Abstract: Introduction.  Today, innovative technologies are widely used in pharmacology (in particular, in the production of herbal preparations), in cosmetology (obtaining various extracts and oils, complex preparations), as well as in the food industry (as natural dyes, etc.). Plant extracts with a high level of risk do not have a harmful effect on the human body, except that they provide environmental safety, which creates a special interest for the pharmaceutical industry . vibrocavitation and supercritical fluid CO2 extraction. Aim.  The choice of the optimal level of extraction to obtain a high level of fenugreek seeds. Materials and methods.  Obtaining a vibrocavitation extract with an experimental vibration-explosive installation made at the Department of Processes and Apparatus of the St. Petersburg State Technology Institute. Extracts at a temperature of 60±2 ºС. The frequency of revolutions of the homogenizer ranged from 1000 to 5000 rpm. Ultrasonic impact using ultrasound unit I100-6/4 Ultrasonic effect on solid plant material with an intensity of 22 kHz for 60 minutes. The time of extraction in a vibro-cavitation extractor-homogenizer was studied for optimal values. Supercritical fluid CO2-extraction is obtained in two versions with the use of extragent (96% ethanol in the presence of carbon dioxide: ethanol 9:1) and without it. Extraction of the sound of a supercritical fluid extraction system with a 1-liter vessel. SFE1000-2-BASE with a kit for upgrading the SFE1000-2-BASE system to an SFE1000M1-2-FMC50 system (Waters, USA). The flow rate of the extractant was 60 g/min. Emergency listening for one hour and pressure 200, 300 and 400 bar. Extraction is observed three times. The obtained extracts indicate the amount of extractive substances according to article of Russian state pharmacopoeia 1.5.3.0006.15 «Determination of the content of extractive substances in plant raw materials and medicinal plant preparations». Quantitative determination of the saponin complex of parasitic seed seeds on an Agilent QTOF-6530 chromatograph with two ESI and APCI ionization sources according to Gravel et al. Results and discussion.  Studies have allowed to determine the amount of extractives in the seeds and choose the most promising method.  Conclusion.  As a result of our research, it was found that the most promising extraction method for extracting seeds is a parasitic with vibration extraction at frequent revolutions of the homogenizer of 5000 rpm and an extraction time of 60 minutes.

Abstract: Introduction . In recent years, substances extracted from plant materials have been widely used in the pharmaceutical, cosmetic and food industries. Such substances are used as solutions, dry extracts for the manufacture of medicines, dietary supplements, cosmetic creams, food additives in various forms – tablets, capsules, solutions, granular powders. The extraction of valuable substances from plant materials is carried out using the extraction process, which is carried out by various methods and in apparatuses of various designs. Earlier, a comparative study of the extraction of dioscin from fenugreek by various methods was carried out: in devices with a stirrer, in an ultrasonic field, supercritical, fluid CO2 extraction, and in a vibro-cavitation homogenizer. It is shown that the most effective method is the extraction carried out in a vibrocavitation homogenizer. Aim .To analyze the kinetics of the extraction of dioscin from fenugreek seeds, to determine the optimal values of the required degree of grinding of the raw materials, working temperature, the concentration of ethyl alcohol in the solution and the rotational speed of the rotor of the vibrocavitation homogenizer. Determine the effective mass transfer coefficient responsible for the intensity of mass transfer inside the particles. Materials and methods . An experimental study of the extraction of valuable components from plant materials was carried out in a laboratory unit with a vibrocavitation homogenizer of periodic action. As raw materials were used seeds of hay fenugreek, ecotype of Morocco, acquired in the company Fitokasa, Casablanca (Morocco), which we used for research. Commodity analysis showed that raw materials comply with the requirements of the State Pharmacopoeia XIVth edition. As extractants, aqueous solutions of ethanol with an alcohol concentration of 40, 50, 60, 70, 80, and 90 %. The analysis of the kinetics of the process was based on the following ideas. Extraction begins with the surface of the particles of plant material. As the extracted component moves into the volume of the solution, the extractant penetrates into the internal pores of the particles, and the surface on which the extractant and the extracted component interact is gradually shifted into the individual particles. In this case, the resistance to mass transfer in the region between the specified surface and the outer surface of the particle increases over time. Results and discussion . An analysis of the results shows that the rotor speed significantly intensifies the process. In addition, the influence of the rotor speed is most pronounced at the initial stage of the process, when the surface layers of particles of plant material are extracted. It was also found that the resistance to mass transfer inside particles increases significantly as it approaches the final stage of the process, and with an increase in the rotor speed, it increases, especially at the initial stage of the process, which is associated with the intensity of cavitation and the weakening of its effect as the process deepens inward particles. Conclusions . The obtained dependences are necessary to determine the duration of the extraction process in a batch mode, or the average residence time of seeds in the working volume when organizing the process in a continuous mode.

Abstract: Introduction.  According to the literature, modern technologies, in particular, extraction in an ultrasonic field, make it possible to obtain concentrates of biologically active substances (BAS) with almost complete preservation of the chemical composition inherent in natural raw materials and high yield of extractive substances. At the same time, the ability to regulate the concentration of recoverable active substances during the technological process opens up prospects for the use of natural components as the main pharmaceutical substance. Aim.  The purpose of this study was to select the optimal extraction method for obtaining extracts with a high content of BAS from fenugreek seeds.  Materials and methods.  Extracts were obtained at a temperature of 60±2 °С, by the method of dynamic maceration using an ultrasonic device. Ultrasonic extraction was performed using an ultrasonic installation I100-6/4. In both cases, purified water and ethanol solutions in various concentrations from 40 to 90% were used as extractants. The ratio of raw materials: extractant was as 1:10 (by weight). A portion of vegetable raw materials (10 g) was placed in a glass and poured 100 cm3 of extractant. Next, maceration or sonication was performed. Maceration was performed with magnetic stirring, the rotation speed was 100 rpm. Extraction was carried out at a temperature of 55–60 °C for 5 hours. Ultrasonic effects on solid plant materials were carried out with an intensity in the range from 17 to 22 kHz for 30–60 minutes. Results and discussion.  Studies have allowed to determine the amount of extractives in the seeds of fenugreek hay, and choose the most promising method of extraction to obtain extracts with a high content of biologically active substances. A comparison was made between dynamic maceration and ultrasonic extraction. The most promising was the method of ultrasonic extraction at an oscillation frequency of 22 kHz. For 1 hour of extraction, it was possible to achieve depletion of raw materials. It is established that the content of extractable substances directly proportional depends on the duration of treatment and the frequency of ultrasonic waves. The correlation coefficient was 0.78. Conclusion.  Ultrasonic extraction when exposed for 60 minutes allows you to get a greater amount of extractives compared with dynamic maceration. To achieve the same level of extractive substances by the method of dynamic maceration, the raw materials must be processed within 5 hours.

Abstract: Introduction . Vibration cavitation homogenizers are increasingly used in various industries, including the pharmaceutical industry – for the preparation of creams, gels to give them a homogeneous composition, and more recently for the extraction of valuable substances from plant materials. As we have shown earlier, a comparison of the extraction of dioscin from fenugreek seeds, carried out in devices of various designs, under the same conditions for organizing the process showed that the most effective method was the extraction method in a vibro-cavitation field. Obviously, this is due to the fact that cavitation reduces the diffusion resistance of the process and, thus, increases the intensity of the process of transferring the mass of a substance from the solid phase to the solution. However, the extraction process in apparatus of this type is complex and is accompanied by crushing of seeds, which leads to a change in the dispersed composition of the solid phase. Aim . Conduct a theoretical and experimental analysis of the process of grinding hay fenugreek seeds particles in a vibrocavitation homogenizer, accompanied by the extraction of biologically active substances, as well as obtaining dependences that allow evaluating the contribution of grinding to the formation of the dispersed composition of the meal in this apparatus and determining the average particle size as a result of crushing. In earlier works, using the example of the extraction of dioscin from fenugreek seeds, it was shown that an increase in the rotor speed increases the yield of biologically active substances. However, fine grinding of raw materials often leads to the formation of a sediment layer that pollutes the solution with ballast substances and complicates its purification, and also reduces the yield of biologically active substances, therefore, the study of this process is necessary to control the dispersed composition in order to ensure the highest extraction efficiency in devices of this type. Materials and methods . The first stage of the study was the theoretical analysis of the grinding process, since it is a special case of a large class of processes in which the dispersed composition of the solid phase is not constant. Therefore, in this work, for the mathematical description of particle grinding, a model is used that takes into account the kinetic features of the process under consideration. An experimental study of the extraction of valuable components from plant raw materials was carried out in a laboratory setup with a vibro-cavitation homogenizer of periodic action. As a raw material, we used fenugreek seeds purchased from LLC «Stoing», Moscow (Russia), which we used for research. Commodity analysis showed the compliance of raw materials with the requirements of the GF XIV edition. The initial, aqueous solution of ethanol (volume concentration 60 %) with fenugreek seeds was loaded into glass 6, in a volume of 0.2 liters, then the rotor of the apparatus was brought into rotation and brought to a given rotation frequency. The experiments were carried out at a rotation frequency of 1000, 3000 and 5000 rpm (16.7; 50 and 83.3) 1/s. At each value of the rotor speed, the process time varied in the range from 0 to 50 minutes, and the process was carried out for 60, 120, 180, 240 and 300 seconds. Studies carried out for 5 minutes or more showed that the dispersed composition of the meal practically does not change over time, but significantly depends on the rotor speed. Thus, after 5 minutes, a certain stabilization of the dispersed composition occurs and further residence of the material in the apparatus does not lead to a noticeable change in the dispersed composition. After each experiment, the meal was taken, dried, and sieve analysis of the dispersed composition was carried out. Results and discussion . Based on the results obtained by processing the experimental data according to the equation, the values of the average probability of particle crushing were calculated and, as it turned out, it practically does not depend on time, but depends only on the rotor speed. The dependence of the change in the average probability of particle grinding at different rotor speed was obtained. The analysis of these results showed that the value of the average probability of particle grinding in the cavitation homogenizer increases with an increase in the rotor speed, which is quite expected, since the frequency of contacts of particles with the working organs of the apparatus increases. In addition, the obtained dependence for the average probability of particle crushing is linear. This Expression quite accurately describes the values of the change in time of the relative mass of particles in the working range n = 16.7 – 83.3 1/s. Taking these values into account, the experimental and calculated results are in good agreement. Conclusions . The proposed approach and the results obtained can be used to assess the dispersed composition of particles obtained in other designs of devices of similar action.