material contained in evening primrose oil, and evaporating and evaporating the solvent under reduced pressure. It is described. However, this method has the drawback that only the test substance is removed, and not only peroxide and free fatty acid, which cause the degeneration of evening primrose oil, but also color cannot be removed. Therefore, the present invention was invented in view of the above-mentioned drawbacks, which is characterized by decolorizing the evening primrose oil and selectively separating and removing peroxides and free fatty acids. The explanation is as follows.

1. Extraction process

Selected evening primrose seeds were crushed using a roller circulating with cooling water, and 1 L to 4 L of normal hexane (hereinafter referred to as n-hexane) was added to 1 kg of the crushed seeds, followed by stirring at room temperature for at least 30 minutes, followed by filtration. Obtain an extract containing evening primrose oil.

2. Decolorization Process

Activated charcoal or activated clay is added to the extract containing n-hexane from the extraction process, and 1-20% by weight of evening primrose oil is stirred and filtered at room temperature for 30 minutes or more. By decolorizing the solution in this way to prevent the loss of evening primrose oil by adsorption, easy stirring and filtration to produce a high-quality evening primrose oil as shown in Table 1.

[Table 1] Bleaching Effect of Evening Primrose Oil

Note: 1) By Gardner colorimetric method

3. Ion Exchange Process

end. Ion Exchange Resin Preparation Process

Porous ion exchange resin made of a copolymer of styrene and divinylbenzene. The cationic resin is made of Na as the active group and the anionic resin is made of Cl. After sufficiently washing the ion exchange resin tower with ethyl alcohol having a purity of 80% or more, it is washed again with n-hexane to prepare the ion exchange resin tower in the hexane solvent state.

I. Ion exchange treatment method

Passing the decolorized evening primrose oil extract through an ion exchange column at room temperature, the free fatty acid, which is the main cause of rancidity, is replaced and removed by the ion exchange resin through the following process.

Free Fatty Acids:

Cationic resin: -SO ₃ Na + H ⁺ → -SO ₃ H + Na ⁺

Anion ^{_{resin: -NR '3 Cl + RCOO -}} → -NR' 3 OCOR + Cl -

(R ': methyl group, R: alkyl group)

Therefore, the pH of the extract can be selectively removed without thermal manipulation of fatty acids and peroxides contained in the solution without changing the high purity, high quality extract can be prepared as shown in Table 2.

[Table 2] Ion Exchange Effect of Evening Primrose Oil

Note: 1) The sample used is an extract bleached with 10% activated carbon.

All. Ion exchange resin regeneration process

Resin that has been depleted in ion exchange capacity can be recycled and used continuously That is, in the reverse order of the preparation process, the resin tower in the n-hexane solvent state is sufficiently washed with ethyl alcohol having a purity of 80% or more, and washed again with water, and then regenerated by a conventional ion exchange resin regeneration method.

4. Evaporative Concentration Process

The ion exchange-extracted extract is removed by using a precision filter of 1.2 ㎛ or less, and concentrated by evaporation at high vacuum above 755mmHg vacuum and below 50 ℃ to obtain n-hexane to obtain pure evening primrose oil. By using the evening primrose oil refining method, it is possible to solve the rancidity problem caused by peroxides and free fatty acids, which have occurred when using a conventionally known method. High-purity evening primrose oil can be produced at a price.

Example 1

1 kg of selected evening primrose seeds were crushed using a two-stage roll mill with cooling water circulated, and 2 liters of n-hexane were added thereto, stirred at room temperature for 30 minutes, and 20 g of activated carbon was added to the filtered extract and stirred for 30 minutes. Decolorize and filter. The decolorized solution was passed through a 35 mm diameter ion exchange resin column filled with 0.2 l of cationic resin with Na active group and 0.4 l of anionic resin with Cl active group at a flow rate of 20 ml per minute, followed by precise filtration of 1.2 μm or less. N-hexane was evaporated at 755 mmHg vacuum and 45 ° C. to obtain approximately 200 g of evening primrose oil as shown in Table 3.

Example 2

1 kg of selected Evening Primrose seeds were crushed using a two-stage roll mill with cooling water circulated, and 3 liters of n-hexane were added thereto, stirred at room temperature for 1 hour. Stirring decolorize and filter.

The decolorized solution was passed through an ion exchange resin tower filled with 0.2 l of cationic resin with Na active group and 0.4 l of anionic resin with Cl active group at a flow rate of 15 ml per minute, followed by precise filtration of 1.2 μm or less, and then vacuum 755 mmHg. After evaporating n-hexane at 45 ° C., about 220 g of evening primrose oil was obtained as shown in Table 3.

[Table 3] Evening Primrose Oil Purification Effect in Examples 1 and 2

Note: 1) JAOCS. Vol, 61, No. In accordance with the method of 3 March 1984

Claims (3)

A method of purifying evening primrose oil by dissolving evening primrose oil in normal hexane and discoloring it with activated carbon or activated clay and then passing it through an ion exchange resin tower filled with a cation exchange resin and an anion exchange resin. The method for purifying evening primrose oil according to claim 1, wherein the cation exchange resin has Na as an active group and the anion exchange resin as Cl. The method for purifying evening primrose oil according to claim 1, wherein the ion exchange resin tower in an aqueous solution is washed with ethyl alcohol having a purity of 80% or more, and then washed again with normal hexane and then passed through a decolorized evening primrose oil.