UA123294C2 - METHOD OF PREPARING DRY EXTRACT OF PELARGONIUM PELARGONIUM SIDOIDES AND / OR PELARGONIUM RENIFORME - Google Patents

Abstract

The invention relates to a technological method of obtaining a dry extract of Pelargonium sidoides and / or Pelargonium reniforme, which meets the pharmacopoeial characteristics.

Description

The claimed invention relates to a technological method of obtaining a dry extract from

ReIagdopisht 5idoide5 and/or ReIagdopisht hepitogte in the pharmaceutical industry.

It is known that preparations obtained from Pelargonium species - Rheiagdopisht 5idoide5 and/or Rheiagdopisht hepiugte, which are indigenous species to southern Africa, are traditionally used in this region for the treatment of respiratory disorders and symptoms from the gastrointestinal system.

Liquid extract of the roots of Reiagdopisht 5idoidez and Reiagdopisht hepi'toppe (OEK 1:8-10), extractant ethyl alcohol 11 95 (wt.-) and dry extract of the roots of Reiagdopisth v5idoide5 and Reiagdopist hepitotte (OEV 4-25-1), extractant ethyl alcohol 11 95 (weight) are considered well-studied and described by EMA monographs: "Sottipynu Neba! topodgaryi op Reiiagdopiit vidoide5 OS apa/og Reiiagdopisht hepiopte Siy., gadih" dated March 21, 2011,

Az5ezz5tepi gerogi op ReiIagdopisht 5zidoide5 OS apa/og Reiagdopisht gep'ogte Sygi., gadih of March 21, 2011,

А55еззтепи героп оп Реягдопишт видоидез ОС apa/ог Реягдаопишт гепиопте Sipy., gadih from November 2012, reviewed on June 5, 2018.

Currently, herbal preparations protected by patents use an extract (OEB 1: 8-10) (ER5F 7630) of aqueous ethanol (11 95 m/m) of the root of R. zidoide5. Tinctures or decoctions are used in folk medicine. In Germany, SteCaioaro was registered as a medicine in 2005. Outside the territory of 20 Europe, especially in North America and Mexico, various liquid and solid preparations containing pelargonium root are available as dietary supplements. In turn, in South Africa and its neighboring countries, liquid and solid monopreparations and combined means, which include

R. zidoide 5. In Ukraine, Russia and Latvia, the drug is distributed under the name "Stekaiog".

It has been proven in clinical trials that various extracts and active substances of the root of R. 5idoide5 have antibacterial, antiviral and immunomodulating effects. Antibacterial and antiviral effects are mainly associated with gallic acid and other compounds of the phenolic group, and immunomodulatory activity can be provided by the combined action of phenolic acid derivatives and coumarins (especially umcaline). In addition, pelargonium root extract ERbF 7630 affects the activity of the mucociliary system. Extract of R. 5idoide5

ЗОЕР5Ф7б630 reduces the symptoms of acute bronchitis and accelerates recovery from acute bronchitis.

Methods of obtaining and using plant thick and/or dry extracts are known from the state of the art. Yes, in patent ER 0 589921 (UMO1992021357) SOMSEMTVATEO AMO/V OVU RI AMT

EHTKASTZ) disclosed a method of obtaining plant thick and/or dry extracts with the same or approximately the same spectrum of the active substance of the corresponding liquid extract.

Patent EP 1037647 ((M/01999032130) MEBISIMAI RGAMT OKU EHTKASTZ5) discloses a method of obtaining plant extracts from Rakhziyoga, Adpyv5 sage5, Stagaeda5, SipoKo, extract of stinging nettle, valerian, root or rhizome of Sitisitsda and/or Supaga for oral use of the medicinal product. The extract phase is nonvolatile, alcohol miscible, water soluble, or water miscible solid. And at room temperature, in a microdispersed form and/or in the form of a semi-solid or solid solution, it additionally contains other auxiliary substances and/or additives. This method is characterized by the release of plant ingredients, which is determined by the degree and speed.

The closest analogue to the claimed development is the method of obtaining a dry extract from

REGAXOMIUM 5I0OIRE5 and REGAXOMISHM KEMIROKM, disclosed in the patent EP2134369 (MmO2008125239) OVU EHTVASTZ OB REGAVSOMIUM 5ISOIUEZ AMO REGAVSOMISHM

KEMIROKME). According to this invention, an extract with improved solubility is obtained, using aqueous monoatomic alcohol solutions. According to the method, adding a solid carrier from the group of monosaccharides/oligosaccharides/polysaccharides/sugar alcohols in a mass ratio of the carrier to the dry residue from 1:4 to 9:11. In the given examples of the implementation of the invention, at the stage of maceration, ethyl alcohol (3595 wt.) is mixed with crushed roots of REGAXOMISHM

ZISOIIOE5 in a ratio of 2:11 and kept for 20 hours. at room temperature. At the stage of extraction, the percolation method is used with a solution of ethyl alcohol (6 95 wt.). The carrier is dissolved in the resulting extract solution. They are dried by the vacuum drying method at 50 "C in a vacuum of up to 18 mbar (1800 Pa). The disadvantage of this method can be considered a long-term continuous process of infusing plant raw materials in solvents, with the aim of giving the solvent its properties and thus enriching it, there is no size standardization grinding of raw materials - the roots of REGAXOMIOM 5ISOIIIIOE5, obtaining an extract that does not meet the requirements of the pharmacopoeia for microbiology and purity.

During independent pharmaceutical development, a technology 60 was developed for obtaining a dry extract from the roots of pelargonium for pharmaceutical use.

The basis of the proposed invention is the task of developing a method of obtaining a dry extract of pelargonium Reiagdopisht 5idoide5/or ReiiIagdopisht hepitogte by stages, in which - the maceration stage takes place in a shorter period of time, compared to analogues; the extraction stage allows extracting biologically active substances with maximum release, obtaining a standardized final product that meets pharmacopoeial requirements; optimize the ratio of solid carrier to extract.

The task of developing a method of obtaining a dry extract from ReiIagdopisht zidoidee and/or ReiIagdopisht hepiogte of pharmacopoeial quality is solved by the following technological stages.

Pelargonium root, used to obtain a dry extract, is crushed into particles no larger than 1 mm in size. After grinding, the plant material is sieved to remove dust. Plant raw materials (crushed pelargonium roots), ethanol 9695 and water are weighed on a scale. The prepared raw materials are transferred to the stage of preparation of dry pelargonium extract. Preparation of a water-alcohol solution (ethyl alcohol (119% by weight) is used as an extractant.

The extraction of plant raw materials is carried out in two stages: 1) maceration (the ratio of the carrier and crushed roots of ReiIagdopisht 5idoide5 in a ratio of 2:1 for 1.5-2 hours at a temperature of 70:24 "С; 2) obtaining a dry extract of pharmacopoeial quality using the stages of maceration and extraction are carried out at a temperature of 70 "C with constant stirring in one reactor for 3-4 hours. Extraction with ethanol 1195 is carried out using the countercurrent method at the given parameters of the technological process, the set time period. The extraction ends when the release of the active substance is no longer observed or it is negligible.

Centrifugation and filtration of the resulting solution. The liquid extract from the extracted plant material is obtained by pressing the extracted plant material in a conical screw press to obtain meal. The obtained liquid extract is successively filtered on a filter first with a pore diameter of 80 μm, and then with a pore diameter of 10-30 μm. The concentration of the solution is carried out at a temperature not higher than 50 "C and a pressure of 20 mm Hg to a content of 20-25 95 dry residue. Thermal sterilization of the concentrate is carried out at a temperature of 1204 "6.

Adding a solid carrier in a mass ratio from 1:5 to 1:3.5 (17.5 95 to 22.0 o) (m/m). Maltodextrin is used as a carrier. Maltodextrin is used as the main component to stabilize the product. Various options for obtaining the final product with the addition of maltodextrin have been experimentally developed: after the evaporation and drying stage, or before and after the evaporation and drying stage. Next, the finished extract mixture is dried by the deodorization method (2eoagayop).

The deodorization method allows you to obtain a dry extract with maltodextrin, which retains its activity, without a preservative, has excellent solubility and is characterized as a high-quality product.

The comparative technology for obtaining a dry extract with REGAXOMIUM 5ISOIIIOEZ5 according to the analog method (patent EP2134369) and the proposed method is shown in table 1.

Table 1 pharmaceutical quality (v/v) of the solution. Maltodextrin production (polysaccharides

Addition of a solid carrier from Group y and mass ratio nu | The concentration of monosaccharides/oligosaccharides/polysaccharides/sugars and alcohols in the mass ratio of the carrier and dry residue from (options - after evaporation and drying, 1:4 to 9.1 or in 2 stages - before and after evaporation and

DRYING). dry extract. obtaining a dry extract.

According to point 1, water-methyl alcohol/water-ethyl alcohol/water 1-propanol/water 2-propanol/water mixtures are used. and food products.

A comparison of examples of the production of extracts is given in Table 2.

Table 2

Ethyl alcohol (35 55 wt.) is mixed with Ethyl alcohol (11 95 wt.) is mixed with crushed roots of REGAESOM and I 8IROIOEZ (no rationing with crushed roots of REGAXOM

Maceration of grinding sizes) in ZISOIIUEZ (particle size no more than 1 ratio 2-1 and kept mm) in a ratio of 2:1 and kept for 20 hours. at room temperature for 1.5 hours. at and I temperature 70534 76. temperature.

The second part of the alcohol solution is added to the obtained solution with a solution of ethyl alcohol (6 9% by weight) | extraction in one reactor at a temperature of 70534 "C for 3-4 hours.

Pressed raw materials./ HER 77717171 11111111 |Centrifugation./:.:/:/SS:(UDN/N-OYA

The concentration of the solution at a temperature not higher than 50 "C and a pressure of 20

Concentration of mm Hg. Art. to the content of 20-25 95 dry residue. . Thermal sterilization of concentrates of bone marrow in the obtained solution of the extract In the obtained solution

The introduction of the carrier dissolves the carrier of the sterilized extract concentrate and dissolves maltodextrin

They are dried by the vacuum method - o.

Drying drying at 50 "Su vacuum up to 18 Drying of the finished mixture by the method of mbar (1800Pa8) ceodoratsi!

The method by which the obtained solution of pelargonium extract Reiagdopishcht 5idoiides5/or Reiagdopijt hepigte has the following advantages: during countercurrent extraction (dynamic extraction) - the extraction time is significantly reduced; the centrifugation process allows to increase the output of biologically active substances; filtration and thermal sterilization - significantly reduces the microbiological load; drying by the method of deodorization with the addition of maltodextrin at different stages (options - after evaporation and drying, or in 2 stages - before and after evaporation and drying), which allows you to obtain an extract with a lower moisture content (increase the shelf life) and raw materials with homogeneous the size of the granules. The results are given in the examples of implementation of the invention.

Experimental studies have developed three series (10717; 20717; 30717) according to the patent analog EP2134369 (patent of the originator) and three series according to the proposed technology (40717; 50717; 60717). The obtained results are shown in Table 3.

Table C

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Description brown Corresponds | Corresponds to | Corresponds to | Corresponds to | Corresponds to | The powder is suitable

Umkalin's mouth

Loss in mass of I

Shshshhn (KI knew how to dry "

Residual

QUANTITIES. se nin pH of solvents "

Ethanol

Acceptability criterion: total number of microorganisms (TAMS) 102

CMU/; total number of molds 83 87 10

Microbiological)| mushrooms (TUMS) purity 102 CFU/g.

Aeneas nickname | ov |in ioienine zrmeekionneniya

EzePepspia soy | Corresponds to | Answers | Answers | Corresponds to | Corresponds to | Corresponds to 1 year.

To" | pen | ep carried your penenisnnenia

ZaItopepya in Answers | Corresponds to | Corresponds to | Corresponds to | Corresponds to | Corresponds to 25 g.

Gram negative! bacteria tolerant to 79 75 73 16 11 14 bile 102 CFU/g

Tannin content From 10.0 to 95

Examples of preparation of dry extract

Example 1

Add 100 kg of ethyl alcohol (10 95 m/m) to 10 kg of pre-prepared raw materials of pelargonium roots, turn on the mixer and, while stirring, heat the mixture to a temperature of 65 "C. Turn off the mixer and keep the mixture at a temperature of 70 "C. Extraction is carried out for 4 hours. Centrifuge the resulting solution from the remains of pelargonium roots.

The resulting solution is concentrated at a temperature not higher than 50 "C and a pressure of 20 mm Hg to a moisture content of 20-25 95. Microbiological stabilization of the obtained concentrate is carried out by short-term heating to 121-244 "C. Dissolve a portion of maltodextrin (amount of maltodextrin 15.0 95 (m/m)) and dry the resulting mixture by the ceodorization method.

Example 2

Add 100 kg of ethyl alcohol (10 95 m/m) to 10 kg of pre-prepared raw materials of pelargonium roots, turn on the stirrer and, while stirring, heat the mixture to a temperature of 7076. Turn off the stirrer and keep the mixture at a temperature of 70 "C. Extraction is carried out for 5 hours. Centrifuge the resulting solution from the remains of pelargonium roots.

The obtained solution is concentrated at a temperature not higher than 50 "C and a pressure of 20 mm Hg to a moisture content of 20-25 95. Microbiological stabilization of the obtained concentrate is carried out by short-term heating to 121-244 "C. Dissolve 50 95 measurements of maltodextrin and dry the resulting mixture by the method of ceodorization. The second part of 50 95 maltodextrin is added to the dried mass. The total amount of maltodextrin is 17.5,905 (m/m).

Example C

Add 100 kg of ethyl alcohol (10 95 m/m) to 10 kg of pre-prepared raw materials of pelargonium roots, turn on the stirrer and, while stirring, heat the mixture to a temperature of 7576. Turn off the stirrer and keep the mixture at a temperature of 70 "C. Extraction is carried out for two hours. Centrifuge the resulting solution from the remains of pelargonium roots.

The resulting solution is concentrated at a temperature not higher than 50 "C and a pressure of 20 mm Hg to a moisture content of 20-25 95. Microbiological stabilization of the obtained concentrate is carried out by short-term heating to 121-244 "C. Dissolve a portion of maltodextrin and dry the resulting mixture by the method of deodorization. Dissolve 30,956 measurements of maltodextrin and dry the resulting mixture by the ceodorization method. The second part of 70 95 maltodextrin is added to the dried mass. The total amount of maltodextrin 19.0 9o (m/m).

The claimed invention is a method of obtaining a dry extract from ReIagdopisht 5idoide5 and/or ReIagdopisht hepi'iopt of pharmacopoeial quality, which is characterized by the following technological stages: a) preparation of a water-alcohol solution. Ethyl alcohol (11 95 wt.) is used as an extractant; b) carrying out maceration (the ratio of the carrier and crushed roots of Reiagdopisht 5idoide5 in a ratio of 2:1, for 1.5-2 hours at a temperature of 7024 "С; c) adding the second part of the extractant and carrying out continuous countercurrent extraction at a temperature of 70:24 "С within 3-4 hours; d) centrifugation and filtration of the obtained solution; e) adding a solid carrier (maltodextrin is used as a carrier) in a mass ratio from 1:5 to 1:3.5 (17.5 to 22.0 95) (m/m) with options: after evaporation and drying, or in 2 stages - before and after evaporation and drying; g) evaporation at a temperature not higher than 50 "C and a pressure of 20 mm Hg to a dry residue content of 20-25 95, g) carrying out thermal sterilization at a temperature of 120 "C with a flow rate of 300 l/h; h) drying of the thick extract by the method of seodoration with the addition of maltodextrin.

Claims (1)

FORMULA OF THE INVENTION З The method of obtaining a dry extract from RheiYagdopisht bvidoidee5 and/or RheiYagdopisht hepiogte of pharmacopoeial quality, which is characterized by the following technological stages: a) preparation of a water-alcohol solution (ethyl alcohol (11 95 wt.) is used as an extractant); b) carrying out maceration (the ratio of the carrier and crushed roots of Reiagdopisht 5idoiide5 - 271, for 1.5-2 hours at a temperature of 70-24 C; c) adding the second part of the extractant and carrying out continuous countercurrent extraction at a temperature of 70:24 "C for 3-4 hours; e) centrifugation and filtration of the resulting solution; F) addition of a solid carrier (maltodextrin is used as a carrier) in a mass ratio from 1:5 to 1:3.5 (17.5 to 22.0 95) (m/m) with options: after evaporation and drying or in 2 stages - before and after evaporation and drying; h) evaporation at a temperature not higher than 50 "C and a pressure of 20 mm Hg to a dry residue content of 20-25 9, i) carrying out thermal sterilization at a temperature of 120 "C with a flow rate of 300 l/h; k) drying of the thick extract by the ceodorization method.