RU2496813C2 - Method of producing chlorophyll from high water plants - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: method of producing chlorophyll from high water plants involves washing plant material, crushing, drying the material, extraction with a mixture of hexane and ethyl alcohol, filtering, stripping the solvent, mixing chlorophyll with oil or with NaOH solution in ethanol, and separating chlorophyll in form of a solution.

EFFECT: high output and quality of the food additive.

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Description

The invention relates to the food industry, and in particular to technologies for producing a natural food coloring - chlorophyll from freshwater grass of the Volga river avatelle of the pronotifolia (Potamogeton perfoliatus) and from the sea grass of the Caspian zoster (Zostera nana).

A known method of producing a food additive from plant materials, including grinding dried parsley, extraction under countercurrent conditions with 96% alcohol with a ratio of raw materials and extractant 1: 2-1: 4 for no more than 40 minutes in the presence of MgCO ₃ or MgO, or mixtures thereof 0.1-1.0% of the amount of raw materials at 10-22 ° C. The extract is filtered, collected in a common container, the solvent is distilled off and concentrated at a temperature not exceeding 40 ° C and a residual pressure of not more than 1333 Pa for 1 h, dried to a dry matter content of 78-80% (see RF patent No. 2154075, 2000 g .).

The disadvantages of this method are: the use of ethyl alcohol as extractant, which does not provide the maximum yield of chlorophyll from marine and freshwater grass, over time, chlorophyll in ethanol forms allomeric forms that are unstable during storage. The final product of this method is a black-green paste, which does not provide the necessary color characteristics.

There is also known a method for producing copper derivatives of chlorophyll, including processing waste processing of grassy raw materials, resinous lipid complex with an ethanol solution of chlorinated copper at pH 4.0-5.5 (see RF patent No. 2034556, 1995).

The disadvantage of this method is the use of ethanol as an extractant, which does not provide maximum yield of chlorophyll from marine and freshwater grass. The final product, an oily solution of copper derivatives of chlorophyll, contains ethanol and a lipid complex, which limits its use in certain food products.

The closest in essence (prototype) is a method of processing brown algae, including the extraction of crushed algae (kelp and fucus vesiculus) with an organic solvent with the number of carbon atoms from 1 to 6 at a ratio of raw materials: extractant 1: 1-20. After distilling off the solvent, a lipid concentrate and an aqueous extract are obtained, which are separated. The aqueous extract is dried to obtain a water-soluble concentrate (see RF patent No. 2132622, 1999).

However, the known method has drawbacks: during the extraction, the extractant is heated to the boiling point (above 60 ° C), due to which chlorophyll is destroyed, which leads to a low-quality dye. The extractants used in the method do not ensure the complete extraction of chlorophyll from sea and freshwater grass and are not safe for humans. In addition, the final product, a lipid concentrate, contains fats, various pigments, fat-soluble vitamins, sugars, essential amino acids and proteins, trace elements, so the product is not a food coloring for the intended purpose.

The technical task is to create a method for producing natural food additives (chlorophyll concentrate) from higher aquatic plants while maintaining the possibility of further processing of this type of raw material.

The technical result is an improvement in the quality of a nutritional supplement. It is achieved by the fact that the drying of raw materials is carried out to a moisture content of 5% at a temperature of 45 ° C, extraction is carried out in two stages for 8 hours each with a mixture of hexane and ethyl alcohol in a ratio of 9: 1 at a temperature of 25-40 ° C.

The proposed method is as follows:

Harvested dry vegetable raw materials rhizome przednolistny (Potamogeton perfoliatus) and Caspian zoster (Zostera papa) are washed with water to remove dust and contaminants, excess water is removed by swelling and crushed to a size of 0.1-1.5 cm. Next, the grass is sent for drying in a drying chamber at a temperature of 45 ° C for 0.5-1 hours to a moisture content below equilibrium 5% and extraction is carried out in two stages of 8 hours with a mixture of hexane and ethyl alcohol in a ratio of 9: 1 at a temperature of 25-40 ° C and a water module of 1:10 -fifteen. The extract is drained and filtered, and the herbal residue is sent for further processing - obtaining pectin substances and feed products. The solvent is distilled off at a temperature of 68-78.4 ° C from the extract and returned to the production cycle. Chlorophyll is dissolved in deodorized clear vegetable oil. Packed in a glass container of opaque glass, sealed and packaged.

The selected parameters of drying and extraction of raw materials are justified by the fact that the use of temperature conditions not higher than 45 ° C ensures the protection of the chlorophyll pigment from partial or complete destruction, which ultimately leads to the production of a low-quality food coloring. The duration of extraction (8 h) and the extractants used ensure the completeness of extraction of chlorophyll from marine and freshwater grass.

Example 1

A method of producing chlorophyll in the form of an oil solution.

Harvested dry grass - 50 g. Of resta or zosters are washed with cold water (in the shower) and swelling is carried out for 15 minutes. Next, the grass is ground to a particle size of 1 cm in length and dried in a drying chamber at a temperature of 45 ° C for 1 hour to a moisture content of 5%. Extraction is carried out in two stages of 8 hours with a mixture of hexane and ethyl alcohol in a ratio of 9: 1 at a temperature of 25-30 ° C and a water module of 1:10. The raw material is placed in a sealed extraction container and poured with an extractant (mixture of 450 g of hexane and 50 g of ethanol). The extracts separated from the grass after the first and second stages are mixed and filtered through a glass filter, and the grass residue is sent for further processing. The total yield of chlorophyll after two stages is 0.74% by weight of the feed. The solvent is distilled off from the obtained extract in a vacuum rotary evaporator, and then the pigment is mixed with 100 g of deodorized clear vegetable oil. A bright green liquid is obtained. The dye is poured into a glass container of opaque glass, sealed and packaged.

Example 2

A method of producing chlorophyll in the form of an aqueous solution.

All technological operations are carried out analogously to example 1. The resulting extract after filtration is subjected to distillation of the solvent, mixed with a 25% solution of NaOH in ethanol in a ratio of 1: 1, and the chlorophyll saponification reaction is carried out for 1 hour at a temperature of 45-50 ° C. Next, warm water is added with stirring in a ratio of 1: 2. After settling, an aqueous chlorophyll solution is separated.

Improving the quality of the food additive is achieved by using a mixture of hexane with ethyl alcohol as an extractant, which prevents the formation of allomer forms of chlorophyll unstable during storage, while ensuring its maximum yield from marine and freshwater grass.

Thus, the proposed method for producing chlorophyll from higher aquatic plants allows to increase its yield and quality, as well as to carry out further processing (obtaining pectin and feed products) of the grass residue. The resulting natural food supplement, chlorophyll, is not only harmless to human health, but also has an immunostimulating effect and is effective in the treatment of cancer and infectious diseases. Therefore, chlorophyll can be used not only as a natural food supplement, but also used in the manufacture of biologically active additives (BAA).

Claims (1)

A method of producing chlorophyll from higher water plants, including washing plant materials, grinding, drying the raw materials at a temperature of 45 ° C to a moisture content of 5%, extraction, carried out in two stages of 8 hours each with a mixture of hexane and ethyl alcohol in a ratio of 9: 1 at a temperature of 25 -40 ° C, filtering, distilling off the solvent, mixing chlorophyll with vegetable oil or with a 25% solution of NaOH in ethanol in a 1: 1 ratio for 1 h at a temperature of 45-50 ° C, followed by the addition of water, and separating chlorophyll into in the form of a solution.