RU2569728C2 - Method of extracting water-soluble plant components - Google Patents

Abstract

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to pharmaceutical industry, in particular, to method of extracting water-soluble plant components. Method includes washing of crushed raw material with ozone-saturated distilled water, portioned charging of mixture of raw material, water and flake ice into homogeniser of rotor-pulsation type, filtration, extraction of biologically active components from vegetable raw material and pre-packaging. Method of extracting water-soluble plant components is realised under certain conditions, ratio of raw material and water, water and flake ice; with specified rotations of rotor-pulsation homogeniser. said method makes it possible to obtain water-soluble plant components with high biological activity.

EFFECT: application of flake ice and step-by-step regulation of rate of rotor-pulsation homogeniser results in synergic effect, making it possible to increase preservation of biologically active substances.

5 cl, 1 dwg, 2 tbl, 4 ex

Description

The invention relates to the field of food, pharmaceutical and cosmetic industries.

State of the art

There are various methods for the production of herbal supplements that are carriers of biologically active substances.

Known methods for producing dry plant biologically active additives based on preliminary extraction of water-soluble components of plants in homogenizers. For these purposes, rotor-pulsation homogenizers are also used [1, 2].

The closest technical solution is described in RF patent No. 2384342 [3].

The invention relates to the field of food and pharmaceutical industry, in particular to a method for producing a therapeutic and prophylactic food supplement from macrophyte algae. According to the method, the crushed dry and / or wet algae is washed with distilled water in the presence of ozone, then the mixture is portioned into a rotary type homogenizer and sodium alginate is introduced, homogenization is carried out when distilled water is supplied under certain conditions.

The disadvantage of this method is the uncontrolled high heating of plant components during their destruction of plants at the first stage of homogenization, which leads to a decrease in the number of biologically active components in the composition of the food additive.

The objective of the present invention is to develop a method to expand the arsenal of high-quality extracts with a high content of biologically active substances.

The technical result of the claimed method is the technology for extracting biologically active water-soluble components from the aerial parts, leaves, fruits, inflorescences, bark and rhizomes of plants, with a high yield of the final product.

SUMMARY OF THE INVENTION

One of the aspects of the invention is a method for extracting water-soluble components of plants, including washing the crushed raw materials with distilled water saturated with ozone, portioning the raw materials into a rotary-pulsation homogenizer, extracting biologically active components from plant materials. According to the invention, flake ice with a temperature of from -8 to -12 ° C is added to the mixture of raw materials and water, which is prepared on distilled water or distilled water saturated with carbon dioxide. Subsequent batch loading of the mixture of raw materials of water and flake ice is carried out when the temperature of the mixture in the range from 20 to 30 ° C. In this case, the preliminary extraction of water-soluble components from plant materials is carried out at rotational-pulsating homogenizer revolutions of 10 to 50% of the maximum revolutions, the final extraction of water-soluble components from the raw materials is carried out at maximum rotational-pulsating homogenizer revolutions and the temperature of the mixture is from 55 to 65 ° C.

List of figures

Figure 1 Timing diagram characterizing the temperature change of the mixture in the process of extracting components, where:

1) an increase in temperature in the volume of the homogenizer without the introduction of flake ice;

2) a change in temperature at the stages of fractional loading of raw materials and flake ice with access to the optimum temperature for the extraction of components.

Description

The method of extracting water-soluble plant components from leaves, fruits, inflorescences, bark and rhizomes with a high yield of biologically active product is based on the unexpected use of flake ice as a component of the working mixture. Another technical solution is associated with a stepwise change in the speed of rotation of a rotary pulsation homogenizer.

In accordance with the proposed method, the extraction of water-soluble plant components involves washing the crushed raw materials with distilled water, which has an electrical conductivity of 1.0-2.0 MΩ and is saturated with ozone in an amount of 0.4-0.8 g per 100 l.

A working mixture is prepared, including vegetable raw materials, chilled water with a temperature of from 0 to + 1 ° C (4-6 ° C) and flake ice with a temperature of from -8 to -12 ° C. The ratio between plant material, water and flake ice is selected from 0.2 / 1.0 / 1.0 to 0.05 / 1.0 / 2.0, depending on the type of plant material. Flake ice is prepared in distilled water or in distilled water saturated with carbon dioxide to a concentration of 8-10 g / l.

To extract biologically active components from plant materials, batch loading of raw materials into a rotary pulsation homogenizer is carried out [1, 2]. Portion loading in the range from 10 to 30% of the total amount of the mixture, which includes raw materials, water, flake ice, is carried out in several stages. The beginning of each stage following the first stage is selected when the temperature of the mixture rises to a value of +15 to 30 ° C. The preferred range is from +18 to 25 ° C. More preferably +19 to 20 ° C.

In this case, the preliminary grinding of raw materials is carried out at rotational-pulsating homogenizer revolutions of 10 to 50% of the maximum engine speed, which is provided by the current frequency variator.

After the preliminary stages of loading are completed, the water-soluble components are finally removed from the raw materials, while the engine speed is increased stepwise or smoothly in 1-5 minutes to the maximum value of the rotational-pulsating homogenizer speed and the temperature of the mixture from 55 to 65 ° C.

The use of a rotor-pulsation-type hydrodynamic installation with a rotor-stator diameter of 350 mm with special processing and hardening with a motor power of 18-25 kW provides the impact of water hammer and cavitation on plant cells, which allows to obtain concentrated solutions and maximize the extraction of water-soluble components.

The use of flake ice allows for cooling in the entire volume of water extraction, which cannot be achieved by cooling the shirt of the homogenizer bowl, especially when extracting water-soluble components from the roots. With an increased homogenizer volume, for example, a volume of 500 liters, it is practically not possible to control the temperature by cooling the jacket of the homogenizer bowl. When using flake ice for cooling, there is practically no need to make water cooling of the homogenizer, which significantly reduces the cost of the manufacturing process of the homogenizer bowl.

Thus, the use of flake ice and stepwise regulation of the rotor-pulsation homogenizer speed leads to a synergistic effect, which allows to sharply increase the preservation of biologically active substances in the product.

At the end of the extraction process, the product is sent for centrifugation without cooling while accelerating the gravity of 4000-5000 g for 30-60 minutes.

The supernatant is collected, and the sediment can be sent for re-extraction. The supernatant contains from 20 to 55% of the plant components extracted by water at a concentration of from 2.0% to 10.8%. The supernatant solution is sent to microfiltration with a pore size of the membrane of 0.22-0.45 microns.

A product containing biologically active components extracted from plant materials is stored in a hermetically sealed container of opaque material at a temperature not exceeding 25 ° C or at low temperatures from -20 to -60 ° C to more effectively maintain the biological activity of water-soluble components.

The liquid product can be packaged in sterile plastic ampoules with a volume of 5 to 50 ml, which may contain a single dose with a reasonable amount of active substances.

The product may be freeze-dried or otherwise.

Figure 1 presents a diagram of temperature changes at the stages of fractional loading of the roots of Eleutherococcus and flake ice with access to the optimal temperature for the extraction of components. Experimental conditions: the volume of the bowl is 100 liters, the ratio of roots and water is 1:10.

The results of water extraction are shown in table 1.

Table 1 Extraction of water-soluble plant components in a rotary-pulsation type plant Type of plant Amount of raw gram Amount of water ml Solids concentration% The amount of recovered substances% Valerian (roots) 1588 7970 3.44 28 Valeriana Wallichii Soap tree (fruits) 1390 6000 12.05 51.79 Sapindus trifoliatus Psoralea 1950 15,000 5.54 41.43 Psoralea corylifolia Turmeric 1880 15,000 5.75 78,2 Curcuma longa Amla Emblica officinalis 1900 12000 9.59 60.5 Henna Lawsonia inermis 1930 13000 4.7 24.35 Eclipta White Eclipta Alba 2000 16000 1.55 9.3 Soap beans Acacia Concina 1920 13000 5.57 34.79 Tinospore hearty Tinospora cordifolia 1990 15,000 4.31 28.1 Chamomile pharmaceutical Matricaria Reculita 2500 16000 3.73 23.8 Ivan Tea Chamerion 1500 15,000 2.43 24.8 Wormwood Artemisia 2000 20000 3.02 28.6 Horsetail Equisetum 2000 15,000 2.42 23.5 Nettle Urtica 2000 20000 4.3 29.4 Saber Comarum 1500 15,000 4.9 31,4 Icelandic moss Cetraria islandica 2000 20000 2,8 22.4

Table 2 presents data on the extraction of water-soluble components of the roots of Rhodiola rosea.

table 2 Plant name Extraction conditions % Concentration Product yield% Rhodiola rosea,
the roots Distilled water,
75 ° C, 3 hours 3.36 21.48 Sludge after centrifugation Distilled water, 75 ° C, 3 hours 1,5 6.0 Rhodiola pink roots Flake ice, СО ₂ , 60 ° С, 3 hours 4.1 26.65 Sludge after centrifugation Flake ice, СО ₂ , 60 ° С, 3 hours 3.66 16.45

The total yield of water-soluble components from the roots of Rhodiola rosea, extracted from a solution that includes distilled water - 27.48%.

In some cases, ice is prepared from distilled water saturated with carbon dioxide in a saturator, which increases the yield of soluble components. When using ice saturated with carbon dioxide, the total yield of water-soluble components from the roots of Rhodiola rosea is 43.1%

Example 1

Dry chamomile pharmacy 2500 g is loaded in portions of 250 grams into a homogenizer with a mixture of flake ice 1 kg and distilled water 600 ml. The final volume of water and ice is 1600 ml. The current frequency is set to 20 Hz, which provides a rotation speed of 30% of the maximum speed of the rotor-pulsation homogenizer. Fractional loading of five portions is carried out within 30 minutes. Temperature at the end of loading + 10 ° C. The frequency in steps of 10 Hz was increased to 50 Hz within 30 minutes. The temperature reached 40 ° C. Homogenization was continued until the temperature rose to 60 ° C.

The product containing biologically active components extracted from plant materials was hot centrifuged on a HERAEUS 600i centrifuge, rotor No. 6694, 4000 rpm, 5000 g, 30 minutes.

After centrifugation, the product is poured and sealed in drinking ampoules with a volume of 5, 10, 15, 20 ml.

Example 2

5000 g of dry crushed motherwort is washed 3 times with water saturated with ozone at a concentration of 10 mg / liter.

The washed motherwort is loaded into a rotary-pulsation-type apparatus in portions of 20% each in a mixture of distilled water and flake ice (temperature -12 ° C) saturated with carbon dioxide to a concentration of 10 g / kg in a water / ice ratio of 1: 1 at an engine speed of 50% from the maximum. The amount of water and ice is 100 kg.

At the loading stages, the temperature did not exceed + 20 ° C. The loading process and homogenization at 20 ° C lasted 90 minutes.

At the end of the batch loading, the engine speed is gradually increased to the maximum value and the homogenization process is continued for at least 90 minutes until the temperature reaches 60 ° C. The homogenate is centrifuged for 30 minutes at 5000 g and the supernatant is filtered through a 0.22 micron membrane with a solids concentration of 3.06%.

The filtrate is Packed in 10 ml in sterile plastic ampoules under aseptic conditions.

Example 3

10,000 g of dry roots of Eleutherococcus are washed 3 times with 50 liters of water saturated with ozone (10 mg / l), dried under a stream of warm air and crushed to a particle size of 1-2 mm.

Crushed and washed roots are loaded into a rotary pulsation-type apparatus in portions of 20% each in a mixture of distilled water and flake ice (temperature -12 ° С) saturated with carbon dioxide to a concentration of 10 g / kg in a ratio of water / ice 1: 1 at engine speed 50% of the maximum. The amount of water and ice is 100 kg.

At the loading stage, the temperature did not exceed + 20 ° C. The loading process and homogenization at 20 ° C continue for 40 minutes.

Slowly increase the engine speed to the maximum value and continue the homogenization process for 90 minutes until the temperature reaches 60 ° C. The homogenate is centrifuged for 30 minutes at 5000 g.

The supernatant is filtered through a 0.22 micron pore membrane. Solids concentration 2.02%

Example 4. Obtaining a drink containing a water-soluble extract of the plant.

100 liters of natural cranberry juice are diluted with distilled water in a ratio of 1: 1, 20 liters of Eleutherococcus extract and 10 kg of liquid grape sugar are added (70% solids), 0.5% potassium sorbate. Mix thoroughly and pour 250 ml into glass bottles.

Industrial application

The invention allows to expand the arsenal of high-quality extracts with a high content of biologically active substances. The use of flake ice allows you to scale the volume of homogenizers and, in some cases, to abandon the external cooling of the homogenizer.

A product containing biologically active components extracted from plant materials in liquid or dry form can be used in traditional fields of application of medicinal plants, for example, in the production of biologically active additives, drinks, and confectionery (sweets, chocolate).

Literature

1. Popov A.M., Kravchenko S.N., Rogalev N.N. DEVICE FOR DISPERSION AND EXTRACTION OF FRUIT-BERRY AND VEGETABLE RAW MATERIALS. Pat. RF №2340383, publ. 12/10/2008.

2. Budrik V.G., Novikov G.S., Kharitonov V.D. PLANT FOR PRODUCING LIQUID-FLOWING MULTICOMPONENT MIXTURES. Pat. RF №2195996, publ. 01/10/2003.

3. Owl VV METHOD FOR PRODUCING A MEDICINAL AND PREVENTIVE ADDITIVE Pat. RF №2384342, publ. 03/20/2010.

Claims (5)

1. A method of extracting water-soluble components from the aerial part, leaves, fruits, inflorescences, bark and rhizomes of plants, including washing the crushed raw materials with distilled water saturated with ozone, portioning the mixture of raw materials and water into a rotary-pulsation homogenizer, filtering, extracting biologically active components from vegetable raw materials and packaging, characterized in that the batch loading is carried out in the range from 10 to 30% of the total ratio of the mixture of raw materials, water and flake ice, while the ratio of raw materials I and water are selected in the range from 0.05 to 0.2, and the ratio of water to flake ice is 1/1 with a temperature of -8 to -12 ° C, which is prepared with distilled water or distilled water saturated with carbon dioxide to a concentration 8-10 g / l, subsequent batch loading of a mixture of raw materials, water and flake ice is carried out when the temperature of the mixture reaches 15 to 30 ° C, where the preliminary extraction of water-soluble components of plant materials is carried out at rotational-pulsating homogenizer revolutions of 10 up to 50% of maximum revolutions, the final extraction of water-soluble components from raw materials is carried out at maximum revolutions of the rotary-pulsating homogenizer and the temperature of the mixture from 55 to 65 ° C. 2. The method according to claim 1, characterized in that the water-soluble components are isolated by centrifugation and filtration. 3. The method according to p. 2 is characterized in that centrifugation is carried out at 5000 g. 4. The method according to p. 1 is characterized in that the filtration is carried out through a membrane with a pore size of 0.22-0.45 microns. 5. The method according to claim 1, characterized in that the packaging is carried out in sterile plastic ampoules with a volume of 5 to 50 ml.

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