SU1693001A1 - Method for preparation of red food dye - Google Patents

Abstract

The invention relates to the food industry, in particular, to the technology for producing food dye from vegetable raw materials. The purpose of the invention is to increase the yield of the dye and improve its quality. To obtain a red food dye, extraction of black grape varieties was carried out with a 28-33% aqueous solution of ethyl alcohol containing a mixture of citric and acetic acids in an amount of 0.9-1.0% and 0.4-0.5%, respectively the subsequent concentration of the obtained extract to a dry matter content of 37-42% and anthocyanins 34-39 g / l, settling the concentrate, separating the precipitated precipitate from an aqueous solution of anthocyanins, dissolving the precipitate in ethyl alcohol containing 0.5-1.0% citric acid, concentration of the resulting solution d anthocyanin content of 34-39 g / l and mixing the resulting concentrate with an aqueous solution of anthocyanins, the remaining after separating the precipitate. Stock-rose flowers were extracted with a 1.5-2.0% aqueous solution of citric acid, followed by concentration of the obtained extract at 65-70 ° C to a solids content of 42-45% and anthocyanins 33-36 g / l and by mixing concentrates derived from black grape varieties and stem-rose flowers in the ratio of 4: 1-5: 1 with the addition of tannin in the amount of 3-6% of the total mass of the concentrate. 2 tab. fe o -cso about

Description

The invention relates to the food industry, in particular, to the technology for producing food dye from vegetable raw materials.

The aim of the invention is to increase the yield, stability of the dye and improve its quality.

The method is carried out as follows.

The extraction of dyes from husks of black grape varieties and stockrose flowers is carried out from each raw material separately. Extraction of black grape varieties was carried out with a 28-33% aqueous solution of ethyl alcohol containing a mixture of acetic and citric acids in an amount of 0.4-0.5% and 0.9-1.0%, respectively, followed by concentration of the extract to dry matter 37-42% and

anthocyanins to 34–39 g / l at 65–70 ° C, separating the precipitated precipitate from the aqueous solution of anthocyanins, dissolving it in ethanol containing 0.5–1.0% citric acid, concentrating the resulting solution to anthocyanins 34- 39 g / l and mixing the obtained concentrate with the anthocyanin aqueous solution remaining after separation of the precipitate. Stock-rose flowers were extracted with a 1.5-2.0% aqueous solution of citric acid, followed by concentration of the obtained extract at 65-70 ° C to a solids content of 42-45% and anthocyanins 33-36 g / l and mixing concentrates obtained from pomace of black grape varieties and stockrose flowers in the ratio of 4: 1-5: 1 with the addition of tannin in the amount of 3-6% of the total mass of the concentrate.

The proposed sequence of methods makes it possible to extract from the flowers of the stock rose such types of anthocyanin dyes as cyanidine, pionidine, and dolphinidin glycosides, which have a bright red color. The grapes of black grape varieties produce poorly soluble in water glycosides of petunidin, malvidin and delphinidin, which impart stability to the final product and contribute to obtaining a clear mark on meat carcasses.

The extractant specified in the known method, containing 22–25% aqueous alcohol, 0.6–0.8% acetic acid, and 0.7–0.9% citric acid, completely removes anthocyanins from the stem-rose, represented by glycosides of cyanidine and peonidine, but does not fully extract the glycosides required for carcass brands — malvidin and petunidine, which are not contained in the stem-rose, but in the squeeze of black grape varieties. The results of the research show that it is necessary to use components from grape marc, to obtain a dye for clump of meat carcasses,

For a more complete extraction of anthocyanins, extraction of grape marches should be carried out with 28-33% aqueous ethanol containing citric and acetic acids, which help to extract the hardly soluble anthocyanin groups, glyvides Malvidin and Petunidine, contained in the husks of grapes.

An increase in the alcohol content in the extracting agent to 33% has little effect on the content of anthocyanins in the diffusion juice and dye concentrate from stem-ro-Zy flowers, in which the cyanidine and peonidine glycosides are the main coloring substances. When using 28-33% aqueous alcohol containing 0.5% acetic acid and 1.0% citric acid to extract anthocyanins from dark grape varieties, the content of anthocyanins in the diffusion juice and dye concentrate increases markedly, and therefore the output of anthocyanins from this kind of raw material. how

0 can be seen from the data, an increase in the number of anthocyanins compared with the known prototype is observed in the diffusion juice and in the dye concentrate. Thus, when using 28-33% aqueous

5 ethanol containing 0.5% acetic acid and 1.0% citric acid, when compared with the known method, the output of dye from grape marc, which constitutes the main part of the target product, is significantly increased. It should be noted that along with an increase in the content of anthocyanins in the dye concentrate from grape marc, the content of anthocyanin groups poorly soluble in water also increases.

5 of the final product, which are essential for obtaining a clear mark on meat carcasses.

When dye is extracted from the grape extracts of grapes, along with anthocyanins, tannin is extracted, present in this type of raw material in an amount of 1-3%. This amount was not enough to obtain a stable dye, therefore, to increase its stability to the single dye concentrate, tannin is added in an amount of 3-6% of the total weight of the dye so that the content in the final product reaches 4-8%. Tannin, besides its main binding function

0 dye with protein, increases the durability of the dye during storage.

Example 1. Preparation of dye concentrate from stem-rose flowers: 1.8 kg of air-dry stem-rose petals are loaded into 4 extractors. Anthocyanin dyes are extracted from stem-rose flowers at room temperature by sequential extraction with 1.5% aqueous citric acid solution for 2 h 40

0 min The resulting diffusion juice (extract) is concentrated in a vacuum evaporator at 65 ° C to a dry content: 42.3% and anthocyanin content to 33.2 g / l. Received 10.2 kg of kra5 concentrate concentrate from flowers of rose stem.

Preparation of dye from black grape varieties: 3.6 kg of grape residue is loaded into four extractors and the dye is successively extracted with a 30% aqueous solution of ethyl

alcohol containing 0.9% citric acid and 0.45% acetic acid for 3 h 30 min. Diffusion juice (extract) is concentrated at 65 ° C to a solids content of 38.2% and anthocyanins at 35.8 g / l. The concentrate is settled, the precipitated precipitate is separated from the aqueous solution of anthocyanins and dissolved in ethyl alcohol containing 1.0% citric acid. The alcohol solution is concentrated to an anthocyanin content of 36.5 g / l and combined with the anthocyanin aqueous solution remaining after separation of the precipitate.

4 kg of the combined aqueous and alcohol concentrate dye from grape extracts are mixed with 1 kg of dye concentrate from stem-rose flowers and when heated to 45-50 ° C and stirring add tannin in the amount of 6% of the total weight of the dye concentrate.

The resulting dye is a dark red syrupy liquid with a solids content of 41.6%, anthocyanins of 35.2 g / l, a sour taste with a fruity odor, with the following composition:

Cyanidine glycoside 0.20-0.45

Glycoside peonidina 0.60-0.95

Delphinidin glycoside 0.75-1.85 Malvidin glycoside 0.91-2.15

Petunidin glycoside 0.25-0.55

Tannin4.0-8.0

Flavonols1.0-2.0

Organic acids 13.0-18.0 Mineral salts, trace elements and polysaccharides10, 0-17.0 Water and ethyl alcohol Else To the dye concentrate, tannin can be added in the form of a solution, with 4 kg of the combined water and alcohol concentrate dye from grape marc mixed with 1 kg of dye concentrate concentrate (4: 1); 0.6 kg of a 5% solution of tannin in 65% aqueous ethanol and 0.17 kg of tannin in the form of powder are added and mixed until complete dissolution of tannin. The resulting dye is impregnated with a foam pad, a stamp is pressed to the surface of the pillow to apply a dye on it, a stamp is placed on the carcass and an impression is obtained.

Examples 2-22. Carried out as in Example 1.

The results of the dependence and quality of the dye on the process parameters are given in table. 1, which shows the average, boundary and foreign values of the process parameters and their influence on the quality, anthocyanin content and yield of the target product. Data on the dye output from stem-rose flowers and grape marc are given in table 2.

5 The most optimal amounts of citric acid — 1.5–2.0% in aqueous solution when extracting stem-rose flowers are presented in examples 1–3 (Table 1), and the concentration temperature of 65–70 ° C in

10 examples 1-6 (table. 1). An increase in the concentration of citric acid leads to an increase in the ballast substances, which affects the quality of the final product, and also leads to an increase in the consumption of citric acid (Example 8, Table 1). A decrease in the concentration of citric acid (less than 1.5%) leads to incomplete extraction of the necessary types of anthocyanin dyes (examples 5 and 7, Table 1). Extraction of the basic amount of dyes from flowers of stock-roses is carried out for 2 hours 30 minutes - 3 hours, and for dye from grape marc for 3-4 hours it is quite enough (examples 1-4, table 1).

5 A decrease in the evaporation temperature leads to inhibition of the process (Example 13, Table 2), and an increase (above 75-80 ° C) to the decomposition of anthocyanins, which also leads to a decrease in the quality of the final product

0 (examples 7 and 8, table. 1). Since the dye from grape marches is difficult to dissolve in water, it is necessary to extract the dye from the raw material in aqueous ethyl alcohol. The use of a 28-33% aqueous solution of alcohol containing 0.9-1.0% citric and 0.4-0.5% acetic acids is quite sufficient to extract the main amount of dye from grape marc and helps to remove hardly soluble parts dye. When using low concentrations of alcohol and acids, dyes are not completely removed (Example 5, Table 1), and at a concentration of more than 33% alcohol and citric acid more than 2%

5 is economically disadvantageous (examples 8 and 14S table. 1).

When evaporation of diffusion juice from grape marc, a significant part of the dye (more than 20% of the total

0 dye) precipitates out, which makes it difficult to further concentrate and obtain a dye with the necessary concentration of dye and anthocyanins.

5 Separating the precipitate by filtration facilitates further concentration of the dye, and dissolving the precipitate in alcohol containing 0.5-1.0% citric acid, followed by concentration of the alcohol solution to a content of 34-39 g / l anthocyanins, allows to obtain a dye concentrate from marc grapes with a high content of anthocyanins, represented mainly by delphinidin, malvidin and petunidin glycosides, which are essential for an optimal dye composition for meat carcass brand names. In addition, to improve the color and optimal composition of the dye, the combined aqueous and alcoholic concentrate from grape marc is mixed with the concentrate of the dye from stem-rose flowers in a ratio of 4: 1-5: 1. A dye concentrate from an alcohol solution containing 34–39 g / l anthocyanins in the presence of tannin gives a good and very clear mark on meat carcasses (Example 18, Table 1), but the dye alcohol concentrate makes up a small part of the total amount of dye. the grape marc, while the mark applied using the aqueous portion of the filtrate obtained after separating the sediment (part of the dye soluble in water), which is more than 65% of the total amount of dye, does not give a very clear spot (example 17, Table 1). When the concentrate is mixed with the aqueous part of the dye in the presence of tannin, the clarity of the stigma and, consequently, the quality of the dye is improved (Example, 16, Table 1). Therefore, for a more complete use of the dye, the water part of the dye was also used.

The ratio of concentrates obtained from grape marc and stockrose flowers 4: 1-5: 1 with the addition of tannin is optimal (examples 1-6, Table 1), and an increase in the amount of dye in grape marrows leads to the precipitation of a significant part of the dye during storage .

Claims (1)

The invention The method of obtaining a red food dye, involving the extraction of marc black grape varieties an aqueous solution of ethyl alcohol containing a mixture of citric and acetic acids, extraction of the stem-rose petals with the process of concentrating the diffusion juice extract, settling the obtained concentrate and separation of the precipitated sediment, characterized in that, in order to increase the yield, stability of the dye and improve its quality, when extracting black grape varieties, the concentration of the aqueous solution of ethyl alcohol is set to 28-33%, and citric and acetic acids are used in the amount 0.9-1.0% and 0.4-0.5%, respectively, followed by concentration of the obtained extract to a dry matter content of 37-42% and anthocyanins 34-39 g / l, settling of the concentrate with separation of the precipitated precipitate from the aqueous solution and anthocyanins, by dissolving the precipitate in ethyl alcohol containing 0.5-1.0% citric acid, concentrating the resulting solution to contain anthocyanins 34-39 g / l and mixing the resulting concentrate with an aqueous solution of anthocyanins left after separation of the precipitate, and Stock-rose flowers are extracted with a 1.5-2.0% aqueous solution of citric acid, followed by concentration of the obtained ex tract at a temperature of 65-70 ° C to a solids content of 42-45% and anthocyanins 33-36 g / l and mixing concentrates obtained from marc of black grape varieties and stem-rose flowers in 4: 1-5: 1 ratio with the addition of tannin in the amount of 3-6% of the total mass of the concentrate. .Table 1 Continuation of table 1