JPH0799927A - Production of emulsion of concentrated and naturally occurring red coloring matter oil for food product and emulsion product therefrom - Google Patents

Abstract

PURPOSE:To obtain a red coloring matter which has excellent color tone, light resistance and coloring properties and is produced by phaffia yeast in the form of an emulsion of solvent-free concentrated coloring matter oil reduced in contaminants and with no smell. CONSTITUTION:The phaffia yeast producing a red coloring matter is extracted with a hexane-ethanol mixture, the crude oil is cencentrated, when needed, deodorized to give the objective concentrates natural coloring matter oil for food products. The oil is emulsified by stirring together with an emulsifier for food. As the emulsifier, is used perferably a fatty acid ester and/or a polyglycerol ester.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an emulsion of concentrated natural red dye oil for food and an emulsion of the obtained concentrated natural red dye oil for food. More particularly, it relates to a method for producing an emulsion of concentrated natural red dye oil for foods from Phaffia yeast that produces red pigments, and an emulsion of the obtained concentrated natural red dye oil for foods.

More specifically, astaxanthin-producing yeast Phaffia rhodozyma (Phaffia rhodomo)
An emulsion of a concentrated natural red pigment oil for foods, which is produced by extracting a pigment contained in zym) to produce a concentrated natural red pigment oil for foods and emulsifying the concentrated natural red pigment oil for foods. And the obtained concentrated natural red dye oil emulsion for food. The obtained concentrated natural red dye oil emulsion for foods is not only excellent in color tone, light resistance, colorability, and heat resistance, but also has a new physiological activity such as antioxidant activity, anti-inflammatory effect, and immunostimulatory effect. Used as an emulsion of functional edible natural pigments.

[0003]

2. Description of the Related Art Various coloring agents have been used for food dyes. Synthetic colorants include red, yellow, green, and blue tar dyes and their aluminum chelates, iron oxides, titanium dioxide, and copper chlorophyllin sodium.
Iron chlorophyllin sodium, water-soluble anato, and β-carotene are approved according to their intended use. Although these colorants are widely used due to diversification of consumer demand and convenience of coloring, in recent years, these synthetic colorants have been replaced with natural pigments as consumer interest in health and safety has increased. is there.

As such a natural pigment, β-
Carotenes, paprika pigments, annatto pigments, red yeast rice pigments, cochineal, safflower pigments, etc. are on the market and are often used, but most of the raw materials are imported and there are many things that are unstable in supply, price, etc. Further, there is nothing satisfactory in terms of light resistance, heat resistance, dye concentration, odor, etc., and development of new food dyes is desired in the food industry.

The natural pigments are mainly those obtained by simple operations such as extraction, squeezing, concentration, drying and crushing from natural products such as plants and animals. Since it is obtained from natural products, it is common for extracted oil to contain many components. Commercially available natural pigments often have a pure pigment concentration of several percent, and their use may be limited in terms of the concentration. The high concentration of natural pigments has become a major issue in pigment development.

Phaffia yeast producing astaxanthin as a natural pigment is known. The red pigment produced by Phaffia yeast is redder and has a specific color tone than paprika, but this natural pigment also needs to be further concentrated. Further, in order to extract the pigment from the Phaffia yeast, a solvent is used from the crushed yeast, and a highly polar solvent such as acetone or ethanol is suitable for the solvent used for this extraction. However, these solvents have the drawbacks that they cannot be used for extraction of food additives, are very expensive, and that the use of highly polar solvents increases the amount of contaminants in the extracted pigment oil.

Due to its unique color tone, the red pigment produced by Phaffia yeast is expected to be in demand for fish paste products, jellies, chocolates and the like, and it is necessary to further increase the pigment concentration in order to expand its versatility in beverages and the like. Yes, and
It is desired to emulsify the concentrated pigment oil from the viewpoint of improving the solubility and dispersibility in water and expanding the application.

[0008]

SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing an emulsion of concentrated natural red dye oil for food and an emulsion of concentrated natural red dye oil for food. This invention, by producing an emulsion of concentrated natural red pigment oil for foods, has excellent coloring properties, stability, and pigment concentration, which have been the drawbacks of natural pigments, without impairing the characteristics of natural pigments. It aims to provide new dyes and expand their applications.

Since the Phaffia dye has a vivid color tone from orange to reddish orange and is superior in light resistance to paprika dyes of similar colors, it can be expected to be widely applied to foods. It is an object of the present invention to provide a stable and characteristic reddish Phaffia dye which can be used in the form of an emulsion of concentrated dye oil.

[0010]

[Means for Solving the Problems] Astaxanthin, which is a main component of the Phaffia dye, has the highest red color tone among carotenoid dyes such as β-carotene, and has high heat, light, and PH.
It has relatively good stability against the like, and since it is ingested daily from produced foods such as crab, shrimp and salmon, there is no problem in terms of safety. Furthermore, astaxanthin is also known to have useful functions such as antioxidative properties and immunostimulation, and is attracting attention as a new functional dye that has never existed as a natural dye.

In the present invention, first, a concentrated natural red dye oil for food is produced, and then the concentrated dye oil is emulsified. The above-mentioned concentrated natural red dye oil for foods is produced by the method described below. That is, in the present invention, the Phaffia yeast producing a red pigment is subjected to an extraction treatment using a specific extraction solvent, and then the obtained crude extracted pigment oil is subjected to a concentration treatment and, if necessary, a deodorizing treatment, whereby a food concentration is first conducted. A natural red pigment oil is produced. The pigment contained in Phaffia yeast producing red pigment is extracted using a mixed solution of hexane and ethanol as an extraction solvent. Adopting a mixed solvent of hexane and ethanol as an extraction solvent and using it to extract astaxanthin from Phaffia yeast, various concentration treatments are performed, and further deodorizing treatment is performed to produce concentrated natural red pigment oil for food. .

[0012] In the production of concentrated natural red dye oil for foods, a low temperature fractionation treatment, a saponification treatment, or a combination of a low temperature fractionation treatment and a saponification treatment is preferably used as the concentration means. When the low temperature fractionation treatment and the saponification treatment are used together, a method of performing the low temperature fractionation treatment and then the saponification treatment, and a method of simultaneously performing the low temperature fractionation treatment and the saponification treatment are adopted. As the saponification treatment, it is preferable to apply a method of forming a fatty acid alkali soap or a method of applying a fatty acid metal soap. As the above deodorizing treatment, steam distillation is preferably adopted.

The Phaffia yeast which produces a red pigment used as a raw material yeast is a yeast which belongs to an incomplete fungus in terms of microbiological classification and produces a red pigment, for example, Phaffia rhodozyma. Phaffia yeast used for extraction is collected by centrifugation or filtration after culturing, then thoroughly washed with water, and then either as it is or after drying, is physically crushed by ball mill, freeze crushing, compression crushing, ultrasonic treatment, or enzymatically using cellulase. Pretreatment by treatment is desirable. When the pigment oil is extracted from the wet cells using an organic solvent, contaminants are significantly mixed, and
Since the extraction rate also decreases uniformly, it is industrially more common to perform solvent extraction from dried cells.

Acetone, ethyl acetate, hexane, ethanol and the like can be considered as the extraction solvent used when the pigment is extracted from Phaffia yeast. However, acetone and ethyl acetate, which have a good extraction rate, cannot be used to extract food additives. Hexane is low in price, but has a problem in terms of extraction rate, and ethanol has a good extraction rate, but has a problem of increase in extraction cost and concentration cost due to increase in highly polar components.

These problems can be solved by mixing the disadvantages of hexane with ethanol to provide an inexpensive and excellent extraction solvent for concentrated natural red dye oil for food. That is, in extracting astaxanthin pigment from Phaffia yeast, astaxanthin can be extracted more efficiently by appropriately selecting the mixing ratio of hexane and ethanol from crushed Phaffia yeast.

Regarding the mixing ratio of hexane and ethanol, the higher the ratio of ethanol, the higher the extraction rate. However, if the proportion of ethanol increases, the extraction cost increases and the amount of highly polar substances increases, and the subsequent concentration operation becomes complicated. Therefore, the mixing ratio was judged from the extraction ratio of the dye, the extraction cost, the azeotropic composition of hexane and ethanol, and the like. Hexane: ethanol is 90-50: 10-5
It is used in a proportion of 0, preferably 85-80: 15-20. As for the extraction method, the treatment can be carried out more smoothly by feeding the treatment liquid obtained by stirring and mixing the extraction solvent and the dry cells to the compression grinder while stirring with a pump. It is desirable to perform the crushing process multiple times depending on the extraction.

Triglycerides and free fatty acids play a major role in the lipid composition in Phaffia yeast, and efficient removal of these major components is necessary in order to increase the pigment concentration of the extracted pigment oil. Triglyceride, which is one of the main components, can be removed efficiently by low temperature fractionation. Low temperature fractionation is performed at -60 ° C to 10 ° C, preferably at -50 ° C with hexane, acetone,
It can be performed using an organic solvent such as ethanol, and astaxanthins can be concentrated and purified. For example,
When a material yeast containing a large amount of triglyceride is used, it can be said that low temperature fractionation is an excellent concentration treatment.

Free fatty acid, which is one of the main components, can be efficiently removed by saponification treatment. In the saponification treatment, astaxanthins can be concentrated and purified by removing an alkaline soap of a fatty acid produced by adding an alkali such as sodium hydroxide, potassium hydroxide or calcium hydroxide. For example, when a raw material yeast containing a large amount of free fatty acids is used, the saponification treatment can be said to be an excellent concentration treatment. The saponification treatment can be carried out in an organic solvent such as acetone or hexane or a fat and oil, but the most efficient one is in acetone.

Concentration by low temperature fractionation has a free fatty acid removal rate of about 40%, and in the concentration method utilizing the soap formation method, only fatty acids are selectively removed. , It is possible to concentrate pigments to a higher degree from crude extract pigment oils that have multiple major lipid components.

The concentrated natural red dye oil for foods is used for foods, and it is preferable to perform deodorizing treatment for removing yeast odor and removing solvent. Steam distillation is used as a deodorizing means. Steam distillation is preferably usually 100-
200 ° C., preferably 120-150 ° C., vacuum degree 30
It is performed below torr. Dye oil extracted from Phaffia yeast generally has an irritating odor peculiar to fermentation products. This pungent odor is particularly severe when the dye is used at a high concentration, and it significantly limits the range of use of the dye oil.

Since this fermentation odor is derived from the medium used for culturing Phaffia yeast, it is considerably reduced by thoroughly washing the collected bacterial cells with water.
This alone is insufficient to deodorize the pigment oil. Further, hexane used as an extraction solvent and acetone used for concentration should not remain in the dye oil as the final product. Therefore, the pigment oil after extraction is usually added to 1
Fermentation odor is remarkably reduced by steam remaining at 0 to 200 ° C., preferably 120 to 150 ° C. and a vacuum degree of 30 torr or less, and hexane and acetone, which are extracted from the pigment oil and purified solvents, are used together with water. It could be completely removed by boiling.

Then, a food grade emulsifier is used to emulsify the concentrated food grade natural red dye oil. Food emulsifiers recognized by the Food Sanitation Act include fatty acid monoglycerides, polyglycerin fatty acids, sorbitan fatty acid esters (spans, etc.), nonionic activators such as fatty acid esters of sucrose and lecithin, enzyme-treated lecithin, There are natural products such as gum arabic, quillaia extract and egg yolk.

These food-grade emulsifiers include, for example, 1 to 2% of fatty acid monoglycerides added to shortening,
When bread and cakes are used with this product, it contains a lot of water and is soft and bulky. When about 0.3% of margarine is used, the temperature range that can be kept soft in addition to the emulsifying action is expanded. Then add 0.
A good structure can be obtained by using 3 to 1.0%. When 0.25 to 0.50% is used in peanut butter, oil separation can be prevented and the feel is smooth.

Besides, it is used for candy, chewing gum, mayonnaise, salad dressing and the like. Examples of sorbitan fatty acid esters include sorbitan monooleate (Span 80) and sorbitan monolaurate (Span 20). When used in caramel and chewing gum, the plasticity and binding properties are improved, and the crispness is improved. Esters containing palmitic acid and stearic acid as fatty acids of sucrose fatty acid esters are used in the above various foods, and lecithin is used in margarine, mayonnaise and the like. In the present invention, these food-grade emulsifiers are appropriately selected and used according to the type of food. In the present invention, a fatty acid ester and / or polyglycerin ester is preferably used as a food emulsifier.

[0025]

The details of the present invention will be described with reference to examples. The present invention is in no way limited by the examples. Extraction example Phaffia rhodozyma
The strains belonging to Zyma) were cultured, the obtained cultures were collected by centrifugation and filtration, and dried bacterial cells were obtained by a spray dryer. Ethanol,
Hexane, acetone, ethyl acetate, and 3 L of a mixed solvent of each ratio of hexane and ethanol were added, and the mixture was stirred and mixed, and compression pulverization was performed using a compression pulverizer (15MR manufactured by APV GAULIN). The results are shown in Table 1 (dye extraction rate by solvent).

[0026]

[Table 1]

Acetone and ethyl acetate are not suitable for the extraction of food dyes, but both have good extraction ratios of 90% or more, and thus can be sufficiently used in other fields of application. The dye extraction rate of hexane alone was as low as 65.8%, but as the content of ethanol increased, the extraction rate improved almost linearly to 87% when the ethanol content was 15%. The ethanol content must be 75% or more for the extraction rate to be 90% or more, but the proportion of highly polar components other than astaxanthins increases, and subsequent processing becomes complicated, and coexistence of hexane and ethanol From the boiling composition ratio, it was revealed that hexane: ethanol = 85: 15 was the most desirable value.

Concentrated Dye Oil Production Example 1 A low temperature fractionation treatment was performed to remove free fatty acids and triglycerides from crude dye oil. Crude extract dye oil 10,5
Three times the amount of acetone or n-hexane / ethanol (85:15) was added, and the mixture was stirred at -50 ° C for 1 hour, filtered with 4A filter paper (ADBANTEC), and the filtrate was concentrated under reduced pressure to prepare lipids. The amount and carotenoid amount were determined. When the amount of solvent added was 3 times that of the extracted oil, the concentration of precipitates in the solution was so high that it could not be fractionated because it solidified during low temperature fractionation, but triglyceride was obtained by performing low temperature fractionation with 5 volumes of acetone. , Sterols and phospholipids were removed, and the dye concentration was concentrated about 1.5 times. The results are shown in Table 2 (concentration of pigment oil by low temperature fractionation treatment).

[0029]

[Table 2]

Concentrated Dye Oil Production Example 2 The free fatty acid and the equivalent amount of potassium hydroxide in the crude dye oil were adjusted to 0.
Stir to dissolve in 20 ml of 8% hydrous acetone at 40 ° C., and
g oil (75.39% free fatty acid) was added and potassium soap was formed with stirring for 10 minutes at room temperature. In order to form a metal soap, calcium chloride in an amount equivalent to 4 times the free fatty acid was added as a powder, and the mixture was sufficiently stirred at room temperature until metal soap was formed and filtered. The results of obtaining the recovery rates of fatty acids and pigments remaining in the oily substance obtained by concentrating the filtrate under reduced pressure are shown in Table 3 (removal of fatty acids from pigment oil). 90% or more of the free fatty acids were removed, and the pigment concentration was concentrated 2.9 times.

[0031]

[Table 3]

Concentrated Dye Oil Production Example 3 1 g of dye oil (free fatty acid: 75.39%) was dissolved in 20 ml of acetone, and the free fatty acid in the dye oil and an equivalent amount of potassium hydroxide were added to sufficiently precipitate the fatty acid. The resulting potassium soap was filtered and concentrated.
Acetone was distilled off from the filtrate under reduced pressure, and the recovery rate of fatty acid and dye remaining in the oily substance obtained was obtained. As shown in Table 4 (removal of fatty acids in pigment oil), the free fatty acids were 92.1%.
Removal of dye improved to 90.2%, and dye concentration was 2.
It became 8 times.

The effects of the alkali treatment on the lipid composition, fatty acid composition and pigment composition of the extracted pigment oil are shown in Table 5 (composition change due to concentration treatment). Fatty acids were selectively removed from lipids by alkali treatment, and palmitic acid was most removed from free fatty acids, followed by oleic acid and linoleic acid. There was no change in the astaxanthin ratio in the dye composition, and there was no effect of alkali treatment.

[0034]

[Table 4]

[0035]

[Table 5]

The same treatment was carried out using hexane, hexane: ethanol (85:15) and ethanol, and the fat recovery rate and pigment recovery rate were determined. The results are shown in Table 6 (removal of fatty acids from pigment oil in hexane / ethanol system). As shown in Table 6, these hexanes and hexanes:
The removal rate of lipid (ethanol: 85: 15) and the solvent of ethanol and the recovery rate of the dye were remarkably lower than those of acetone, and its concentration effect was not observed.

[0037]

[Table 6]

Concentrated Dye Oil Production Example 4 This shows the case where the alkali treatment and the low temperature fractionation were carried out continuously or simultaneously. For continuous treatment, 10 g of crude extracted pigment oil was dissolved in 5 times the amount of acetone, potassium hydroxide equivalent to the free fatty acid in the pigment oil was added, and the mixture was stirred until potassium soap was sufficiently formed, and then potassium soap was filtered once. Aside,
Furthermore, low temperature fractionation was performed at -50 ° C for 1 hour. Simultaneous treatment was carried out by adding 5 times the amount of acetone to 10 g of crude extracted pigment oil, adding free fatty acid in the pigment oil and an equivalent amount of potassium hydroxide,
Low temperature fractionation was performed at -50 ° C for 1 hour.

When low temperature fractionation was carried out after the alkali treatment, a small amount of free fatty acids, triglycerides, sterols and the like remaining after the alkali treatment were removed and the dye was concentrated about 4.4 times. The dye was 4.2 times more concentrated when the two treatments were performed simultaneously. Table 7 shows the results of the alkali treatment, the continuous treatment of the low temperature fractionation and the simultaneous treatment.

[0040]

[Table 7]

Concentrated Dye Oil Production Example 5 About 20 kg of a concentrated dye oil obtained by the continuous treatment of Concentrated Dye Production Example 4 was allowed to remain with steam under the following conditions. Vacuum degree: 30 Torr Temperature: Tower top 96 ° C., Tower bottom 140 ° C. Vapor amount: 5 kg / hr Feed amount: 20 kg / hr The residual solvent was completely removed from 0.3% before the steam distillation. . In addition, the deodorizing effect was lowered to a level at which there was no problem in use by sensory evaluation. Since steam distillation is carried out at a relatively high temperature, there is a concern that the dye may be lost, but due to the countercurrent contact with steam, there was little decrease in the amount of dye before and after the treatment due to the short residence time at high temperature.

Example 1 Sugar ester and sodium caseinate were dissolved in distilled water in the following blending ratio. The concentrated pigment oil and monoglyceride obtained in Concentrated pigment production example 5 were heated (70 ° C).
The mixture was mixed with stirring to obtain a pre-emulsion. A high pressure homogenizer (150 kg / cm ² , 2
Times) to obtain an emulsion concentrated pigment oil. Concentrated pigment oil 20 g Sugar ester 0.6 g Monoglyceride 0.4 g Sodium casein 1.0 g Distilled water 78 g

Example 2 By the same method as in Example 1, an emulsified concentrated pigment oil was obtained with the following compounding ratio. Concentrated dye oil 20 g Enzyme-treated lecithin 0.2 g Monoglyceride 0.2 g Polyglycerin ester 0.6 g Distilled water 79 g

[0044]

EFFECTS OF THE INVENTION The red pigment produced by Phaffia yeast can be provided as an emulsion of a concentrated pigment oil containing a small amount of contaminants, odorless, and containing no solvent. Emulsification of concentrated natural red pigment oil for foods, which is used as a new functional natural edible pigment having not only excellent color tone, light resistance and colorability but also physiological activity such as antioxidant activity, anti-inflammatory effect and immunostimulatory effect. You can provide things.

Claims (10)

[Claims] 1. A crude pigment oil is obtained by subjecting Phaffia yeast producing a red pigment to an extraction solvent using a mixture of hexane and ethanol as an extraction solvent, and then concentrating the crude pigment oil to obtain a food product. A method for producing an emulsion of concentrated natural red dye oil for food, which comprises adding a food emulsifier to concentrated natural red dye oil for stirring to form an emulsion. 2. A red dye-producing Phaffia yeast is subjected to an extraction treatment using a mixed liquid of hexane and ethanol as an extraction solvent, and then the obtained crude pigment oil is subjected to a concentration treatment and a deodorizing treatment to obtain a food product. A method for producing an emulsion of concentrated natural red dye oil for food, which comprises adding a food emulsifier to concentrated natural red dye oil and stirring the mixture to form an emulsion. 3. The method for producing an emulsion of concentrated natural red dye oil for foods according to claim 2, wherein the deodorizing treatment is steam distillation. 4. The process for producing an emulsion of a concentrated natural red dye oil for food according to claim 1, 2 or 3, wherein the concentration treatment is a low temperature fractionation treatment and / or a saponification treatment. 5. The method for producing an emulsion of concentrated natural red dye oil for foods according to claim 4, wherein when the low temperature fractionation treatment and the saponification treatment are used in combination, the low temperature fractionation treatment is first performed and then the saponification treatment is performed. 6. The method for producing an emulsion of concentrated natural red dye oil for foods according to claim 4, wherein when the low temperature fractionation treatment and the saponification treatment are used in combination, the low temperature fractionation treatment and the saponification treatment are carried out at the same time. 7. The method for producing an emulsion of concentrated natural red dye oil for food according to claim 4, 5 or 6, wherein the saponification treatment is an application of a method for forming a fatty acid alkali soap. 8. The method for producing an emulsion of a concentrated natural red dye oil for food according to claim 4, 5 or 6, wherein the saponification treatment is an application of a metal soap forming method of fatty acid. 9. The use of a fatty acid ester and / or a polyglycerin ester as a food emulsifier, claim 1, claim 2, claim 3, claim 4, claim 5, claim 6, claim 7 or claim 8. A process for producing an emulsion of the concentrated natural red dye oil for food as described. 10. A food concentrate obtained by the method according to claim 1, claim 2, claim 3, claim 4, claim 5, claim 6, claim 7, claim 8 or claim 9. Emulsion of natural red pigment oil.