CS252992B1 - A method of preparing a water-alcoholic extract of chamomile - Google Patents

Abstract

The present invention relates to a process for the preparation of an aqueous alcoholic extract of chamomile containing active ingredients consisting of a lipophilic and hydrophilic component. The process consists in extracting the chamomile drug after separation of the lipophilic component by distillation with water vapor at a temperature of 20 to 50 ° C for 1 to 8 hours, separating the solid phase and adding 0 to the solution after sedimentation and filtration. 5 to 10 wt. % propylene glycol extract of fresh flower of chamomile and 0.2 to 5 wt. % solubilizer. The extract is used in pharmaceuticals and cosmetics.

Description

The invention relates to a method of preparing a hydroalcoholic extract from the drug chamomile after separating part of the lipophilic component.

The multifaceted healing effect of chamomile is due to the presence of several groups of substances. The pharmacodynamic effect is shown by the lipophilic components of the drug (bisabolol, bisabololoxides, chamazulene, ene-in-dicycloethers) having a predominantly antiphlogistic and slightly antiseptic effect and also hydrophilic components (flavonoids apigenin, luteolin and coumarin derivatives umbelliferone and herniarin) with a spasmolytic effect (Felklová M., Čes. farm. 27, [8], 359 [1978]). The most favorable medicinal effect of the constituents of chamomile shows a complex containing both their lipophilic and hydrophilic parts (O. Isaac: Deutsch. Apoth. Zeit. 114, 7, 225 [1974]).

Many procedures have been developed to obtain active substances from the drug chamomile. For example, a mean heel. file NSR 1296 305, the drug of true chamomile is ground in a ball mill with dexylolsate for 6 hours and the extract is obtained by pressing and centrifuging. Mean heel. of EP 583 365 and DE 2 709 033, the drug of chamomile is extracted using supercritical gases, for example carbon dioxide. Other methods use the organic solvent alone or its combination with water to obtain active substances from the drug true chamomile. file NSR 1 093 951, NSR 2 165 633, NSR 2 249 433, NSR 2 227 292, NSR 2 316 363, NSR 2 548 820, Swiss. heel file 430 947. In the mentioned procedures, the active substances are isolated directly from the undigested chamomile drug. Other procedures use a combination of isolation methods, e.g. under mad. heel of the Hung file. Feljes 14 432, part of the lipophilic component is steam distilled from the drug of chamomile, the aqueous residue is concentrated to a dry matter content of 48% and dissolved in 80% ethanol, the obtained extract is combined with the dichloromethane extract of the fresh drug, which was dissolved in 96% ethanol after concentration, the combined extracts are treated with ethanol to a concentration of 70% ethanol and the dried lipophilic component obtained by steam distillation is added. Another combined procedure according to art. heel file 15 020 after isolation of part of the lipophilic component by precipitation with steam, describes the extraction of residues with water, concentration of the extract to 50% dry matter, filtration and spray drying of the product. The isolated lipophilic component is applied to the dried product, which is combined with sodium bicarbonate, vitamin C and polyvinylpyrrolidone, and the mixture is dried.

The disadvantage of the above-mentioned procedures when using an organic solvent to isolate active substances is the obtaining of a predominantly lipophilic component in the extract and the precipitation of polymeric substances after mixing it with water. In the case of combined procedures, the disadvantage lies in the isolation of only a part of the lipophilic component by distillation with steam (Glasl. H., Wagner H. Deutsch. Apoth. Zeit. 116, 3, 45 [1976]]), and a part remains in the distilled residue of the drug, unused. For example, bisabolol oxide and spiroether are isolated only in a minimal amount during distillation with steam not only for reasons of instability under the given conditions, but also because of its specific physico-chemical properties.The table shows the quantitative GC determination of the components of the essential oil distilled with water vapor at different pH values compared to the extraction of the drug with dichloromethane.

Values in mg/% of drug Bisabolone oxide Bisabolol Spiroether Bisabolol oxide A Bisabolol oxide B Eth. oil (dist. pH 3) 0.9 15.9 footprints 6.0 62.8 Eth. oil (dist, pH 5.5) 0.9 16.9 17.3 7.1 70.3 Eth. oil (dist. pH 7) 1.0 18.5 43.8 7.7 78.1 Eth. oil (dist. pH 10) 1.0 18.5 53.8 8.0 75.4 Dichloromethane 1.1 20.2 358.6 18.8 86.4 Chamazulene Suma (without Gham: zulene) Eth. oil (dist. pH 3] 16.2 101.8 Eth. oil (dist. pH 5.5] 12.4 124.9 Eth. oil (dist. pH 7) 8.6 157.7 Eth. oil (dist. pH 10} 10.0 166.7

485.1

The most common method of isolating essential oil from chamomile is steam distillation of the drug. With this procedure, the active substances are not isolated comprehensively from the quantitative drug. A drug after distillation with steam, which contains flavonoids, coumarin derivatives, choline, mucilaginous substances and part of ^! a drop of essential oil remains unused waste in this processing method.

252932

Utilization of the substance after distillation of chamomile drug with steam solves the process of the stage of the invention so that the drug of true chamomile is stripped of the lipophilic component by distillation with steam, after adjustment to a dry matter content of 10 to 35% by mass, extracted with ethanol at a temperature of 10 to 50 °C for 1 to 8 hours, the solid phase is separated and to the solution after sedimentation and filtration, 0.5 to 10% by weight of a propylene glycol extract prepared by extracting fresh flowers of the primrose with propylene glycol in a ratio of 1:4 to 1:5, and then 0.2 to 5% by mass is added. solubilizer, type of esters, fatty acids with polyoxyethylene glycerins, polyoxyethylene sorbitans, or polyoxyethylenes and polyethylene glycols. The drug after steam distillation contains 10 to 20% by mass. of dry matter and by centrifuging part of the aqueous extract, the dry matter content is adjusted to 20 to 35% by mass. The drug prepared in this way, which contains mainly flavonoids, coumarin derivatives, mucilaginous substances, choline, sugars and non-isolated essential oil in the steam distillation process, is extracted with such an amount of ethanol that its final concentration in the extract is 35 to 60% by mass. The added propylene glycol extract mainly contains essential oil components dissolved in a mixture of propylene glycol and water 4:1. The addition of this propylene glycol extract significantly improves the organoleptic properties of the prepared water-alcoholic extract. The prepared water-alkaline extract with the addition of propylene glycol extract of fresh chamomile flowers is stabilized by the addition of a solubilizer of the fatty acid ester type with polyoxyethylene glycerins or with polyoxyethylene sorbitans or polyoxyethylenes. The addition of a solubilizer causes the extract to mix with water in any ratio without forming turbidity. The use of this type of solubilizer is not known in this process. The use of this type of solubilizer in direct drug extraction and in the preparation of essential oil solutions is known. The extract prepared by the process according to the invention has very good organoleptic properties, it mixes with water without the formation of turbidity and is characterized by higher stability. The procedure of the stage of the invention prepares an extract containing a complex of active substances of a lipophilic and hydrophilic nature, and a higher evaluation of the chamomile drug is achieved.

In the following, the object of the invention is clarified by three examples without limiting it.

Example 1 kg of dried chamomile (Matricaria chamomilla) drug is steam distilled for 5 hours. The boiled mass is then centrifuged. To 20 kg of centrifuged mass with a content of 23.6% dry matter, 13 kg of ethanol is added in parts while stirring. The whole mixture is stirred for 5 hours and then centrifuged and filtered. 12 kg of water-alcoholic extract with a dry matter content of 3.9% is obtained, to which 0.06 kg of propylene glycol extract from a fresh flower is added, and the extract is stabilized with 60 g of stabilizer.

Example 2 kg of boiled mass, obtained by distillation of a dry drug of true chamomile (Matricaria chamomilla], with a dry matter content of 26.9%, is mixed for 3 hours with 3.65 kg of ethanol. By separating the solid phase, 3.93 kg of aqueous alcohol extract is prepared with a dry matter content of 4.49 °/o and a density of 924 kg . m~ ³ , to which is added 0.2 kg of propylene glycol extract from the fresh flower.The extract is stabilized by the addition of 19 g of solubilizer (Arlatone 980).

Example 3 kg mass of true chamomile with a dry matter content of 24% by mass, obtained by distillation of fresh drug of true chamomile (Matricaria chamomilla) with steam and centrifugation of the aqueous phase. mixed for 8 hours with 43.3 kilograms of ethanol. 52 kg of water-alcoholic extract with a density of 928 kg is prepared by centrifugation and subsequent filtration. m~ ³ and with a dry matter content of 2.1%. 5.2 kg of propylene glycol extract of fresh chamomile flowers is added to the extract. The extract is stabilized by adding 1 kg of solubilizer (Arlatone 980).

Claims (5)

SUBJECT 1. A process for the preparation of a water-alcoholic extract of true camomile, characterized in that the camomile drug is extracted with ethanol at 20 DEG-50 DEG C. for 1-8 hours after separation of a portion of the lipophilic component by steam distillation, the solid phase is separated. 0.5 to 10 wt. % propylene glycol extract of fresh camomile flower and 0.2 to 5 wt. solubilizer. 2. A process for the preparation of a water-alcoholic extract of the true lumen according to claim 1, characterized in that the dry matter content of the camomile drug used for the extraction is adjusted to 10 to 35% by weight. VYNALEZU 3. A process for preparing a water-alcoholic extract of camomile, wherein the final concentration of ethanol in the extract is 40 to 60% by weight. 4. A process for preparing a water-alcoholic extract of camomile according to claim 1, wherein the propylene glycol extract is prepared by extracting the flower with propylene glycol in a ratio of 1: 4 to 1: 5. 5. A process for the preparation of a water-alcoholic extract of camomile according to claim 1, characterized in that fatty acid esters of polyoxyethylene glycerines or polyoxyethylene sorbitans or polyoxyethylenes are used as solubilizers. Severography, n, Mr. Plant 7, Most Price 2,40 Kčs