JPS59176384A - Preparation of antioxidant - Google Patents

Abstract

PURPOSE:To prepare an antioxidant with a high content of antioxidant components, by treating a solution extracted from spices with a non-polar organic solvent, with an aqueous solution of alkali, with an acid and then with a non- polar organic solvent to remove unnecessary ingredients effectively. CONSTITUTION:An aqueous solution of alkali (e.g. NaOH) is added to a solution extracted from spices (e.g. olegano, sapori, thyme, sage or rosemary) with a non- polar organic solvent. The resultant water layer is taken out and an acid (e.g. sulfuric acid) is added to it. The a non-polar organic solvent is added and after washing of the solvent layer with water to bring its pH to almost neutral, the solvent is removed, e.g., by heating to the boiling point of the solvent, followed by collection of residues by steam distillation to obtain an antioxidant which is almost free from smell and taste peculiar to spice and has an excellent antioxidant action.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for obtaining natural antioxidants from spices, which are useful for preventing the oxidation of oils and fats.

It has long been known that spices have antioxidant properties, and many research reports have been published. However, spice o'
has a unique flavor, so it has not been possible to use the spice as it is or extract it from the spice with a solvent as an antioxidant.

As a method to solve these problems, a method has been developed in which solvent extraction from spices is treated with an adsorbent.

According to this method, it is possible to remove the flavor of the blind pieces to some extent and to obtain a relatively excellent antioxidant product, but the uninventive old people are not satisfied with this fact and are not satisfied with this fact. We conducted research to obtain an excellent antioxidant. As a result, by subjecting the liquid extracted from spices with a non-polar organic solvent to aqueous alkali treatment, acidic treatment, and caustic solvent treatment, it is possible to achieve the purpose described in item 1. I got 1U of knowledge.

The gist of the present invention, which was completed based on the above knowledge, is to add an alkaline aqueous solution to the liquid extracted from spices with a non-polar organic solvent, take out the resulting aqueous layer, add an acidic agent to it, and then An antioxidant characterized by adding an organic solvent, washing the resulting solvent layer with water to make the pH neutral, and then performing a solvent removal treatment, followed by steam distillation to collect the residue. This is the manufacturing method.

The contents of the present invention will be described in detail below.

The spices used in the present invention include all spices that have antioxidant properties, such as orecano, shibori, thyme, marshoram, zege, and rosemary.

In the present invention, these spices are extracted with a non-polar organic solvent to obtain an extract. The spices to be extracted with non-polar organic solvents may be powders or residues after extraction, or even the residues extracted with various solvents.
J: Yes. The point is that there are antioxidant ingredients in spices.
Extract it with a non-polar organic solvent? If you want to
It may also be in the form of . Further, as the nonpolar organic solvent that can be used, commonly used ones such as diethyl ether, chloroborum, petroleum ether, and hexane are sufficient. The liquid extracted with the non-polar solvent contains a large amount of antioxidant components.

Next, an alkaline aqueous solution is added to the above extract and thoroughly shaken and mixed. This treatment makes the antioxidant components in the extract water-soluble. After that, it is left to stand and fractionated into a water layer and a solvent layer, and only the water layer is taken out. On the other hand, the bath medium layer 811 contains fat-soluble components such as chloronoyl contained in spices and essential oils.The alkaline aqueous solution used in the above treatment is an aqueous solution of notrium hydroxide. In addition, the amount of the alkali aqueous solution added may vary depending on the concentration of the alkali agent, or may be adjusted so that the P l-1 of the mixture of the extract and the alkali aqueous solution is 8.0 or more. Good to have.

Next, an acidic agent is added to the water layer taken out, but before that (
If necessary, the aqueous layer may be treated with a nonpolar organic solvent. That is, a non-polar organic solvent is added to the water layer, shaken and mixed, and then statically bought to separate into 1n parts of water and a solvent layer. After that, only the aqueous layer was removed. This treatment makes it possible to remove fat-soluble components such as chlorophyll and essential oils that remain slightly in the aqueous layer.

An acidic agent such as sulfuric acid and W-phosphoric acid is added to the aqueous layer thus obtained to make the aqueous layer acidic. This insolubilizes the antioxidant components dissolved in the aqueous layer. When implementing this, it is preferable to keep the pH of the aqueous layer below 5.

Thereafter, a non-polar organic solvent is added to transfer the insolubilized antioxidant component to the non-polar organic solvent.

Then, take out only the solvent layer and its pH is almost neutral.
Repeat the washing with water until it gets close to normal. Thereafter, it is treated with an IBM solvent under reduced pressure or under a pressure of 7°C and heated at a temperature near the boiling point of the solvent. The concentrate thus obtained is steam distilled by a conventional method to collect the residue. In addition, before steam distillation, alcohol is added to the concentrate and the -
After dissolving the concentrate, decolorization treatment is performed by adding activated carbon and refluxing, etc. to obtain -6. The residue thus collected is the antioxidant targeted by the present invention.

As described above, according to the method of the present invention, unnecessary components such as essential oils and chlorophyll in spices are removed by treating the liquid extracted from spices with a non-polar organic solvent by aqueous alkali treatment, acidic agent treatment J5, and non-polar organic solvent treatment. It is possible to effectively remove oxidants and use an antioxidant containing a large amount of antioxidant components. Therefore, the resulting antioxidant has excellent antioxidant capacity. Furthermore, according to the method of the present invention, flavor components in spices are also effectively removed, so that the antioxidants produced do not have the flavor characteristic of spices.

The antioxidant of the present invention having such properties includes lard,
Animal and vegetable oils and fats such as head, soybean oil, and cottonseed oil; oil and fat processed foods such as butter, margarine, dressing sinks, and shortening; oil and fat processed foods such as 11-1 noodles, donuts, fried sweets, and chocolates; and many other foods. Not only can it be added to and used in foods, but it can also be added to and used in oil-containing products other than food, such as cosmetics.

In this case, the addition amount is o as dry powder weight,
A very small amount of o o s-0.05% is sufficient.

Examples of the present invention are listed below, as well as comparative examples to clarify the effects of the present invention.

Example 1 Diethyl ether 5
, 'j was extracted under reflux. To the obtained extract, 0.5N hydroxide W-1-S.Kum2; Jz was added, shaken, mixed, and then allowed to stand still to take out only the -C aqueous layer. Sulfuric acid was added to the resulting aqueous layer and shaken and mixed until the P of the aqueous layer became 3.0. Then, 1'/l of diethyl ether was added, shaken, mixed and allowed to stand. Then, the diethyl ether layer was taken out and washed with water until its I)H became almost neutral.

(The obtained diethyl ether layer was heated at about 40°G and subjected to -C desolvation treatment, then 17 tons of hot distilled water was added and steam distilled to obtain a residue of 1.7%.The yield of the obtained residue was Liborio'! J) My youngest uncle gave me 12 sura, 1 cup of thyme powder cost 21 Z5, 1 cup of marjoram powder cost 112'', and 1 cup of orecano powder cost 12 7j.

In this way, the antioxidant effect of each residue obtained by () was confirmed by the AOI\4 method using lard, and tC0, that is,
AOM test always contains tocopherol and butyl hydroxyl
20ml of purified lard that does not contain antioxidants such as toluene
After adding 1, 0.022 double circles of each of the above-mentioned residues and ]・]Noerol were added separately, and clean air was blown at a flow rate of 2.33+nl/sec in a constant temperature bath kept at 97.8 ° G. ,
The time required for the peroxide value (+) OV ) to reach 100 meQ/kg was measured. The measurement results are shown in Table 1.

As is clear from Table 1, the unadditive lard has a POV of 100 m eq/kg in 355 hours, whereas the POV of the lard added with the residue obtained by the method of the present invention is 100 m eq/kg. /ka Ck-/l It took more than 681 minutes. On the other hand, it was 48.0 hours in the category to which Coal was added. From these facts, the residue extracted from spices by the method of the present invention has an antioxidant effect comparable to or greater than that of tocopherol, and can be fully utilized as an antioxidant.

Example 2 A residue (A) was obtained from 1 quart of A recano powder using the same method and conditions as in Example 1. The conventional method is to add 1 part of oregano powder to 5 parts of dini[chill]-ter. After engraving, fast flow extraction was performed at 85°G for 3 hours. The obtained extract was refluxed for 30 minutes under conditions C.
After being treated with activated carbon, it was heated to about 40 tons under reduced pressure to remove the solvent, and 1'α of distilled water was added thereto and steam distilled to obtain a residue (B) of 19.

The antioxidant effect of the residues (Δ) and (B) thus obtained was confirmed using the same method and conditions as in Example 1. The measurement results are shown in Table 2.

Table 2 As is clear from Table 2, the residue (A) obtained by the method of the present invention is better than the residue (B) obtained by the conventional method.
The antioxidant effect was superior to that of 1.

Claims (1)

[Claims] (1) Incense! I- Add an alkaline aqueous solution to the liquid extracted with a non-polar organic solvent from the side, take out the resulting aqueous layer, add an acidic agent to it, then add a non-polar organic solvent, and wash the resulting solvent layer with water. 1. A method for producing an antioxidant, which comprises making the Pl neutral, followed by desolvation treatment, followed by steam distillation to collect the residue.