The aim. This article is devoted to the intensification of the production process of a thick extract of milk thistle fruits using ultrasonic processing of raw materials.Materials and methods.As an object of the study, the crushed milk thistle fruitss from Penza “Biokor” company were used. As the extractant, an aqueous solution of ethanol 70% vol. was used. For ultrasonic processing of plant materials and extractant, the installation “Bandelin SONOPULS HD 3200” was used, the ultrasound frequency was 20 kHz, the radiator power was 280 W, and the temperature was 25°С. The concentration of the extract was performed using a rotary evaporator RV-10 at the temperature of 60°C and a vacuum of 600–650 Mmhg to a residual moisture content of 25%. Qualitative and quantitative analysis of the thick extract was carried out using spectrophotometry and chromatography. Quantitative analysis of the amount of flavolignans was performed on an SF-56 spectrophotometer. The separation of the flavolignan complex and the quantification of silibinin was performed on a liquid chromatograph “Agilent Technologies 1200 Infinity”.Results and discussion. During the study it was found out, that processing of the crushed milk thistle fruits by ultrasound at the soaking stage almost doubles the output of the flavoligan complex from medicinal plant materials. The maximum amount of flavolignans is extracted when the fruits of milk thistle and extractant are processed with ultrasound at the frequency of 20 kHz for 5 minutes. Thus the obtained thick extract of milk thistle fruits in the component composition contains both the target flavolignan complex (87.39%, silibinin – 24.36%), providing the hepatoprotective effect, and flavonoids – chlorogenic acid (1.69%) and dihydroquercetin (10.92%) exhibiting antioxidant activity. It was established that, according to the qualitative composition of flavolignans, the obtained thick extract corresponds to preparations based on milk thistle. Thus, for the first time, the method was proposed for obtaining a thick extract of milk thistle fruits using ultrasonic processing of raw materials and extractant at the soaking stage. The obtained thick extract is proposed to be used as an active pharmaceutical substance for the production of granules based on methionine and milk thistle flavolignans.Conclusion. The results of the experiments allow us to recommend obtaining a thick extract of the milk thistle fruits, using the stage of ultrasonic processing of raw materials and extractant for 5 minutes at the ultrasound frequency of 20 kHz.
The aim of this study was to investigate the kinetics of baicalin hydrolysis in the process of its extraction from Scutellaria baicalensis Georgi roots.Materials and methods. For the studies, Scutellaria baicalensis Georgi roots with a particle range of 0.1–0.5 mm were used. The method of extraction was a simple maceration during a specified period of time, the ratio of plant raw material : extractant was 1:10 w/v at the temperature of 24±1°С. Baicalin and baicalein contents were analyzed by reverse phase high performance liquid chromatography (RP HPLC) at the analytical wavelength of 275 nm. The extractant was a water solution of ethanol 26, 43, 59, 72, 81, 97±1% v/v. The time of the extraction was from 1 to 24 hours.Results. The experimental points of dependency of baicalin concentration in the extract on the time of extraction for ethanol solutions with a concentration of 43 and 72% v/v are closely approximated by a linear equation in coordinates lnC=f(t). The value of determination coefficient is more than R²˃0,99. Half lifetime for baicalin has been calculated: for ethanol with the concentration of 43% v/v it is 4.3±0.7 hours, and for ethanol with the concentration of 72% v/v it is 42.3±1.8 hours.Conclusion. Baicalin hydrolysis kinetics in the process of its extraction from Scutellaria baicalensis Georgi roots with 43 and 72% v/v ethanol concentration. has been studied. It has been established that the process of baicalin hydrolysis is well described by the first order kinetic equation. The constants of baicalin hydrolysis during its extraction from Scutelaria baicalensis roots with ethanol having different concentrations have been calculated. Recommendations on technology optimization for baicalin or baicalein extraction from Scutellaria baicalensis Georgi roots have been given.
This article presents results of the study and modeling of solvent influence on isosalipurposide extraction from Helichrysi Arenarii flowers.The aimof this work is to study the influence of the solvent on isosalipurposide extraction from Helichrysi arenarii flowers and suggest a theoretical model for description of the results obtained.Materials and methods. The basic materials were: a ground plant raw material of Helichrysi arenarii flowers. water solutions of ethanol (26, 43, 59, 72, 81, 97±1% v/v.), methanol, 1-propanol, 2-propanol, acetone and ethyl acetate. The extracts were obtained from the plant raw materials / solvent at the ratio of 1:5 (wt./vol.) by maceration for 24 hours at the temperature of 24±1°С. The analysis of the extracts was carried out by reversed-phase high performance liquid chromatography and isosalipurposide reference substance.Results and discussion. A dependence of isosalipurposide concentration in ethanol-water extracts on ethanol concentration in the solution was studied. It has been found out that maximum concentration of isosalipurposide is observed in the solutions with ethanol concentration of 75±5% v/v. This range of ethanol concentrations corresponds to solvent’s dielectric constant value of 38±3 units. The regression equation of dependence between isosalipurposide concentration in the extract and dielectric constant of ethanol-water solution has been obtained. Optimal concentration of the solvent has been theoretically predicted and experimentally verified as in the case of water solutions of methanol, acetone, 1-propanol, and 2-propanol.Conclusion. It has been determined that solvent’s dielectric constant has the most significant influence on the extraction process of phytocompound from the plant raw material. A mathematical model for description of the dependence of isosalipurposide concentration on dielectric constant of ethanol-water solutions has been substantiated theoretically and tested. The optimal range of solvent’s dielectric constant to obtain maximum concentration of isosalipurposide in the extract has been found.
Цель. Проверка адекватности выдвигаемой рабочей гипотезы, которая объясняет и количественно описывает распределение БАВ в экстракционной системе из цветков бессмертника песчаного и растворителя, с помощью регрессионного анализа в предсказанных теорией координатах. Материалы и методы. Для исследований использовали измельченное фармакопейное растительное сырье «Бессмертника песчаного цветки» (Helichrysum arenarium L. flores). Анализ извлечений проводили с помощью ОФ ВЭЖХ метода. В качестве стандартных веществ использовали изосалипурпозид, салипурпозид, хлорогеновую кислоту ФСО ГФУ, содержание ≥98,0 %. Аналитические длины волн 370, 290 и 325 нм. Результаты. Экспериментальные данные хорошо аппроксимируются регрессионными линейными уравнениями в предсказанных теорией координатах 1/С=f(V) и ln(b/a)=f(1/T). При этом коэффициент детерминации регрессионных уравнений, имеет значение R²≥0,998, что говорит о функциональной зависимости между изучаемыми параметрами и подтверждает адекватность разработанных уравнений. Эксперимент выявил необходимость введения в математическую модель дополнительной константы. Заключение. Предложена рабочая гипотеза, которая объясняет и количественно описывает распределение БАВ в экстракционной системе из цветков бессмертника песчаного и этанола 80 % об. С помощью рабочей гипотезы разработаны математические модели, адекватность которых доказана с помощью регрессионного анализа в предсказанных теорией координатах. Полученные результаты не отвергают гипотезу, что механизм распределения БАВ между фазами в экстракционной системе объясняется и описывается классическим распределением Больцмана для дискретных значений энергии молекул (или квантовым распределением Ферми-Дирака). Ключевые слова: цветки бессмертника песчаного; Helichrysum arenarium, изосалипурпозид; салипурпозид; хлорогеновая кислота; равновесие; классическое распределение Больцмана для дискретных значений энергии молекул
Introduction. The creation of rational combined medicines with hepatoprotective activity is an urgent task of medicinal science. Ademetionin shows pharmacological ef-fectiveness in cytolysis, cholestasis, synthetic insufficiency. Silybin, in turn, is effective in cytolysis, synthetic insufficiency, mesenchymal inflammation, fibrosis and pathological regeneration. Thus, the combination of these substances covers almost the entire set of clinical and morphological syndromes of liver damage and has a wide range of effects in various liver pathologies.Aim. The purpose of this study was to develop a combined granular dosage form containing a thick extract of milk thistle, ademetionin and analytical support for this process.Materials and methods. To obtain a thick extract from the fruits of Silybum marianum L. a traditional percolation method was used in a battery of 3 diffusers. Extractant removal was performed using a rotary evaporator IR-1M3 under vacuum. For the analysis of silybin in the obtained thick extract from the fruit of S. marianum L. the method of HPLC was used. Validation evaluation of the method was performed according to generally accepted parameters.Results and discussion. A modular combined dosage form based on a thick extract of S. marianum L. and ademethionine was developed. Lactose was introduced as an auxiliary agent. The quality of pellets was evaluated according to generally accepted criteria. The validation parameters of the manufactured dosage form were determined using the HPLC method. Accuracy and precision were determined by the method of additives in a series of 9 experimental samples of granules. The results of determining the linearity, precision and correctness of the method for determining silybin and ademetionin in a combined model drug form showed correct results.Conclusion.Thus, a combined granular dosage form containing a thick extract of milk thistle, ademetionin, has been developed. Analytical support of this process using the HPLC method was performed. Validation studies of the developed methodology were carried out. The field of application of the obtained results is practical pharmacy. Further research should concern the conduct of a set of pharmacological tests.
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