RU2288582C2 - Method for producing of biologically active preparation - Google Patents

Abstract

FIELD: agriculture.

SUBSTANCE: method involves extracting larch and/or fir wood with organic solvent; distilling extractant for producing of aqueous emulsion of total of biologically active natural compounds. Organic solvent used is aliphatic alcohol with 1, 2, 3 carbon atoms, or acetone containing water not in the excess of 60 wt%, or mixture of these extractants. After distilling of extractant, active substance is produced, said substance being based on total of flavonoids of the following composition, wt%: dihydroquercetinic acid 70-86; dihydrokaempferol 4-12; naringenin 2-6; other compounds being the balance. Claimed preparation is preferably used in the form of aqueous emulsion comprising 2-10 wt% of active substance.

EFFECT: increased biological activity of preparation.

2 cl, 3 ex

Description

The invention relates to methods for producing biologically active preparations from plant materials, which are a biologically active amount of natural compounds dissolved in an aqueous emulsifier solution, used to increase the productivity of agricultural plants through the use of biologically active preparations of plant origin.

A known method for the isolation of larch wood from dihydroquercytin of especially high purity (99.5%) used in medicine, namely in the pharmaceutical industry (Pat. RF No. 2111431, class A 61 K 35/95, C 07 D 311/32 published on 07/10/98). Isolation is based on the extraction of wood with aqueous acetone.

The disadvantage of this method is its complexity and high cost.

A known method of obtaining funds for the complex treatment of diseases, which consists in extracting sawdust of larch wood, filtering, evaporating the extract, recrystallizing the target product, filtering it and drying. In this method, the extraction is carried out with an aqueous-acetone extract in an acidic medium immediately after processing the raw material with boiling water, and the target product is crystallized from alcohol or an aqueous-alcoholic solution. The resulting product has a composition, wt.%: Dihydroquercetin 90-92, dihydrocampferol and naringenin 8-10, and naringenin no more than 2%. (Pat. RF No. 2088256, class A 61 K 35/78, publ. 1997.08.27).

The agent obtained in this way is used in medicine, and the method for its preparation is complicated and expensive.

The closest technical solution that we have chosen for the prototype of the claimed method, for a larger number of common features, for the achieved result and for the field of application, is a method for producing a biologically active preparation (SILK) (Pat. RF No. 2083111, class A 01 N 65/00 publ. 04/20/98).

SILK preparation is obtained by extraction of crushed dried fir green with a mixture of petroleum ether and ethyl acetate. The extract was treated with saturated aqueous sodium bicarbonate, acidified with hydrochloric acid and re-extracted with ethyl acetate. After removal of ethyl acetate, a preparation is obtained which is the sum of triterpenic acids in the form of a gray-green hygroscopic powder with an active substance content of 95% by weight. This substance is soluble in emulsifiers.

The drug obtained according to the above method, in the form of an aqueous emulsion is used to increase the productivity of agricultural plants.

The disadvantage of this method is its complexity, multi-stage, the use of expensive extractants.

The problem solved by the claimed method of obtaining the drug is to cheaper and simpler way to get a new effective drug, previously not used in crop production.

The problem is solved in that in a method for producing a biologically active preparation for increasing the yield of agricultural plants, including extraction of plant materials with an organic solvent, obtaining an aqueous emulsion of a biologically active amount of natural compounds, larch and / or fir wood is extracted with aliphatic alcohol with the number of carbon atoms 1, 2 , 3 or acetone containing not more than 60 wt.% Water, or a mixture of these extractants, and then the extractant is distilled off.

The drug is prepared in the form of an aqueous emulsion containing 2-10 wt.% The active substance.

After distillation of the extractant receive the active substance (DW) of the following composition, wt.%:

dihydroquercetin - 70-86 dihydrocampferol - 4-12 - naringenin - 2-6 - other compounds - the rest

After distillation of the extractants, it is possible to reuse them (even in the form of azeotropic mixtures) in the process of extracting organic matter from fir and / or larch wood.

Salient features of the proposed method of obtaining are:

- use of larch wood and / or fir.

- carrying out extraction with aliphatic alcohols with the number of carbon atoms 1, 2, 3 or acetone containing not more than 60 wt.% water, or a mixture of these extractants;

- obtaining a biologically active active substance (DW), the claimed composition, previously not used in crop production.

The combination of these essential distinguishing features allows you to get a new biologically active drug based on flavonoids of the above composition. Used aqueous solutions of the listed alcohols or acetone are selective extractants to isolate the claimed active amount of natural compounds based on flavonoids.

The use in the crop of DV based on flavonoids of the claimed composition to increase productivity and reduce the incidence of crops is new.

To justify the criterion of "industrial applicability" of the claimed method, the following specific examples of its implementation.

Example 1. 20 kg of sawdust of Siberian fir wood with a moisture content of 13 wt.%, Bulk density of 0.2 kg / l was placed in a stainless steel extractor, filled with 100 l of isopropyl alcohol containing 10 wt.% Water until the sawdust was completely coated with a solvent. Insisted 1 h, the extract was drained. Sawdust was poured a second time with 70 L of aqueous alcohol, insisted for 1 h, the extract was drained. An additional 70 L of extract was isolated. The extracts were combined, heated in a distillation apparatus, aqueous isopropyl alcohol was distilled off for 4 hours at the boiling temperature of the mixture until the azeotrope was removed. The remainder in the cube consisted of a yellowish aqueous layer and a resinous brown substance. This residue is hereinafter referred to as a “water / DV mixture” (DV is an active substance).

Water was distilled off from the residue, and an anhydrous residue, referred to as “DV”, was obtained in an amount of 1.2 kg in the form of a tan viscous mass.

The analysis of DW, carried out by known methods (4), shows that it is mainly flavonoid dihydroquercetin (3.3 ', 4', 5,7-pentahydroxyflavanone) - 80%, as well as dihydrocampferol - 4%, naringenin - 3 wt. %, other compounds - flavonols and glycosides of flavonoids. Their quantitative content has not been established.

Example 2

20 kg of larch wood sawdust with a moisture content of 18 wt.%, Bulk density 0.25 kg / l was placed in a stainless steel extractor, 100 l of ethyl alcohol containing 10 wt.% Water was poured until the sawdust was completely covered with a solvent. Insisted 1 h, the extract was drained. Sawdust was poured a second time with 70 L of aqueous alcohol, insisted for 1 h, the extract was drained. An additional 70 L of extract was isolated. The extracts were combined, heated in a distillation apparatus, aqueous ethanol was distilled off for 4 h at the boiling temperature of the mixture until the azeotrope was distilled off. The remainder in the cube consisted of a yellowish aqueous layer and a resinous brown substance.

Water was distilled off from the residue, a dry residue was obtained, referred to as "DV", in an amount of 0.6 kg in the form of a light brown viscous mass.

Analysis of DV, performed as described above, showed that DV is a mixture similar in composition to that obtained in Example 1. The content of the main components: dihydroquercetin — 86%, dihydrocampferol — 10%, naringenin — 6 wt.%, Other compounds — flavonols and glycosides of flavonoids.

Example 3. Small chips of Siberian larch 15 kg with a moisture content of 9% were extracted as described in example 1, as an extractant, a mixture of acetone and methyl alcohol in a ratio of 1: 3 by weight containing 60 wt.% Water was used. 0.42 kg of a viscous light brown residue was obtained from the combined extracts with the content of the main components, wt.%: Dihydroquercetin - 86, dihydrocampferol - 4, naringenin - 3, other substances - the rest.

The yield of the target product of DV using fir wood was 5.8-6.2%, while using larch wood, 3.2-3.6%, depending on the time and place of logging.

Preparation of the drug - a standard 10% solution of DV in a mixture of water / emulsifier.

Option 1. 1 kg of DV obtained above, was mixed with 9 kg of a 10-20% solution of emulsifier in water. As the emulsifier used soap, industrial emulsifiers OP-7, OP-10, PO-6 or others. The resulting emulsion is called "standard 10% emulsion DV". The drug is non-toxic (LD50 for rats 5.2 g / kg, oral).

Option 2. From the mixture of water / DW decantation separated the resinous part from the water. By distillation of water from a sample of the water part, the content of DW in water was determined. The resinous and aqueous parts were mixed with the calculated amount of water and an emulsifier and a standard 10% DV emulsion was obtained.

Similarly prepared standard 2% and 5% emulsion DV in a mixture of water / emulsifier.

From the preparation thus prepared — the standard emulsion of DV — a working solution was prepared with which vegetative plants were treated.

Claims (2)

1. A method of obtaining a biologically active preparation for increasing the yield of agricultural plants, including extraction of plant materials with an organic solvent, obtaining an aqueous emulsion of a biologically active amount of natural compounds, characterized in that the larch and / or fir wood is extracted with aliphatic alcohol with the number of carbon atoms 1, 2, 3 or acetone containing not more than 60 wt.% Water, or a mixture of these extractants, and then the extractant is distilled off. 2. The method according to claim 1, characterized in that the preparation is prepared in the form of an aqueous emulsion containing 2-10 wt.% The active substance.