The Development of the New Approaches to the Standardization of the Monarda fistulosa L. Herbs

In the present paper are discussed the results of the study on the development of the new approaches to the standardization of the Monarda fistulosa L. herbs. From the herb of the Monarda fistulosa L. there were isolated for the first time isorhoifolin (apigenin-7-O-rutinoside) and linarin (acacetin-7-O-rutinoside) chemical structures of which there were elucidated by means of 1H-NMR-, 13C-NMR-, UV-spectroscopy, mass spectrometry and results of chemical transformations. It was determined, that the isolated flavonoids cause the spectral characteristics in the UV spectra of the water-ethanolic extracts from the Monarda fistulosa L. herbs. It was substantiated the expediency of the estimation of the total flavonoids in the herbs of Monarda fistulosa L. calculated on isorhoifolin. As results there was development the method of the quantitative determination of the total flavonoids in the herbs of Monarda fistulosa L. by the using of the differential spectrophotometry at an analytical wavelength of 394 nm. It was determined that the content of the total of flavonoids in the raw materials of the studied plant varies from 4.23±0.08% to 7.68±0.12%.

Design of Experimental Approach Biosensor for the Development and Validation of UV Spectrophotometry Method for Determination of Thiamine in Biological Samples and Tablet Formulation

UV-Visible spectroscopy method has been developed for the analysis of Thiamine in biological and pharmaceutical product, based on a chromogenic derivatizing reaction using PDAB (P- dimethyl amino benzaldehyde) reagent. A Central Composite Design (CCD) design with response surface methodology was executed for optimization of experimental conditions of drug with a smaller number of experimental trials. Three independent factors, the concentration of PDAB, the volume of PDAB reagent, and volume of HCl, were used to construct a mathematical model and study the effects of these independent factors on responses as absorbance. The colored complex exhibits a Red shift with absorption maximum λmax at 425 nm, which was selected as the analytical wavelength. The drug seems to be linear, which was established via the regression analysis from 5-30 μgmL-1, with an R2 value of 0.998.The % RSD for intraday and interday precision was < 2%, with good recovery ranging from 95.02 to 101.43% with biological and pharmaceutical samples. LOD and LOQ of the developed method were found to be 1.51 μg mL-1 and 4.57 μg mL-1.This method can be used in routine analysis of pharmaceutical products containing aromatic primary amines along with an estimation of biological samples like urine, blood, sweat, faeces.

pKa Determination of Carvedilol by Spectrophotometry

Proper knowledge of the pKa value of a compound is of uttermost importance for understanding the behavior of a drug inside the body. The pKa value of Nonselective alpha-1 and beta-blocker Carvedilol shows controversies in literature, whereas values between 7.7 and 8.7 have been previously reported. In this research paper, the pKa value of Carvedilol was re-evaluated using UV-vis spectroscopy. The analytical wavelength used was 241nm. The obtained sigmoid pattern was non-linear fitted using the Boltzmann sigmoidal algorithm. The determined pKa was 7.77 ± 0.09. This value is in accordance with some of the literature publications. Since extensive statistics and multiple replicate experiments were performed, it is assumed that 7.8 is the true pKa value of Carvedilol.

Method of Determining the Sum of Flavonoids in Tanacetum Vulgare Flowers

Одно из лекарственных растений, являющихся источником создания высокоэффективных лекарственных средств, – пижма обыкновенная. Цветочные корзинки пижмы содержат значительное количество флавоноидных соединений (лютеолин, апигенин, акацетин, кверцетин, цинарозид), эфирные масла, фенольные кислоты, дубильные вещества, горечи и др. Основными методами извлечения биологически активных веществ из лекарственного растительного сырья являются методы экстракции, которые приводят к накоплению необходимых биологически важных компонентов в определённом экстрагенте. В работе изучено влияние концентрации экстрагирующего вещества и времени экстракции на полноту извлечения суммы флавоноидов из цветков пижмы обыкновенной. В результате анализа определяли содержание суммы флавоноидов (в пересчёте на цинарозид) в экстрактах этанола различной концентрации. Установлено, что оптимальным экстрагентом является 70%-й этиловый спирт, а экстрагирование в течение 30 минут наиболее эффективно при соотношении сырьё/экстрагент 1:50. Считаем наиболее целесообразным использование в методике количественного анализа суммы флавоноидов дифференциальную спектрофотометрию и государственный стандартный образец (ГСО) цинарозида при длине аналитической волны 425 нм. One of the medicinal plants that are the source of the creation of highly effective drugs is Tanacetum vulgare. Anthodium of Tanacetum vulgare contains a significant amount of flavonoid compounds (luteolin, apigenin, acacetin, quercetin, cinaroside), essential oils, phenolic acids, tannins, bitterness, etc. The main methods for extracting biologically active substances from medicinal plant raw materials are extraction methods that lead to the accumulation of the necessary biologically important components in a certain extragent. In the paper the effect of the concentration of the extracting substance and the extraction time on the completeness of the extraction of the sum of flavonoids from the flowers of Tanacetum vulgare was studied. As a result of the analysis the content of the sum of flavonoids (in terms of cinaroside) in ethanol extracts of various concentrations was determined. It was found that the optimal extragent is 70%-ethyl alcohol, and extraction for 30 minutes is most effective at a raw material/extragent ratio of 1:50. We consider it most advisable to use differential spectrophotometry and a state standard sample (SSO) of cinaroside at an analytical wavelength of 425 nm in the method of quantitative analysis of the sum of flavonoids.

Development of the quantitative test methods to determine the number of flavonoids in flowering shoots of semi-soft hawthorn

Flowers, fruits and shoots of various genus Hawthorn (Crataegus L.) species are used in domestic and foreign medical practice as cardiotonic agents. It is also possible to use hawthorn raw material for the prevention of cardiovascular system diseases among medical and pharmaceutical personnel. We consider semi-soft hawthorn Crataegus submollis Sarg. to be a prospective raw material species as its flowering shoots are chemically similar to the red-haw hawthorn flowers. We developed the quantitative test method to determine the number of flavonoids expressed as hyperoside in flowering shoots of semi-soft hawthorn using differential spectrophotometry with an analytical wavelength of 412 nm.

Development of the method for spectrophotometric quantitative determination of the total flavonoids in Bupleurum multinerve herb

The article presents the method for the quantitative determination of flavonoids for the analysis of Bupleurum multinerve herb based on the method of differential spectrophotometry. The optimal conditions for analysis have been determined. They include extractant 40% ethyl alcohol, ratio of raw materials and extractant 1 : 100, extraction time of 60 minutes in the boiling water bath, complexing agent of 1 ml of 2% aluminum chloride. The use of rutin as a standard has been experimentally validated, analytical wavelength is 412 nm. The relative error of the mean result (for n = 9) was 3.20%. Validation studies of the method have shown that it meets the criteria: linearity (r = 0.99988), correctness, specificity, and precision. The analytical range of the method is 8.6726.08 g/ml. The method is recommended for the inclusion into the new edition of the Pharmacopoeia Monograph for this type of plant material.

Development and validation of methods of quantitative determination of biologically active compound n-(2-[4-oxo-3(4h)-quinazolinyl]propionyl)guanidine

This paper presents the results of the selection and justification of the conditions for determination of a new biologically active compound (BAC) VMA-13-15, which is N-(2-[4-oxo-3(4H)-quinazolinyl]propionyl)guanidine bymeans of the spectrophotometry. By using the calculated values of BAC ionization constants, it was proposed to use purified water as a solvent. The maximum light absorption at 266 nm was chosen as the analytical wavelength. This was justified by the fact that in aqueous solutions 99% BAC are in the molecular form, which allows to determine it with the error limit of 1.29%, and with the least amount of dilutions. The study showed that the proposed method is specific and linear in the analytical concentration of 0.0010.004%, as well as it is precise and correct, which confirms the possibility of its use for quantitative determination.

STUDY OF BAICALIN HYDROLYSIS KINETICS IN THE PROCESS OF ITS EXTRACTION FROM SCUTELLARIA BAICALENSIS GEORGI ROOTS

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.

A New Technology for Extraction of Essential Oil from Anethum graveolens L. Fruits

The aim of this work was to study the possibility of perfluoroorganic solvents use for extraction of main compounds of essential oil from Anethum graveolens L. fruits. We used Anethum graveolens L. fruits with particle size of 0.1–0.5 mm for extraction. We used the method of simple maceration for 24 hours, with raw material to solvent ratio of 1:10 w/v at 24±1°С. Besides, we used the method of circulation extraction in the Soxhlet extractor with raw material to solvent ratio of 1:5 w/v for 1 to 4 hours. The qualitative analysis of extracts was carried out by the method of GC-MS. The quantitative analysis of carvone was carried out by the method of RP HPLC at 240 nm analytical wavelength. The use of simple maceration method provided the following yields of carvone into all types of solvents: 95±4 % for n-hexane, 95±4 % for Novec 7100, and 69±3 % for Novec 1230. The use of the circulation method of extraction for 60 min of solvent circulation provided the following yields of carvone: 93±4 % for Novec 1230 and 92±4 % for Novec 7100. It was noted that the extract obtained with solvent Novec 7100 was contaminated by fatty oil and required an addition stage of purification. The results obtained suggest that perfluoro organic solvents have good prospects and applicability in the phytotechnology for the extraction of some types of biologically active compounds and essential oils from the plant raw material.