RU2034879C1 - Method of food dye preparing - Google Patents

Abstract

FIELD: food industry. SUBSTANCE: reagent is added to the invert sugar solution following by heating for melanoidines formation and cooling of food dye solution. Lysine (16-49 g) or a mixture of phenylalanine and lysine (16-49 g) per 100 g invert sugar is used as a reagent. Quantity of phenylalanine and lysine is 5-15 and 85-95 g, respectively, per 100 g mixture. After addition of indicated mixture to solution citrate-phosphate buffer mixture is added to the latter up to pH 7-10. Heating is carried out at 95-150 C for 1.5-10 h, and cooling is performed for two stages: firstly up to 50-70 C following by centrifugation for precipitate separation, and then - up to environment temperature. EFFECT: improved method of food dye preparing.

Description

 The invention relates to the food industry. The resulting product can be used in various liquid products and confectionery.

A method of obtaining a food colorant, comprising mixing granulated sugar with 1-2% water, heating the mixture in an open pot to 160-165 ^{° C} and a melt sugar, cessation of heating and slow mixing the resulting mass to 8% of a water temperature of 75-90 ^C. , further heating to 180-200 ^{° C,} boiling until the sample weight at which a drop of the product placed on the glass, does not spread; Slow dilution with water caramel mass temperature of 60-65 ^{° C} and 70% solids [1]
The dye obtained by this method has a brown-brown color with a low light absorption coefficient, the smell of burnt bread crust. During its manufacture, 27-30% of sugar is lost, and when dissolved, a precipitate is formed. During its preparation, harmful gases are released.

A method of obtaining a food colorant, comprising invert sucrose hydrochloric acid, adding ammonia to the syrup in excess, autoclaving at 140-150 ^{° C} for 1-1.5 hours, depressurization to atmospheric pressure and boiling until complete removal of ammonia [2]
The disadvantage of this dye is the low color intensity, faded gray-brown tint, lack of aroma, sour-bitter taste and instability in an acidic environment.

The closest to the proposed method for the technical essence and attainable result is a method for obtaining a food colorant, comprising administering to a solution of invert sugar reactant ammonium salts of sulfurous acid, sodium hydroxide solution to establish a pH of 8-11, _20, followed by heating under pressure at 145-150 ^C. during 1-1.5 hours for the formation of melanoidins and cooling of the finished product [3] The resulting food coloring does not have a taste, aroma, color, gray-brown, dull, smells of traces of ammonia. During storage, part of the molecules of the coloring matter polymerizes (“ages”) to a particle size of a colloidal degree of dispersion, some of them precipitate, and the color of the product sharply increases. The starting reagents sulfite-ammonia salts decompose quickly and are unsuitable for storage.

 The purpose of the invention is improving the quality of the dye by imparting greater stability during storage, increasing its color, as well as improving organoleptic characteristics.

To this end, the proposed method involves the introduction of an invert sugar solution of a reagent, followed by heating to form melanoidins and cooling the dye solution. The reagent used is lysine in an amount of 16-49 g or a mixture of amino acids phenylalanine and lysine in an amount of 16-49 g of the mixture per 100 g of invert sugar, while the amount of phenylalanine in 100 g of the mixture is 5-15 g, and lysine 95-85 g and after the introduction of said mixture into the solution added thereto citrate-phosphate buffer mixture until a pH of 7-10, wherein the heating is carried out at 95-150 ^{° C} for 1.5-10 hours, and cooling is performed in two stages, at the first of which up to 50-70 ^{° C} with subsequent centrifugation for separation of the precipitate, and the second mortar and to ambient temperature.

The proposed method is as follows. A lysine reagent in the amount of 16-49 g or a mixture of essential amino acids of phenylalanine and lysine in the amount of 16-49 g per 100 invert sugar is introduced into an invert sugar solution with a concentration of 25-50% solids, while the amount of phenylalanine in 100 g of the mixture is 5-15 g, and lysine 95-85 g. The ratio of invert sugar to amino acids should be at the rate of 1 mol of monosaccharide and 0.2-0.6 mol of the amino acid. In the case of using phenylalanine containing an aromatic core, the smell of the resulting dye improves. Considering that the reaction of formation of colored products of alkaline decomposition of monosaccharides will proceed in parallel with the reaction of melanoidinogenesis, this ratio of sugars and amino acids is optimal. It is known that the maximum intensity of the formation of coloring substances in the reaction occurs in the range of pH 7-10, therefore, after the introduction of amino acids into the solution, a citrate-phosphate buffer mixture is added to it, which ensures buffering at these pH values. The high concentration of reagents in the initial solution is due to the fact that in the melanoidin reaction, which is a second-order reaction, an increase in the concentration of reagents by a factor of n ensures the intensity of color formation by a factor of n ² times.

The thus obtained reaction mixture was placed in a sealed container made of corrosion-resistant material that provides minimal effect of metal ions on dye formation reaction, heating is performed to 95-150 ^{° C,} and the reaction mixture was kept under stirring for 1.5-10 hours. The sealed vessel necessary to preserve the volatile aromatic and flavoring substances formed in the dye. There is no emission of harmful gases in the reactions of sugars with amino acids, as is the case with the preparation of food coloring [1], so there is no need to remove harmful gases.

The reaction time is 1.5-10 hours related to the temperature of the reaction at the temperature 140 ^{° C} reaction duration melanoidins about 1.5 hours and the temperature decreases to 10 ^{° C} according to the van't Hoff rule, the reaction time is increased approximately 2 times. The duration of heating the reaction mixture more than recommended leads to precipitation of the dye as a result of polymerization of its molecules and, as a result, to a decrease in the color intensity of the dye.

Cooling the resulting food coloring is effected in two stages, the first of which up to 50-70 ^{° C} with subsequent centrifugation for separation of the precipitate and in the second stage to ambient temperature.

The two-stage cooling of the reaction mixture initially to 50-70 ^{° C} and then to 15-25 ^{° C} because the concentrated solutions have a high viscosity and is difficult to filter. Therefore, filtration in the present process is replaced lightening solution in a centrifugal field following the first stage of cooling it to 50-70 ^{° C,} when the viscosity is still relatively low solution. And only after clarification, the solution is cooled to storage temperature.

This dye may be further concentrated under vacuum at about 55 ^° C to a solids content of 69-72% may also be obtained by further drying of food coloring to a powder in a spray dryer.

EXAMPLE EXAMPLE 1 In 50 ml of a solution containing 25 g of invert sugar, ^at 50 ° C were dissolved 3.6 g lysine, 0.4 g phenylalanine, making 30 ml of phosphate-citrate buffer mixture. The volume of the solution was adjusted with water to 100 g, stirred for 3 minutes, placed in a hermetically sealed stainless steel vessel and heated for 10 hours in a boiling water bath. Then, the contents of the vessel cooled ^to 50 ° C, clarified in a centrifugal force field to the separation factor of 300, cooled ^to 15 ° C and analyzed. The analysis results are as follows: average pH of ₂₀ (before and after heating) 9.24; solids content (CB) 29.7% glucose by paper chromatography 2.5% by weight of the solution, fructose was not detected, the optical density of the obtained dye, when diluted 100 times, in a cuvette l = 10 mm at a wavelength of λ540 nm, pH ₂₀ 8 is D = 0.23. When recalculating the dye concentration per 1 g of CB / L, this value is equal to D = 0.92. The isoelectric point of the dye particles is at pH 1, the particle charge is negative. The hue of the dye is red-brown, the aroma of bread with a touch of rose. Durability is high.

PRI me R 2. In 65 ml of a solution containing 50 g of invert sugar, at 60 ^about With dissolved 18 g of lysine, 1.6 g of phenylalanine, make 20 ml of a solution of the buffer mixture. The solution volume was adjusted to 100 mL with water, stirred for 5 min, placed in a sealed vessel and heated for 1.5 hours in an oil bath at 145 ^C. After incubation, the content is cooled to ⁶⁰ ° C, clarified by centrifugation at a separation factor of 650, then cooled to 25 ^about C and analyze analogously to example 1. The results obtained: pH20 8.5; CB = 65.3% VCD = 0.4% by weight of CB, glucose traces, D = 0.68. When recalculating the concentration of CB dye to 1 g / l, D = 1.04. The isoelectric point of the dye is at pH 1.2, the particle charge is negative. The color of the dye is red-brown, bread flavor with pleasant tones of roses, jasmine. Durability is high.

PRI me R 3. In 60 ml of a solution containing 40 g of invert sugar, dissolve 16 g of lysine, make 20 ml of the buffer mixture. The solution volume was adjusted to 100 mL with water, stirred for 5 minutes in a closed vessel and heated for 6 hours at 125 ^C. The solution was cooled to ⁷⁰ ° C, clarified when the separation factor 650, cooled ^to 20 ° C and analyzed as in Example 1. The results obtained are: pH ₂₀ 8.8; CB = 45.8% VKD = 0.2 to the mass of CB, glucose traces, D = 0.43. When recalculating the dye concentration by 1 g / l (according to ST), D = 0.96. The isoelectric point of the dye particles is at a pH of 1.15. The particle charge is negative. The color is brown-ruby, the smell of bread.

PRI me R 4 (prototype). In 70 ml of a solution containing 50 g of invert sugar, 7 g of ammonia sulfate are added. The volume was adjusted to 100 ml water, stirred for 3 min, a concentrated NaOH solution adjusted to pH 11, the mixture is placed in a hermetically sealable container made of corrosion-resistant steel and heated in an oil bath for 1.5 h at 145 ^{° C,} then cooled ^to 20 ° C and analyze. The results obtained: pH ₂₀ 5.1; SW = 56.7% VKD = 1.5% by weight SW, 5% glucose and traces of fructose. The optical density of the dye solution with a concentration of 1 g / l at pH 8, λ540 nm, l = 10 mm, D = 0.115. The isoelectric point of the dye particles is pH 1.7, the particle charge is negative. The color is brown, dull, the smell of ammonia.

 Thus, the results presented in examples 1, 2, 3, compare favorably with the prototype. The color intensity of the dye obtained by the proposed method is approximately 5 times higher than that of the dye obtained by the prototype. The charge of the dye particles is negative, and the isoelectric point is close to pH 1, which ensures the stability of the dye in slightly acidic environments characteristic of beverages.

 The dye obtained by the proposed method does not form precipitates with plant extracts, has a bright ruby color with brown tones and a pleasant smell of freshly baked bread and flowers.

 The dye is easily concentrated by evaporation under vacuum to a thick syrup or powder, which then dissolves without precipitate. To achieve the same color intensity, its consumption is 5 times less than the dye obtained by the prototype, and 16 times less than the dye [1] Food color is storage stable, does not lose quality. Prepared, as described in examples 1-3, the dyes were stored for a year. Their parameters did not change.

 A feature of the proposed dye is its complete biological safety. Both the initial components for the preparation of the dye, and it can itself be used in the food industry to give drinks and confectionery products all shades from light yellow to dark brown with ruby tones.

Claims (1)

METHOD FOR PRODUCING FOOD DYE, which involves introducing a reagent into an invert sugar solution followed by heating to form melanoidins and cooling the food coloring solution, characterized in that 16 49 g of lysine or a mixture of phenylalanine and lysine amino acids in the amount of 16 49 g of the mixture are used per 100 g of invert sugar, while the amount of phenylalanine in 100 g of the mixture is 5 15 g, and lysine 85 95 g, after the mixture is introduced into the solution, citrate-phosphate buffer is added to the latter the mixture until pH 7 10 is reached, and heating is carried out at 95 150 ^o C for 1.5 10.0 h, and cooling is carried out in two stages, in the first of which up to 50 - 70 ^o C followed by centrifugation to separate the precipitate, and in the second stage to ambient temperature.