RU2390130C1 - Method of obtaining of biologically active additive - Google Patents

Abstract

FIELD: agriculture. ^ SUBSTANCE: invention refers to area of the substances influencing on plants growth and development. The method of obtaining of biologically active additive is carried out by drying the leaves of the mountaineer Sakhalin Reynoutria sachalinensis under normal conditions within 10-20 days and it's crushing. Later select a fraction of 0.5-4.0 mm and extract it by mix of carbon dioxide in a supercritical condition and the ethanol taken in number of 0.5-15 % of weights, of carbon dioxide weigh. Thus the correlation of fraction of the crushed leaves and extragent weightis from 2 % to 12 %. ^ EFFECT: invention allows expanding assortment of biologically active substances influencing of plants growth and development. ^ 2 dwg

Description

The invention relates to the field of production of biologically active preparations, namely, substances that affect the growth and development of plants, by extraction with a solvent, preferably carbon dioxide in a supercritical state, from parts of plants.

Known (RU, patent 2025985) is a method for the manufacture of herbal preparations for feed, including grinding plant materials, preparing an extracting mixture, combining the crushed raw materials with it and obtaining an extract. When implementing the method, the preparation of the extracting mixture is carried out by dissolving inorganic salts in the vapor condensate, and the compound of the crushed vegetable raw materials with the extracting mixture is carried out in a ratio of 1: 6.5, after which the pulp is obtained by processing the resulting mixture in an extractor-dispersant at a temperature of not more than 60 ° С then the pulp is processed by heating it to a temperature of 150 ° С, holding it at a pressure of 4.8 · 10 ⁵ Pa for 30-35 min, followed by a sharp decrease in pressure to 1.0 · 10 ⁵ Pa and cooling precipitation to a temperature of 50-55 ° C, and extracting is carried out by separation of the raffinate solid fraction from the cooled pulp. After receiving the extract, it is purified from ballast substances and microparticles, then it is evaporated to 50% concentration of dry matter in the extract under vacuum at a temperature of not more than 100 ° C, and then phytopreparations are obtained by drying a 50% extract concentrate at a temperature not more than 90 ° C and until the humidity reaches 11.5-12.5%.

The disadvantage of this method should recognize its duration and complexity.

Known (RU, patent 2060683) is a method for producing a biologically active additive, including grinding vegetable raw materials, preparing an extracting mixture, combining ground vegetable raw materials in a steam condensate with it, treating the pulp by heating it, separating the solid fraction from the cooled pulp, purifying the extract from ballast substances, and microparticles, evaporating the extract under vacuum. In this case, the crushed vegetable raw materials in the first stage of extraction are soaked in a cold extraction mixture with inorganic salts dissolved in it in a ratio of 1: 6.5 and kept for 20-60 minutes, the pulp solid fraction is separated, and the extract is processed by heating to 130 to 155 ° C at a pressure soak of 4.5 · 10 ⁵ ÷ 6.5 · 10 ⁵ Pa for 30 ÷ 35 min, the extract is evaporated under vacuum to 35–45% of the dry matter content in the extract at a temperature of not more than 100 ° С.

The disadvantage of this method should recognize its duration and complexity.

Known (RU patent, 2086249) is a method for producing a biologically active preparation for treating diseases of farm animals, comprising extracting plant materials with an organic solvent, and dimexide is used as extractant and organic solvent.

The disadvantage of this method should recognize the narrow scope of its application.

The technical problem solved by the developed method is to expand the range of biologically active substances that affect the growth and development of plants.

The technical result obtained by the implementation of the developed method consists in obtaining a new biologically active preparation from the Sakhalin mountaineer Reynoutria sachalinensis, which affects the growth and development of plants.

To obtain the specified biologically active additives, it is proposed to use the developed extraction method. When implementing the developed method, the leaves of the Sakhalin mountaineer Reynoutria sachalinensis are dried under normal conditions for 10-20 days, crushed, a fraction of crushed leaves of 0.5-4.0 mm is taken and extracted with a mixture of supercritical carbon dioxide and ethanol taken in an amount of 0 , 5-15 wt.% By weight of carbon dioxide, while the ratio of the mass of crushed leaves and the mass of the extractant is from 2 to 12%.

In a preferred embodiment, the leaves are ground to a fraction of 1-3 mm. Drying was carried out preferably within 14-16 days. The extraction was preferably carried out with a mixture of supercritical carbon dioxide and ethanol taken in an amount of 1-10 wt.% By weight of carbon dioxide.

During the patent search, no solutions were found aimed at extracting the leaves of the Sakhalin highlander Reynoutria sachalinensis using a mixture of supercritical carbon dioxide and ethanol as an extractant.

When implementing the method, standard equipment for supercritical fluid extraction is used, as well as a standard laboratory plant grinder.

In determining the optimal conditions for the experiment, it was found that less than 0.5 wt.% Ethanol does not produce a solution, but a homogeneous paste, the shelf life of which does not exceed two weeks. The use of ethanol in amounts exceeding 15 wt.%, Does not allow to isolate from the plant mass all the necessary active components. Grinding leaves to a size of less than 0.5 mm is not advisable, since this does not affect the extraction results, but significantly increases the grinding process time. Grinding the leaves to a size of more than 4 mm does not allow the complete extraction of biologically active substances from the leaves. Drying the leaves for less than 10 days does not allow moisture to be removed from them to a residual amount that impedes the completeness of extraction; exceeding the drying period of more than 20 days does not affect the completeness and quality of extraction.

The method was implemented as follows.

The leaves of the Sakhalin mountaineer Reynoutria sachalinensis were dried under normal conditions without additional heating for 15 days (humidity was not determined). The dried leaves were crushed to fractions 1-3 mm and placed in a 200 ml extraction vessel. Extraction was performed on a SFE-1000M1-2-FMC50 plant manufactured by Thar Instruments, Inc. As a solvent, carbon dioxide was used in a supercritical state with the addition of 1-10% ethanol by weight as a co-solvent. The result was an extract of dark green color with a brownish tint with a herbal aroma. The extract is an active substance dissolved in alcohol.

The obtained extract has the following characteristics: it leads to an increase in the photosynthetic activity of plant leaves treated with this drug, effectively protects crops from phytopathogenic fungi, and induces plant resistance to infection and adverse conditions.

The homogeneity of the obtained product is proved using the chromatographic method of analysis. Analysis was performed on a Semi-Prep Investigator supercritical fluid chromatograph manufactured by Thar Instruments, Inc. The product was obtained by the same method from raw materials taken from various lots. All chromatograms obtained in the analysis of the alcohol solution of the final product are identical (see figure 1 - analysis of the product obtained from raw materials collected in late July, and figure 2 - analysis of the product obtained from raw materials collected in early September).

When using the product, dilute it with water in accordance with subsequent use. For example, when used as an accelerator of seed germination, an aqueous solution containing 3 ml of product per 100 ml of water is used. Seeds are soaked in the solution for about 6 hours. When using the product as a growth promoter, use a solution of 2 ml of the product per 100 ml of water. The resulting aqueous solution is sprayed with plants at the rate of 100 ml of the final solution in approximately 2 m ^{2 of} plants. When used as a root dressing of plants, a solution of 1 ml of product per 100 ml of water is used; plants are watered at the roots with this solution at the rate of 100 ml per 1 m ² . When using the extract as an activator of bean seed germination, the following results were obtained: in comparison with bean plants whose seeds were treated with water, bean plants whose seeds were treated with Reynoutria sachalinensis SCF extract diluted with water to a concentration of 2%, sprouted by 2-3 days faster and 1-2 days faster than plants whose seeds were treated with Epin-extra in the concentration recommended by the manufacturer. At the same time, the germination rate of seeds treated with the Reynoutria sachalinensis GFR extract was higher than for plants treated with water or the Epin-Extra solution, the plants were noticeably stronger, developed faster and were more resistant to adverse conditions such as freezing and drought. When spraying leaves, for example, beans and cucumbers, it was found that the photosynthetic activity of plants increases by 37% compared to control (plants treated with water) and by 22-25% compared to plants treated with Epin-Extra and Zircon preparations diluted to concentrations recommended on the package. An increase in photosynthetic activity led to an increase in the green mass of plants. It was noted that plants treated with GFR-extract of Reynoutria sachalinensis were more resistant to drought and infection by phytopathogenic fungi and thrips. When used as a root dressing, plants treated with Reynoutria sachalinensis GFR extract were compared with plants that were watered with water, a solution of Epin-Extra and Zircon. It was found that plants treated with the GFR extract of Reynoutria sachalinensis are more resistant to drought and frost, as well as stronger. These plants develop faster and within a week from the time of feeding, the height of the bean plants treated with GFR-extract of Reynoutria sachalinensis increased by about 7 cm, while the height of the control (water-treated) plants increased by 3-4 cm, and the height of the plants treated with the preparations Epin-Extra and Zircon increased by an average of 4-5 cm.

It was established that the product obtained in this way is not toxic, and toxic substances are not used in its preparation. When disposing of a product that has expired, no additional cleaning agents are required.

Claims (1)

A method of obtaining a biologically active additive, characterized in that the leaves of the Sakhalin mountaineer Reynoutria sachalinensis are dried under normal conditions for 10-20 days, crushed, a fraction of 0.5-4.0 mm is taken and extracted with a mixture of supercritical carbon dioxide and ethanol, taken in an amount of 0.5-15 wt.% by weight of carbon dioxide, while the ratio of the fraction of crushed leaves from the mass of extractant is from 2 to 12%.

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