RU2516637C1 - Method of obtaining natural mixed carotinoid-anthocyanine dye - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: to obtain dye applied is milled thermally processed carrot and dried and milled squeezed blackberry berries Carrot is crushed to small chips and processed in air atmosphere at 40°C, 60°C and 80°C with keeping at each temperature for 2 hours Squeezed blackberry barriers are dried at 55-60°C and milled Mixture of prepared carrot and squeezed berries in ratio 1:1-3:1 is twice extracted by 4-multiple volume of ethyl alcohol with volume part of ethanol 96% at 55-60°C for 1 hour Extracts are combined, settled for 2 hours, filtered and concentrated under vacuum to the content of dry substances not less than 68%.

EFFECT: obtaining natural dye, enriched with natural antioxidants, with high dyeing ability with extension of colour range from yellow to vinous-red and reduction of prime cost of dye due to application of wastes of blackberry berries processing.

1 dwg, 1 tbl, 3 ex

Description

The invention relates to the food industry, in particular to methods for producing natural dyes from vegetable natural colored raw materials, and can be used for coloring various food products.

A known method of producing carotenoid dyes [OA Kharlamova, B.V. Kafka Natural food colors. - M.: Food industry, 1979. - 191 p .; S.E. Kudritskaya. Carotenoids of fruits and berries. - Kiev. Higher School, 1990. - 211 p., A.P. Nechaev, A.A. Kochetkova, A.N. Zaitsev. Nutritional supplements. - M .: Kolos, 2001. - 256 S.], including the preparation and grinding of raw materials, followed by extraction of pigments with an organic solvent, concentration of the extract.

The disadvantage of this method is that in the process of extraction insoluble hydrophobic β-carotene is recovered.

A known method of producing soluble in polar solvents of natural carotenoid dyes [A method of obtaining a modified carotenoid dye from plant materials. RF patent №2139306, IPC С09В 61/00. Bolotov V.M., Magomedov G.O., Rudakov O.B., Komarova E.V. Claim 07/20/98. Publ. 10.10.99], including grinding and drying of natural carotenoid raw materials, thermal oxidation of natural hydrocarbon carotenoid pigments with atmospheric oxygen in the feedstock, followed by extraction extraction of coloring substances with ethanol.

The disadvantage of this method is the low quality of the dye due to the formation of melanoidins and the destruction of part of natural β-carotene during prolonged heat treatment from 11 to 12 hours at a high temperature of 110-160 ^º C.

A known traditional method for producing red anthocyanin food coloring from squeezed berries of black currant and aronia [O.A. Kharlamova, B.V. Kafka Natural food colors. - M.: Food industry, 1979. P. 91 - 99], which consists in double extraction of frozen pomace with hot water, acidified with citric acid, combining the obtained extracts and concentrating them by evaporation under vacuum.

The disadvantage of this method is that the dye obtained in this way can be used for coloring a limited range of food products, in particular confectionery.

The closest in technical essence and the achieved effect is a method for producing anthocyanin dye from fruit raw materials [RF patent No. 2228344, IPC С09В 61/00. Odin A.P., Khayrutdinova A.D., Bolotov V.M. Claim 11/19/2002. Publ. 05/10/2004, bull. No. 13], including drying and grinding squeezed berries of blackcurrant and chokeberry, twofold extraction of dyes with 96% ethanol at a temperature of 50-65 ° C with holding at each temperature for 1-1.5 hours with constant stirring and then combining both fractions of the extract, settling it at a temperature of 10-20 ° C for 6-8 hours, concentrating to a dry matter content of 55-65% by distillation of ethanol at a pressure of 140-170 mm Hg and a temperature of 30-40 ° C.

The disadvantage of this method is the ability to extract only anthocyanin pigments, the duration of the settling process of the combined extract.

An object of the invention is to develop a method for producing a natural carotenoid-anthocyanin dye, which allows to obtain a natural dye with a high coloring ability and enriched with natural antioxidants contained in the feedstock (squeezed blackcurrant and chopped carrots), to increase the efficiency of allocation of coloring substances, vary the weight ratio of the weighed portions raw materials to obtain a wide color gamut of the produced dye from burgundy red (if appropriate Ocean feedstock dried and ground black currant pomace and shredded carrot thermoprocessed 1: 1) to yellow (in the ratio 1: 3, respectively). These mass ratios of the raw materials are selected based on the color characteristics of the obtained dyes and considerations of economy of the used extractant (ethyl alcohol).

To solve the technical problem of the invention, a method for producing a natural carotenoid-anthocyanin dye is proposed, characterized in that the raw material for the dye is a mixture of the carotenoid component, which is used as a crushed heat-treated carrot, and the anthocyanin component, which are dried and crushed squeezed blackcurrant berries, while carrots are crushed to small chips and subjected to stepwise gradient processing in an atmosphere of air at temperatures x 40, 60, 80ºС with exposure at each temperature for 2 hours, squeezed blackcurrant berries are dried at a temperature of 55-60ºС and chopped, then prepared carrots and squeezed blackcurrant berries, mixed in a ratio of 1: 1 ÷ 3: 1 are extracted 4 -fold volume of ethyl alcohol with a volume fraction of ethanol of 96%, stirring periodically, extraction is carried out twice at a temperature of 55-60 ° C for 1 h, followed by combining the obtained extracts, the combined extract is left to stand for 2 hours, filtered and concentrated in vacuo to soda Zhaniya dry matter at least 68%.

The technical result consists in improving the quality and completeness of the coloring substances of the obtained natural mixed carotenoid-anthocyanin dye due to the presence of both carotenoids and anthocyanins, which are natural antioxidants.

A method of obtaining a natural carotenoid-anthocyanin dye is carried out as follows: pure carrot roots are chopped into fine chips, then subjected to stepwise gradient processing at temperatures of 40, 60, 80 ° C with exposure at each temperature for 2 hours. Anthocyanin raw materials, which are used to squeeze blackcurrant berries, are dried at a temperature of 55-60 ° C to constant weight and chopped, after which prepared carrots and dried and crushed squeezed blackcurrant berries are mixed in a weight ratio of 1: 1 ÷ 3: 1 to obtain the desired color of the obtained dye (from burgundy red with a raw material ratio of dried and crushed squeezed berries of black currant and chopped heat-treated carrots 1: 1 to yellow at a ratio of 3: 1, respectively), data on the weights of the raw materials were selected based on the demand for the dye produced, and then they were coextracted with a four-fold volume of ethyl alcohol with a volume fraction of ethanol of at least 96% for two hours at 55-60 ° C with periodic stirring, the obtained extracts were mixed, settled for 2 hours , filtered and concentrated in vacuo to a solids content of at least 68%. The finished carotenoid-anthocyanin dye is packaged in a glass container.

In the study of alcohol solutions of dyes, a shift in the light absorption maxima relative to individual colorants is observed. So, the light absorption maxima of alcoholic solutions of carotenoids (pure β-carotene) correspond to wavelengths of 420, 460 and 480 nm, anthocyanins 549 nm, and carotenoid-anthocyanin dyes 424, 445, 473 and 542 nm.

The figure 1 presents the electronic absorption spectrum of an alcohol dye solution at a wavelength of 375-600 nm.

A method of obtaining a natural carotenoid-anthocyanin dye is illustrated by the following examples.

Example 1 (prototype)

Raw materials - squeezed berries of blackcurrant and chokeberry - dried, then crushed, treated with 96% ethyl alcohol at the rate of 600 ml of alcohol per 100 g of raw material. The extraction is carried out at a temperature of 60 ° C for 1.2 hours with constant stirring. The extract obtained is separated from the feed by filtration. The extraction operation is carried out in a similar manner again. After the second extraction, the extraction of coloring substances is stopped, the extracts are combined, settled for 6 hours at 10 ° C, filtered and subjected to concentration by distillation of ethyl alcohol at 40 ° C and a pressure of 160 mm Hg up to about 1/8 of the original volume of the extract. The distilled alcohol is again sent for extraction; the residue is subjected to further concentration to a solids content of 60%.

Example 2

Pure carrot root vegetables are crushed to small chips and subjected to a stepwise gradient treatment in an atmosphere of air at temperatures of 40.60.80 ° C with exposure at each temperature for 2 hours. Squeezed blackcurrant berries are dried at a temperature of 55 ° C and chopped. Then, prepared carrots and squeezes of blackcurrant berries are mixed in a ratio of 3: 1 and the mixture is extracted with a four-fold volume of ethyl alcohol with a volume fraction of ethanol of at least 96% for 1 h twice at a temperature of 55 ° C, followed by combining of the extracts. The resulting extract was sedimented for 2 hours, filtered and then concentrated by evaporation in vacuo to a solids content of 68%.

The resulting dye is analyzed, the analysis data are presented in table 1.

Example 3

The preparation of raw materials is carried out analogously to example 2, but the squeezed berries of black currant are dried at 60 ° C, then they are crushed, the prepared carrots and squeezed berries of black currant are mixed in a weight ratio of 1: 1, then extraction is carried out according to example 2, but at a temperature of 60 ° C, concentration is carried out.

The resulting dye is analyzed, the data are presented in table 1.

The main quality indicators of carotenoid-anthocyanin dyes obtained in examples 2 and 3 are presented in table 1.

Table 1. Data analysis of dyes in the examples

Name
indicator
dye one
(prototype) 2 3 Organoleptic indicators Appearance and color Dark red viscous liquid Intense syrupy thick yellow-brown liquid Thick syrupy liquid maroon Smell Weak specific, odorless physical and chemical indicators The content of extractives,% 57.1 68 70 The content of dyes according to CoSO ₄ , g / kg 123.1 210 228.8 The content of carotenoids in terms of β-carotene, g / DM ³ - 378.2 236.5 Solubility in water Infinitely soluble It is soluble in ethanol solutions with an ethanol content of at least 10% PH acidity 2.49 3,5 2

As can be seen from table 1, the dyes obtained in examples 2 and 3 differ from the prototype in a higher content of extractive substances, the simultaneous presence of carotenoids and anthocyanins, in the claimed dye samples there is also a higher content of anthocyanins than in the prototype. In addition, due to the use of squeezed blackcurrant berries, which are processing waste, as a raw material for the production of carotenoid-anthocyanin dye, it is possible to reduce its final cost. Thanks to this technology, it is possible to obtain dye concentrates with a higher content of extractive and coloring substances than in the prototype, which, when introduced into the product, will significantly reduce the amount of dye used without compromising the quality characteristics.

The proposed method for producing a natural carotenoid-anthocyanin dye allows:

- to obtain a dye with a sufficiently high content of coloring substances and, as a result, having a high coloring ability;

- get a natural dye rich in natural antioxidants;

- to expand the color gamut of the produced dye, due to the variation in the masses of weights of carotenoid and anthocyanin raw materials;

- reduce the cost of the final product through the use of waste processing blackcurrant berries as raw materials for natural dye.

Claims (1)

A method of obtaining a natural carotenoid-anthocyanin dye, characterized in that the raw material for the dye is a mixture of the carotenoid component, which is used as a crushed heat-treated carrot, and the anthocyanin component, which are dried and crushed squeezed berries of black currant, while carrots are crushed to fine chips and subjected to stepwise gradient processing in an atmosphere of air at temperatures of 40, 60, 80ºС with exposure at each temperature for 2 hours, survive ki blackcurrant berries are dried at a temperature of 55-60 ° C and chopped, then the prepared carrots and squeezed blackcurrant berries, mixed in a ratio of 1: 1-3: 1, are extracted with a 4-fold volume of ethanol with a volume fraction of ethanol of 96%, stirring periodically, extraction is carried out twice at a temperature of 55-60 ° C for 1 hour, followed by combining the obtained extracts, the combined extract is left to stand for 2 hours, filtered and concentrated in vacuo to a dry matter content of at least 68%.

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