JPS61282357A - Production of concentrated carotene - Google Patents

Abstract

PURPOSE:To concentrate efficiently carotene in palm oil, by treating the palm oil with a specific granular clayey adsorbent, separating the adsorbed carotene and desorbing and extracting the separated carotene with an acid and solvent. CONSTITUTION:Palm oil which may or may not be treated with polyphosphoric acid or anhydrous phosphoric acid is treated with a ganular clayey adsorbent consisting of a solid material prepared by mixing a clayey adsorbent with silicic acid gel or aluminum gel and firing the resultant mixture to adsorb and separate carotene, which is then desorbed and extracted with an organic or inorganic acid and a solvent, e.g. hexane. The solvent and acid are then removed therefrom to afford the aimed concentrated carotene, which is further brought into contact with an ion exchange resin to give the carotene with further improved concentration degree. The carotene in the palm oil as a coloring impurity is subjected to a decoloring step, but the carotene can be effectively concentrated before the step.

Description

DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing a carotene concentrate using palm oil as a raw material.

(Conventional technology) Carotenes contained in palm oil contain β-
There are carotenes such as α- and γ-carotene, and their content is said to be 0.03 to 0.1%, although it varies depending on the variety and production area of the oil palm.

It is well known that carotenes have physiological activity as vitamin A precursors, but in recent years, their anticancer effects against certain cancers, antitumor effects, and ovulation promoting effects in livestock have been demonstrated. For this reason, there is increasing momentum around the world to develop a method for concentrating natural carotenes.

Plant resources containing relatively large amounts of carotenes include carrot root, alfalfa leaves, palm oil, and seaweed (Dunal).
iejla 5alina). Among these, palm oil is: (1) The production scale is large and the production volume is increasing year by year, (3) The collection system is better than other carotene-containing plant resources, and (3) Palm oil is produced with a high content of carotenes. The oil palm produced by palm oil is suitable as a raw material for molding carotenes, as it has been obtained through breeding. Currently, the carotenes contained in palm oil are decomposed and removed as colored impurities during the palm oil refining process.

(Means for Solving the Problems) Therefore, the present inventors have made efforts to develop a method that can effectively e-condense carotenes contained in palm oil prior to the palm oil refining process, especially the decolorization process. As a result of repeated research, it was discovered that the objective could be achieved by combining the use of a specific clay adsorbent and an adsorption conflict extraction process, and based on this knowledge, the present invention was completed.

That is, the present invention provides palm oil or phosphoric acid, polyphosphoric acid,
Alternatively, palm oil that has been treated with phosphoric anhydride is treated with a granular clay adsorbent consisting of a clay adsorbent mixed with silicic acid gel or aluminum gel and fired to adsorb and separate carotenes. The present invention provides a method for preparing concentrated carotenes, which is characterized by desorbing and extracting carotenes with an organic or inorganic acid or a solvent.

The palm oil to which the present invention is applied is obtained by separating crude palm oil (crude palm oil) molded from palm pulp and separating the crude palm oil.
) Palm oil contains carotenes such as a liquid fraction (palm olein) and a palm stearin fraction (palm stearin).

In addition, as a raw material, palm oil is contacted with phosphoric acid, polyphosphoric acid, or phosphoric anhydride at room temperature or heated F, and the phosphoric acid content is separated and the oil is used as it is or after washing with water and dehydrating. Good too.

In the present invention, such palm oil is brought into contact with a granular clay adsorbent made of a solid material obtained by mixing a clay adsorbent with silicic acid gel or aluminum gel and calcined at room temperature or under heating to obtain the oil contained in the palm oil. The carotenes present are adsorbed onto the granular clay adsorbent. The oil and adsorbent are then separated.

At this time, sufficiently removing the oil adhering to the adsorbent is effective in reducing the amount of carotenes.

Note that when carotenes in palm oil that has not been treated with phosphoric acid, polyphosphoric acid, or phosphoric anhydride are to be adsorbed to the granular clay adsorbent, the amount of the adsorbent used may be increased.

Adsorption operations can be performed on palm oil, palm oil treated with phosphoric acid, polyphosphoric acid, or phosphoric anhydride to separate the phosphoric acid content, and oils that have been washed with water and dehydrated. If you do it in two steps, carotenes! The shrinkage is made more effective. This is because the first stage adsorption operation removes substances that inhibit the adsorption of carotenes to the granular clay adsorbent. Therefore, the adsorbent used in the first stage adsorption operation is not limited to the granular clay adsorbent mentioned above, but also an adsorbent that has the effect of removing substances that inhibit the adsorption of carotenes to the granular viscous adsorbent described above. Any agent may be used.

The methods of bringing oil into contact with the adsorbent include dispersing the adsorbent in oil and passing the oil through a column filled with the adsorbent. , is effective in removing substances that inhibit the adsorption of carotenes to the double adsorbent.

I. The carotenes adsorbed on the granular viscous adsorbent are desorbed and extracted with organic or inorganic acids or solvents, or
At that time, carotenes are adsorbed." - A method of applying an organic or inorganic acid to a granular clay adsorbent and then extracting the desorbed carotenes with a solvent. A method of desorbing and extracting carotenes by adding an organic acid or FjIM-free in the coexistence of a granular viscous adsorbent and a solvent, and a method of desorbing and extracting carotenes using a solvent containing an organic acid or an inorganic acid. Both are effective. The solvent used for extracting carotenes may be any solvent as long as it dissolves carotenes, but in consideration of solvent removal and operation, a hydrocarbon solvent with a relatively low boiling point, such as hexane T, is preferred.

A concentrate of carotenes is obtained by removing the solvent and solvent from the carotene extract. A solution of this carotene concentrate dissolved in alcohol is passed through a column filled with an ion exchange resin, and alcohol is removed from the effluent to obtain a carotene concentrate with a higher degree of concentration.

(Effects of the Invention) According to the present invention, concentrated carotenes can be efficiently produced prior to the step of decolorizing palm oil.

(Example) Next, the present invention will be explained in more detail based on examples.

Example 1 Add 6 g of polyphosphoric acid to 300 g of palm crude oil and heat at 80°C
After stirring vigorously for 1 hour, the mixture was filtered using a funnel kept at 60°C to obtain 295 g of dark red lipid and a dark green residue. Visible absorption spectrum analysis of this lipid (H, A, B
Ockenoogen, “Analysis and
Characterization of 0
ils Fatsand Fat Produc
ts"Vo12Int erscience (19
68)9.648) The results showed that this lipid contained 0.034% carotenes in terms of β-carotene. While maintaining 100 g of this 1 lipid at 50'C, aluminum gel was mixed with clay adsorbent, 10 g of granular clay adsorbent made of calcined solids was added, and after stirring for 1 hour, the lipid and adsorbent were separated by filtration. . Lipids adhering to the adsorbent were removed by washing with hexane. The hexane-washed adsorbent was transferred to a flask, 5 ml of acetic acid and 50 ml of hexane were added, and the mixture was heated to 50°C to desorb and extract the adsorbed material. Next, the adsorbent was washed three times with 50 ml of hexane, and the washing liquid was combined with the extract, and the acetic acid was removed by washing with water. The hexane layer was dried over anhydrous sodium sulfate, and the hexane was carefully removed under reduced pressure.
．． 662 g of extract was obtained. From the measurement effect of the visible absorption spectrum, this extract has a content of 0.39 in terms of β-carotene.
% of carotenes.

Example 2 A solution in which 0.53 g of the extract obtained in the example process was dissolved in 50 ml of methanol was passed through a glass column filled with 5 g of Amberlite 401 type anion exchange resin that had been activated in advance, and the liquid that flowed out was Methanol was distilled off to obtain a 0.018 g effluent fraction. As a result of visible absorption spectrum analysis, this effluent fraction contained 1
The presence of 0.8% carotenes was observed.

Example 3 6 g of phosphoric anhydride powder was added to 300 g of palm crude oil liquid fraction (palm olein) and stirred at 80° C. for 1 hour. After filtering off the anhydrous phosphorus, the oil was washed with water and dehydrated to obtain 293 g of oil. Add 0.5% by weight of activated clay to this oil,
50' (!) for 1 hour. This treated oil was 0.055% in terms of β-carotene as a result of visible absorption spectrum analysis
Contains carotenes.

To 100 g of activated clay treated oil, 10 g of granular clay adsorbent mixed with silica gel and calcined was added.
The mixture was stirred at ℃ for 1 hour to allow the carotenes to be adsorbed onto the adsorbent. Desorb and extract the adsorbate that adsorbed carotenes, 0.7
5g of extract was obtained. As a result of IIT optical absorption spectrum analysis, this extract contained 0.98% carotenes in terms of β-carotene.

Example 4 A solution prepared by dissolving 0.6 g of the extract obtained in Example 3 in 50 mM ethanol was brought into contact with an ion exchange resin in the same manner as in Example 2, and ethanol was removed from the effluent.
g of a dark brown viscous substance was obtained. Based on the absorbance at 445 nm, this viscous substance contains 11.0% in terms of β-carotene.
The presence of 5% carotenes was observed.

Patent applicant: Director of the Agency of Industrial Science and Technology, Todoro Federation ・Second, Pa;・Hiri゛.

Procedural Amendment (Spontaneous) No. 60 Kagiken No. 1172, June 1985, July 23, 1984 - Mr. Michibe Uga, Commissioner of the Patent Office, v. Shiji 1, Indication of Case Patent Application No. 124877 of 1985
No. 2, Title of the invention Method for preparing concentrated carotenes 3
Address of the patent applicant related to the person making the amendment: 1-3-1 Kasumigaseki, Chiyoda-ku, Tokyo'
re'''tb (114) Todoroki, Director of the Agency of Industrial Science and Technology
(Shipping date: Showa, month, day) 8,
Contents of the amendment The following amendments will be made in the specification of the application.

(1) In the second line from the bottom of the second page, ``Suru oil palm 1 ga'' is corrected to ``Suru oil palm ga''.

(2) Page 3, line 3, “10.
" will be corrected to "01. for carotenes in palm oil."

(3) On page 6, lines 7 and 8, "Then, the carotenes desorbed by the solvent are 10." is corrected to "Then, the carotenes desorbed by the solvent are 61.".

(4) Correct "Solvent removal A operation" in the 6th line from the bottom of page 6 to "Solvent removal operation."

(5) On page 8, line 8 from the bottom, “01.
" is corrected to "00."

Claims (2)

[Claims] (1) Palm oil or palm oil treated with phosphoric acid, polyphosphoric acid, or phosphoric anhydride is used as a granular clay adsorbent consisting of a solid substance obtained by mixing silicic acid gel or aluminum gel with clay adsorbent and firing the mixture. 1. A method for preparing concentrated carotenes, which comprises treating and adsorbing and separating carotenes, and desorbing and extracting the adsorbed and separated carotenes with an organic or inorganic acid or a solvent. (2) The method for preparing concentrated carotenes according to claim 1, characterized in that the extracted and separated carotenes are further brought into contact with an ion exchange resin.