KR20110105587A - Method of preparing red betacyanins and yellow betaxanthins from red beet - Google Patents

Abstract

The present invention relates to a method for preparing beta cyanins red pigment and beta xanthins yellow pigment from red beet (Beta vulgaris L.), more specifically, extracting red beet with water; Separating the pigment into a weakly basic anion exchange resin; Desalting is characterized in that it comprises a step.

Description

Method of preparing beta cyanine red pigment and beta xanthine yellow pigment from red beet {Method of preparing red betacyanins and yellow betaxanthins from red beet}

The present invention relates to a method for producing beta cyanins red pigment and beta xanthins yellow pigment from beta vulgaris L. More specifically, extracting the red beet with water; Separating the pigment into a weakly basic anion exchange resin; It relates to a method for producing red beta betayanins (red betacyanins) red pigment and beta xanthin (yellow) pigment, characterized in that it comprises a desalting step.

 Food colorings currently used as food additives include natural colors and artificial colors. Natural pigments are pigments obtained by methods such as extraction from natural products containing the pigments, and are almost harmless to the human body. However, since the source is a natural product, the amount of supply thereof is limited according to the surrounding environmental factors. Therefore, developed as a substitute for this is a synthetic pigment, synthetic pigments are currently being developed and used in a wide variety.

     Synthetic pigments, however, can be supplied reliably unlike natural pigments in terms of their supply, but as further research raises potential hazards to humans (Weller TA, Lasure LL (1981)). , Betalains in beet root tissue culture, Journal of Food Science 47: 162-163).

     Betalain, a kind of natural pigment, is the only chromo-alkaloid water-soluble pigment that exists only in the Centrospermae, and has various colors from red to purple. It is known to be effective as an agent [Mabry TJ, Kimler L, Chang C (1970), The betalains: structure, function and biogenesis and Centrospermae. In: Recent Advances in Phytochemistry 5: 105-134]. This betaline is synthesized by the condensation of cyclone-DOPA with the betaline acid produced from the shikimic acid pathway, i.e., dihydroxyphenylalanine (DOPA) (Girod PA, Zryd JP (1991), Secondary metabolism). in cultured red beet (Beta vulqaris L.) cell: Differential regulation of betaxanthin and batacyanin biosynthesis, Plant Cell, Tissue and Organ Culture 25: 1-12], two types of red beta cyanine and yellow beta xanthine. Are divided into categories.

     In particular, beta cyanine, a natural pigment extracted from red beet, has been shown to be safe for the health and economical advantages of chemically synthesized pigments [Berlin J, Sieg S, Strack D, Bokern M, Harms H (1986). , Production of betalains by suspension cultures of Chenopodiun rubrum L. Plant Cell Tissue Organ Culture 5: 163-174]. Under the approval of the U.S. FDC (1960 Color Additive Amendment, Food Drug and Cosmatic Act of 1938), it is now widely used as a colorant for foods and beverages with relatively low heat treatment, such as sausages, yogurt, ice cream, cold drinks and gelatin desserts. In addition, the red beet is rich in protein group composed of essential amino acids, high-quality dietary fiber, folic acid and vitamins and minerals are widely used as a main component of the health supplement for treating intractable diseases such as various adult diseases.

     Representatives of natural red pigment include anthocyanin and betacyanin, which are present in a large amount in various plants such as grapes, strawberries, roses, and leaflets, but anthocyanins are not red, but reddish purple, and their chemical stability is weak. It is limited in place. In addition, the red pigment present in red beet, pokeberry, and cactus fruit is beta cyanine, and research on it has been proceeded considerably. Stability is also established, and in Europe, including the United States, the only natural red pigment is currently used in many foods. This pigment was studied mainly in red beet, and it is known that the red beet is a water-soluble pigment called betaline, and is mainly composed of red pigment beta cyanine and yellow pigment beta xanthine.

     In addition to beta cyanine-based red pigments, beta xanthine yellow pigments coexist in red beet, but until now, research on red beet pigment has been mainly limited to beta cyanine as a part of research on natural red pigments. However, when developing a method for separating beta cyanine and beta xanthine natural pigments from red beet at high purity at the same time, 1) there is an advantage that various colors can be realized through quantitative pigment mixing, and 2) color interaction. Small beta, 3) high clarity, 4) easy quality control, and 5) improved consumer satisfaction. There is an urgent need for a method for separating xanthine yellow pigments.

In order to solve the above problems, the present invention can be easily separated and desorbed pigment components, while having a selective adsorption to the beta cyanine and beta xanthine of the main pigment components of red beet, high yield weak base It is an object of the present invention to provide a method for producing beta cyanine and beta xanthine with low cost and high purity by applying an anion exchange column method.

 The present invention relates to a method for preparing beta cyanine-based red pigment and beta xanthine yellow pigment from the red beet, to more particularly, to extract the red beet with water; Separating the pigment into a weakly basic anion exchange resin; It provides a natural pigment manufacturing method of beta cyanine and beta xanthine comprising the step of desalting.

By the above configuration, the low cost, high purity separation method of the red beet cyanine-based red pigment and the beta xanthine yellow pigment according to the present invention uses beta cyanine and beta from red beet by using weakly basic anion exchange resin. While effectively reducing the loss of xanthine, it is an excellent invention capable of separating beta cyanine and beta xanthine, which have not been achieved by a simple process, in high purity of 90% or more. Therefore, the present invention can effectively contribute to the development of natural pigments containing the beta cyanine-based red pigment and the beta xanthine-based yellow pigment as an active ingredient. It can increase industrial utilization.

1 is a diagram showing an AW90 preparative chromatogram of red beet water extract,
FIG. 2 is a diagram showing an ultraviolet / visible spectrum of a high peak liquid chromatogram and a main peak of (A) fractions of the AW90 preparative chromatogram of FIG.
FIG. 3 is a diagram showing the high-pressure liquid chromatogram and the ultraviolet / visible light spectrum of the main peaks of the (B) fraction of the AW90 preparative chromatogram of FIG. 1.

Hereinafter, the contents of the present invention in more detail through each step process is as follows.

1) water extraction process

The red beet raw material is cut into a suitable size, pulverized, and then pulverized, water is added from 10 to 30 times the total weight of the red beet and extracted for 30 minutes to 2 hours at a temperature of 5 ^o C to 35 ^o C or less. It is possible to extract the ingredients effectively.

2) filtration process

     After water extraction, separation of the aqueous extract and the insoluble residue is filtered using a dense filter cloth or filter cloth of 50 mesh or more (or 100 micron or more in pore size), centrifuged for 20 minutes or more by a centrifugal force of 1,500 × G, or solid-liquid separation. Extraction can be effectively separated by using a continuous centrifuge or decanter.

3) Separation of Betacyanine and Betaxanthine by Ion Exchange Resin

     A weakly basic anion exchange resin column having, for example, ammonium groups as a complex aqueous solution of the beta cyanine and beta xanthine mixture obtained from the above step (2) as an ammonium group exchanger, for example, styrene-based weakly basic anion exchange. Inject the resin into the column layer filled with resin (e.g. TRILITE AW90, Samyang Co., Ltd.) at a constant speed while avoiding air incorporation. By allowing it to be adsorbed into the resin and washing with water (tap water), it is possible to naturally separate neutral polysaccharide components in addition to beta cyanine and beta xanthine containing carboxyl groups. Secondly, ion with 0.5 to 10% sodium chloride solution. The exchange resin layer was washed with water, and beta cyanine and beta xanthine in the form of salt soluble sodium chloride were bound in the resin. Beta cyanine and beta xanthine can be obtained by conversion, separation and elution.

4) Desalination Process

     Betaxanthine-containing liquid (primary treatment liquid) and beta cyanine-containing liquid (secondary treatment liquid) obtained by the adsorption and elution treatment of the ion exchange resin in the step (3) above have a molecular weight in the range of 100 to 5,000 Daltons Residual sodium chloride was removed by gel filtration chromatography using cross-linked dextran-based gels (eg Bio-Gel P-2, Biorad, Sephadex G-10, GE Healthcare) to separate And desalted beta cyanine and beta xanthine can be obtained.

     Hereinafter, the content of the present invention will be described in more detail with reference to Examples. However, the embodiments are presented to explain the contents of the present invention, but the scope of the present invention is not limited thereto.

Example 1 Preparation of Red Beet Water Extract

After cutting and grinding 1 kg of red beet, 30 times the total weight of red beet was added water, and then extracted at 30 ^° C. for 30 minutes. After extraction of water, the mixture was filtered using a 300 mesh filter cloth to separate the aqueous extract and the insoluble residue. The whole filtrate was lyophilized and the solid content of water extract was 11.57%.

Example 2: Batch Separation of Betacyanine and Betaxanthine from Red Beet Water Extract

In order to separate the beta cyanine and the beta xanthine from the red beet water extract, 50 mg of red beet water extract was dissolved in 5 ml purified water, and then a column filled with 50 g of styrene-based weakly basic anion exchange resin (TRILITE AW90, Samyang) 2.8 × 30 cm, packed volume: 76 ml), adsorbed, and then the beta xanthine separation eluted with 0.1 M sodium chloride solution 4.3 times the fill volume, while the beta cyanine separation resulted in 0.5 M sodium chloride solution 4.5 times eluted and eluted by sequentially injecting at a rate of 5 ml / min, respectively. The pigment components were detected at 476 nm and 537 nm for each aliquot. Beta xanthine was eluted between fractions 5 ~ 90 (Fig. 1 (a)), HPLC analysis was confirmed that beta xanthine was separated by high purity of more than 90% (Fig. 2). Beta cyanine was eluted between fractions 95-145 (FIG. 1 (b)), and the respective fractions were combined and passed through a Sephadex G-10 gel column to desalt sodium chloride, followed by HPLC analysis. It was confirmed that the sum of the red pigment (1) and (2) peaks was more than 90% high purity (FIG. 3).

Claims (3)

Extracting the red beet with water,
Separating the extract into a weakly basic anion exchange resin,
A method of separating beta cyanine-based red pigment and beta xanthine yellow pigment from red beet, characterized in that it comprises desalting the fractionated solution.      According to claim 1, wherein the weakly basic anion exchange resin is selected from polystyrene series, polyacrylic series, styrene divinylbenzene series, methacrylic acid ester series and methyl propylrenic acid ester series beta cyanine series from red beet A method for separating the red pigment and the beta xanthine yellow pigment. The beta cyanine-based red pigment and beta xanthine yellow from red beet according to claim 1, wherein the desalting is performed using a crosslinked dextran-based gel capable of separating components having a molecular weight ranging from 100 to 5,000 Daltons. How to separate the pigments.

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