Method of obtaining aqueous propyleneglycol extracts of plant material with high resistance to microbiological pollution

FIELD: chemistry.

SUBSTANCE: invention relates to household chemistry, medicine, cosmetic-fragrance industry. Material is extracted using aqueous propyleneglycol extracting agent in a rotor-pulse apparatus without presoaking in continuous circulation mode with ratio of plant material to extraction agent ranging from 1:10 to 1:20 and rotor speed of 3600 to 4400 rpm for 5 to 15 minutes at 25 to 55°C with subsequent filtering off the solid plant part. 1,2-propyleneglycol with water content ranging from 0.1 to 95 wt % is used.

EFFECT: invention allows for cutting on extraction time and obtaining extract with high content of flavonoids (by 20 to 40%) and high resistance to microbiological pollution.

2 cl, 3 tbl, 20 ex

 

The invention relates to methods of processing of vegetable raw materials, specifically to methods of making aqueous propylene glycol extracts - essential natural components of household chemistry, medicine, cosmetics and perfume industry. Common methods of extraction of hydrophilic bioactive components from different parts of plants are water-alcohol extraction (use) and supercritical carbon dioxide extraction (CO2-extracts). In recent years, technologists increasingly less willing to use household chemicals and perfumery-cosmetic compositions containing alcohol extracts. Several reasons for this. First, alcohol-based extracts belong to the class of flammable liquids and require special conditions of transportation, storage and use. Secondly, a well-known problem of alcohol-containing substances is their dissecting the action in cosmetics and hygiene detergents, especially in formulations containing perlamutrovymi and infill components [Myupdates. Cosmetics and hygiene detergents. M: "Chemistry", 1990]. Thirdly, since 2001, after the introduction in Russia of excise duties on alcohol-containing solutions, including aqueous-alcoholic extracts, production in Russia considerably what about the rose. Alternative alcohol extracts to create modern products, household chemicals and cosmetics can really serve expensive supercritical carbon dioxide extracts obtained by extraction with carbon dioxide at operating pressure of 250 bar and a temperature of 50°C., and propylene glycol extracts of plant materials. Propylene glycol extracts have been preferred for the reason that when the relative cheapness of their composition closer to CO2-extracts and does not lead to a radical change in the organoleptic properties of products of famous lines, and the 1,2-propylene glycol is an effective skin softener and has the ability to enhance the effectiveness of preservatives finished products [voitsekhovskaya A.L., Wolfenzon I.I. Cosmetics today. M.: Chemistry, - 1991. - 150 S.].

It is known that the relevance of the extracts is determined by two factors: biological value and microbiological purity. Microbiological purity extracts of plant materials must meet the sanitary requirements of SanPiN 1.2.681-97; MUK 4.2.801-99.

The biological value of extracts of plant materials determined by the quantitative content of biologically active substances extracted from plant material, in particular flavonoids. The most widely used methods is zlecenia biologically active substances from plant material are: maceration (infusion), remunerate (repeated insistence), percolation, repurchase, continuous extraction, the circulation [of the State Pharmacopoeia of the USSR, 11th edition, issue 2, Moscow, Medicine, 1990, p.148, Ponomarev E Extraction of medicinal raw material. M.: Medicine, 1976. - 400 C.]. All these methods have significant disadvantages: high energy consumption, low percentage of extraction of useful substances, the need to use high temperatures, which leads to partial destruction of natural compounds, the duration of the process (at least 24 hours), resulting in reduction of yield of recoverable natural compounds. For the intensification of the extraction process in recent years, the use of various electrophysical techniques and methods.

Thus, a method of obtaining an aqueous extract of propolis method of its electrochemical dissolution. Propolis pre-cleaned from mechanical impurities, crushed, pour water and extracted by passing an electric current through the water until the extract pH 7 [EN 2090089, IPC 6 A23L 1/076, A61K 35/64, 20.09.1997,].

Known method of preparing an aqueous extract of the plant, including crushing, processing water, Department of residues of plant parts and filtering the resulting solution, characterized in that the treatment is carried out in the cell with separated IU the patterned cathode and anode space, filled with water, and the crushed plant is placed in the cathode space [EN 2146938, IPC 7 A61K 35/78, B01D 11/02, 27.03.2000,].

A method of obtaining water extracts of plant materials impact on the extraction of the mass of the microwave energy [EN 2237706, 04.11.2002]. For implementing the method using microwave heater with a capacity of 5-6 kW. The effectiveness of the method is achieved in that at 1 stage raw material is saturated with water, affecting the electric current capacity 9-20 kHz in 1-3 min 2 phase extraction mass effect microwave energy heating the liquid to 55°C, 3 stage, the mixture is cooled to 25°C and repeat the cycles repeatedly within 2-4 hours. When carrying out the extraction in this way is stored biological value, flavor and aromatic properties of the product remain unchanged all biologically active substances, the degree of extraction of useful substances is increased by 20-25%.

The main disadvantage of the above methods is the length of the process and significant energy.

Also known is a method of obtaining water-soluble extract from plant material using ultrasonic extraction, characterized in that the grinding and extraction is carried out in the frequency range 22±1,65 kHz in a single reactor [EN 2005124561, B01D 11/02, 02.08.2005] subsequent about the division of liquid extract from ballast substances by centrifugation. Grinding of raw materials is performed with the intensity ultrasound from 4 to 10 W/cm2. Grinding, extraction and drying of the extract is carried out at a temperature of 50°C. the Disadvantage of this method is the multi-stage (stages 6-7) and processing time (several hours).

A common shortcoming of all aqueous extracts obtained by different methods (in addition to water-alcohol), is the rapid loss of microbiological purity. All aqueous extracts, including propylene glycol, obtained any of the above methods require additional preservatives that protect the product from microbial spoilage. For these purposes, are widely used parabens, benzoic acid and salicylic acid; aliphatic alcohols (benzyl alcohol, Phenoxyethanol, ethanol); boric acid and its salts, paraform, antibiotics, triclosan, Katon [Myupdates. Cosmetics and hygiene detergents. M.: Chemistry, 1990; Tsakanov, Larikov. To the question of the protection of plant extracts used in cosmetic industry, from microbiological contamination, http://www.kamelia.ru/science/articles-4/html.

A method of obtaining propylene glycol extracts of plant materials using small industrial percolation [Apacities. Propylene glycol as the extractant for separation cosmetics / products the definition of biologically active substances from natural sources. /SOFW-J/ Russian version, 2002, No. 3, P.56-58. R j chem. 02.20-R - prototype]. As extractant used is 1,2-propylene glycol.

The method consists in the following. Modeling of countercurrent perform sequential pumping the infusion of the first percolator the next and so on. Pre-dried and powdered plant material is loaded into a cylindrical mesh or cloth bags in percolator 1, 2, 3, equipped with a thermometer, a steam jacket and a hinged bottom. The extractant flows into percolator 1, infused for a few hours at the desired temperature (usually 24 hours at 20-30°C). Then the infusion is pumped into percolator 2, the process is repeated. In percolator 1 enters a new portion of the extractant and so the Cycle is completed cleaning and packaging extract, discharging the waste of raw materials and regeneration of the extractant.

The main disadvantages of this method-prototype:

- multi-stage (not less than 10 stages),

- the duration of the extraction process (more than 72 hours),

- not enough high yield of biologically active components of flavonoids (not to exceed 65%),

- the need to use expensive preservatives (triclosan or Cato) to ensure the microbiological purity of the extracts, which leads to higher production.

The objective of the invention n is a new way for slurry propylene glycol extracts of plant materials, ensuring the preservation of microbiological purity of the extracts during the warranty period of storage (up to 12 months) and an increase in the yield of extracted substances in the reduction of time in the process.

The technical result is to simplify and improve the efficiency of the method of extraction by reducing the number of stages of extraction (2.5 times), reducing the time of extraction (200 times) and enhance the yield of flavonoids by 20-40%.

The technical result is achieved by the claimed method for slurry propylene glycol extracts of plant materials.

We propose a method of obtaining an aqueous propylene glycol extracts of plant materials, which as extractant use of 1,2-propylene glycol with a water content of from 0.1 to 95 wt.%, while the extraction process is carried out in a rotary pulsation apparatus when the mass ratio of vegetable raw materials - extractant from 1:10 to 1:20 for 5-15 minutes depending on the feedstock at a temperature of 25-55°C at the optimum speed of rotation of the rotor 3600-4400 rpm, continuous circulation without pre-soaking.

For the extraction of used rotary pulsation apparatus RPA 1111.410.00.00 produced by OJSC "transmission an aircraft engine with the engine power of 2 kW. Declare the parameters of the process extrag the simulation: the mass ratio of vegetable raw materials the extractant from 1:10 to 1:20, the time of extraction from 5 to 15 min, the process temperature in the range of 25-55°C, rotor speed from 3600 to 4400 rpm are the best.

Carrying out the extraction at a ratio of vegetable raw materials - extractant less than 1:10 is not technological, as reaction mass is difficult to mix, the ratio is about 1:20 is not advisable, because a large breeding leads to a quantitative decrease in the content of extractable substances.

The process of extraction over time less than 5 min leads to the reduction of the yield of extracted substances, conducting extraction more than 15 minutes is not economically feasible because it does not contribute to the improvement of the qualitative characteristics of the obtained extracts.

The selected temperature settings are optimal, since during the process below 25°C output low extractables, increasing the process temperature above 55°C also leads to reduction of the yield of flavonoids is associated with their destruction at temperatures above 55°C.

The advantages of the proposed method:

- simplification of the method of producing extracts, reducing the number of stages in 2.5 times,

- reduction of time of extraction is not less than 200 times (from 72 hours up to 15 minutes)

- increasing the yield of biologically active components (flavonoids) by 20-40%

- otsutstvie necessary, the use of preservatives, since carrying out the extraction in a rotary pulsation apparatus ensures the preservation of microbiological purity of the extracts in a long time.

Testing the claimed process was carried out on different types of vegetable raw materials with different contents of flavonoids, such as grass Polygonum pepper, flowers tansy, Echinacea, chamomile.

The effectiveness of the proposed method is confirmed by the following examples:

Example 1. In the reaction capacity load of 0.15 kg pre-dried and powdered herb Polygonum pepper, add 1.5 kg vodnospirtovogo extractant containing about 99.9 wt.% 1,2-propylene glycol and 0.1 wt.% water. The extraction is carried out at a rotor speed of 3600 rpm continuous circulation without pre-soaking of raw materials for 3 min at 25°Poluchennuyu mass was filtered and the extract obtained will be analyzed by the standard quality indicators, the content of flavonoids and microbiological purity. Indicators of the quality of the obtained extract defined by the standards and procedures specified in THE 9154-010-02700055-2002 with changes in 1.2, is shown in table 1. The content of flavonoids are shown in table 2. To determine the content of flavonoids used differential spectrophotometric method [Bratko LI Quantitative analysis of pharmaceutical preparation is tov vegetable origin. - M.: Nauka, 1985. - P.75]. Determination of microbiological purity of the obtained extract was performed in accordance with ANGUISH 4.2.801-99. Data on microbiological purity of the obtained extract is given in table 3.

Example 2. Analogously to example 1, the extraction is carried out flowers tansy.

Example 3. Analogously to example 1, the extraction is carried out Echinacea.

Example 4. Analogously to example 1, the extraction is carried out chamomile.

Example 5. Analogously to example 1, the extraction is carried out herb Polygonum pepper. Extractant: 80 wt.% 1,2-propylene glycol and 20 wt.% water; the ratio of plant material : solvent = 1:20. The time of extraction 5 minutes the temperature of the extraction 30°C. the rotor Speed 4000 rpm Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 6. Similarly to example 5, the extraction is carried out flowers tansy. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 7. Similarly to example 5, the extraction is carried out Echinacea. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 8. Similarly to example 5, the extraction is carried out chamomile. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 9. Analogously to example 1, the extraction is carried out herb Polygonum pepper. Extractant: 50 wt.% 1,-propylene glycol and 50 wt.% water; the ratio of plant material : solvent = 1:20. The time of extraction 10 minutes the temperature of the extraction 40°C. the rotor Speed 4400 rpm Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 10. Analogously to example 9 the extraction is carried out flowers tansy. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 11. Analogously to example 9 the extraction is carried out Echinacea. The rotor speed 4400 rpm Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 12. Analogously to example 9 the extraction is carried out chamomile. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 13. Analogously to example 1, the extraction is carried out herb Polygonum pepper. Extractant: 5 wt.% 1,2-propylene glycol and 95 wt.% water; the ratio of plant material : solvent = 1:20. The time of extraction 15 minutes the temperature of the extraction 45°C. the rotor Speed 4400 rpm Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 14. Analogously to example 13 the extraction is carried out flowers tansy. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 15. Analogously to example 13 the extraction is carried out Echinacea. Quantitative characteristics the specifications specifications of the obtained extract is given in tables 1, 2, 3.

Example 16. Analogously to example 13 the extraction is carried out chamomile. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 17. Analogously to example 1, the extraction is carried out herb Polygonum pepper. Extractant: 5 wt.% 1,2-propylene glycol and 95 wt.% water; the ratio of plant material : solvent = 1:20. The time of extraction 20 minutes the temperature of the extraction 55°C. the rotor Speed 4400 rpm Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 18. Analogously to example 17 the extraction is carried out flowers tansy. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 19. Analogously to example 17 the extraction is carried out Echinacea. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

Example 20. Analogously to example 17 the extraction is carried out chamomile. Quantitative characteristics of the obtained extract is given in tables 1, 2, 3.

The results presented in table 1 show that on organoleptic and physico-chemical indicators of extracts of plant materials, obtained by the claimed method, meet the requirements of the existing regulatory documents: THE 9154-010-02700055-2002 with changes 1.2. THE 9154-014-12967730-2006.

The results in table 2 indicate that the implemented method for slurry propylene glycol extracts of plant materials provides obtaining the target extracts with a high content of flavonoids (20-40%) compared to the prototype.

From the data presented in table 3, it is seen that the inventive method of obtaining provides aqueous propylene glycol extracts increased resistance to microbiological contamination in a long time.

Thus, the inventive method for slurry propylene glycol extracts of plant materials has several advantages:

1. Provides obtaining extracts with a high content of flavonoids (20-40%).

2. Provides obtaining extracts with high resistance to microbiological contamination (up to 12 months from date of manufacture) with preservation of the organoleptic and physico-chemical quality indicators corresponding to the current regulatory documents.

3. You can simplify the method of obtaining and reducing the number of steps 2.5 times (up to 4 stages).

4. Improves the efficiency of the process, specifically to reduce the time of extraction in 200 times (from 72 h to 15 min).

Industrial applicability.

The inventive method of obtaining used to obtain pilot aqueous propylene glycol extracts of plant materials is an indispensable component products, cosmetics and perfume industry and goods of household chemistry in terms of pilot production of the Institute of organic and Fizicheskii them. A.Ye.Arbuzov Kazan scientific centre of Russian Academy of Sciences. Organization of production is planned in 2009

Table 1
Organoleptic and physico-chemical properties of extracts obtained in the rotary pulsation apparatus according to current regulatory documents (technical specifications TU 9154-010-02700055-2002 with changes in 1.2., THE 9154-014-12967730-2006)
ExamplePhysico-chemical characteristics
AppearanceSmelln20Dρ, kg/m3CC
Example 11,432610380,12
Example 21,432210340,12
Example 31,432610350,16
Example 41,433310380,22
Example 51,428610430,18
Example 61,429210320,15
Example 71,428610380,20
Example 81,430810470,24
Example 9 1,431210460,18
Example 101,431810480,16
Example 111,431610460.14
Example 121,431410500,22
The norm, not more on THE 9154-010-02700055-2002 with changes 1.2Clear liquid from yellow to green with various shadesWith a predominance of aromatic substances, the nature of this type of raw materials1,4270-1,43901005-11102.5
Example 131,33821016 0,18
Example 141.336810200,15
Example 151,342810180,14
Example 161.343010180,22
Example 171.339610160,19
Example 181,339210200.14
Example 191.346210220.20
Example 201.344610250,21
The norm, not more on THE 9154-014-12967730-2006Clear liquid yellow to brown with different shadesWith a predominance of aromatic substances, the nature of this type of raw materials1,3330-1,34901000-10601,2

Table 2
The dependence of the content of flavonoids in the extracts obtained in the rotary pulsation apparatus, process conditions
ExampleThe time of extraction, minutesTemperature, °CThe output of flavonoids, %
no PPDaisyTansyHighlander pepperEchinacea
Example 13 2583
Example 232582
Example 332588
Example 432584
Example 553088
Example 653085
Example 7530 92
Example 853087
Example 9104091
Example 10104094
Example 11104095
Example 12104096
Example 13154587
Example 14154592
Example 15154593
Example 16154590
Example 17205582
Example 18205585
Example 19205587
Example 202086
Prototype method72 hours20-3053656264

Table 3
Data on microbiological purity of the extracts obtained in the rotary pulsation apparatus according to current regulatory documents (SanPiN 1.2.681-97; MUK 4.2 801-99)
ExampleThe number of mesophilic aerobic and facultative anaerobic microorganisms, CFU in 1 gSeeding
Fungi and yeast, CFU in 1 gBacteria of the coli group (coliforms); 1 gPseudomonas aerugnosaStaphylococcus aureus
Example 1<10<10Not selectedNot selected Not selected
Example 2<10<10Not selectedNot selectedNot selected
Example 3<10<10Not selectedNot selectedNot selected
Example 4<10<10Not selectedNot selectedNot selected
Example 510<10Not selectedNot selectedNot selected
Example 610<10Not selectedNot selectedNot selected
Example 710<10Not selectedNot selectedNot selected
Example 810<10Not selectedNot selectedNot selected
Example 910<10Not selectedNot selectedNot selected
Example 1010<10Not selectedNot selectedNot selected
Example 1110<10Not selectedNot selectedNot selected
Example 1210<10Not selectedNot selectedNot selected
Example 1360<10Not selectedNot selectedNot selected
Example 1440<10Not selectedNot selectedNot selected
Example 1540<10Not selectedNot selectedNot selected
Example 1680<10Not selectedNot selectedNot selected
Example 174010Not selectedNot selectedNot selected
Example 184010Not selectedNot selectedNot selected
Example 198010Not selectedNot selectedNot selected
Example 20 8010Not selectedNot selectedNot selected
Prototype method1200280Not selectedNot selectedNot selected
Norm, no more than1000100NoNoNo
Note: Microbiological purity of the extracts of examples 1 to 12, 16, 20 defined at the end of 12 months from date of manufacture. Microbiological purity of the extracts of examples 13-15, 17-19 and the method prototype is defined by the expiration of 3 months from the date of manufacture.

1. The method of obtaining the water-containing propylene glycol extracts of plant materials with high resistance to microbiological contamination by processing the raw material aqueous propylene glycol extractive agent, characterized in that the extraction process is carried out in a rotary pulsation apparatus without pre-soaking in continuous circulation during setnoservercaching raw material and extractant from 1:10 to 1:20 and the rotor speed 3600-4400 rpm for 5-15 min at a temperature of 25-55°C, followed by separation of the solid plant parts by filtration.

2. The method according to claim 1, characterized in that as the aqueous extractant use of 1,2-propylene glycol with a water content of from 0.1 to 95 wt.%.



 

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4 cl, 4 ex, 1 tbl, 1 dwg.

FIELD: medicine.

SUBSTANCE: invention concerns chemical-pharmaceutical industry, and can find application in manufacturing of medical, preventive, cosmetic and sanitary-and-hygienic agents like gels, sprays, balms, creams, lotions and liquids for wipes of disinfecting and sanitation actions with antifungal, antiinfective and antiviral activity without by-effects. An effective fungicidal, antiinfective, viricidal, adaptogenic and antiradiation agent contains the active substances made of vegetable raw bee balm in the form of oily, water-alcohol extracts and bee balm essence.

EFFECT: bee balm extract complex (BBEC) as a stabilised suspension of phospholipid vesicles allow incorporating lipophilic and hydrophilic fractions of complex active substances of bee balm as one structure, provides their stable transport and possesses expressed inactivating activity in relation to pathogenic microorganisms (viruses, bacteria, fungi and protozoa).

4 cl, 4 ex, 1 tbl, 1 dwg.

FIELD: medicine.

SUBSTANCE: invention concerns pharmaceutical, food, cosmetic industry. Wood substance of larch root is chopped to particle size 0.5-1.5 mm and at least twice extracted at temperature less than 45°C in cavitation condition at maintained ethanol concentration within 80-86%. Sawdust is separated from the extract. The prepared extract is kept within 20-30 hours and separated from recovered resins and oils. The extract is steamed to concentration 40-45% and separated from recovered resins and oils again. The extract is steamed to concentration 8-11% and separated from recovered resins and oils again. Then the extract is recrystallised by freezing to temperature -20 to -40°C within 6-8 hours. Defrosting is performed 24 to 36 h at 5-10°C. Defrosted solution is elutriated. The prepared solution is filtered and dried in nitrogen atmosphere at temperature not exceeding 40°C. Thus dihydroquercetin in native form of purity 92-96% is prepared.

EFFECT: invention allows for high-yield native DHQ per a unit of initial wood, simplified technological process, reduced consumption of organic solvents and electric power.

1 ex

FIELD: medicine.

SUBSTANCE: invention concerns medicine, namely therapy and neuropathology, and concerns treatments of cardiovascular and nervous diseases. It is ensured by daily intravenously drop-by-drop introduction of physiologic saline 200 ml containing magnesium sulphate, ascorbic acid, hydrogen peroxide in a certain percentage ratio within 15 days. From the 16th day, during the following 7 days, aqueous solution 200 ml containing vitamin complex and cavinton in a certain percentage ratio is additionally introduced. Besides, from first day of treatment, Cerbrum Compositum-N is daily injected intramuscularly every second day within 21 days and 10% herbal tincture of Sophora, mistletoe and arnica taken in equal ratio and dosed 1 tablespoon at 7,12,17,21 o'clock. In addition, a suspension 5 ml containing live hen's egg per 150 ml physiologic saline is introduced once a week.

EFFECT: invention provides effective treatment of cardiovascular and nervous diseases in reduced drug loading ensured by optimum quantitative and qualitative composition, as well as developed schedule of drug introduction.

3 ex, 1 tbl

FIELD: medicine, oncology, amino acids.

SUBSTANCE: invention relates, in particular, to the development of an antitumor preparation based on natural substances. Invention relates to an amino acid preparation comprising at least one modified essential amino acid obtained by treatment of amino acid by ultraviolet radiation (UV) at wavelength 250-350 nm for 12-80 h at temperature 15-30oC or with ozone at temperature 15-25oC. The modified amino acid has no toxicity for health cells. Also, invention relates to a method for preparing such preparation. Invention provides the development of an antitumor preparation based on modified amino acids and expanded assortment of antitumor preparations being without cytotoxicity for normal cells.

EFFECT: valuable medicinal antitumor properties of preparation.

8 cl, 4 tbl, 2 dwg, 4 ex

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