{"title":"Determination of riboflavin in dragee “Revit” by HPLC","authors":"B. Varynskyi, M. Y. Zeleniuk, A. Kaplaushenko","doi":"10.14739/2409-2932.2022.2.258888","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.2.258888","url":null,"abstract":"The aim of the work is development of express, selective, reproducible methods for the determination of riboflavin by HPLC in a multivitamin preparation, dragee “Revit”.\u0000Materials and methods. Degasser, binary pump, autosampler, thermostated column compartment, diode array detector. Chromatographic column Zorbax SB-C18, 30 mm × 4.6 mm, 1.8 µm. Samples were prepared using analytical electronic scales Kern ABT 100-5M, ultrasonic bath Ultrasonic XUBA 3, nylon ultrafilters 0.12 µm.\u0000Results. 0.1 % formic acid was selected as a buffer solution in the eluent. The maximum values of logD were observed at intervals for riboflavin at pH from 2 to 4. Therefore, the maximum retention of the riboflavin was observed when using the eluent, рН which corresponds to this interval. The pH value for 0.1 % formic acid solution was 2.7. Therefore, such a buffer was chosen by us as part of the eluent. Acetonitrile was selected as the organic modifier. The optimal content of the compound was observed at 10 % acetonitrile.\u0000Conclusions. The chromatographic behavior of riboflavin on the basis of chemical-analytical properties was studied. The optimal conditions for chromatographic determination were determined and a specific, express method for the determination of riboflavin in “Revit” dragee was developed. The technique on a real sample of “Revit” dragee was elaborated. The method was recommended for use in control and analytical and research laboratories.\u0000 ","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"113 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79874919","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Ultrastructural changes in renal tissue in rats with renal failure under the influence of herbal composition BNO 2103","authors":"V. Chernykh, К. О. Zupanets, S. Shebeko","doi":"10.14739/2409-2932.2022.2.251800","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.2.251800","url":null,"abstract":"Management of chronic kidney disease is an urgent task of the global health care system, as untreated, it leads to partial or permanent loss of kidney function. Standardized herbal remedies are highly effective and relatively safe. That is why it is suggested to pay attention to herbal remedies already known for the treatment of genitourinary diseases to expand the indications for their use.\u0000The aim of the research is to study the nephroprotective properties of the standardized herbal composition BNO 2103, which is the active ingredient of Canephron N ®, in a model of renal failure in rats.\u0000Materials and methods. An experimental study was performed on 42 male white outbred rats weighing 150–200 g, which were divided into 4 groups. Nephropathy was induced by a single subcutaneous injection of 0.7 ml/kg of 2.5 % potassium chromate solution. Animals in 3 and 4 groups received BNO 2103 at a dose of 33.0 mg/kg and prednisolone at a dose of 1.9 mg/kg intragastrically daily for 20 days. After animals were sacrificed, their kidneys were obtained and studied with standard electronic microscopy methods.\u0000Results. BNO 2103 normalized the ultrastructural picture of the kidneys, however, with the presence of minor pathological signs. BNO 2103 reduced the destruction of basement membranes, improved organelle structure and increased metabolic processes in podocytes, and endotheliocytes, reducing the manifestations of degenerative-dystrophic changes in them. BNO 2103 was superior to the reference drug prednisolone.\u0000Conclusions. BNO 2103 showed a significant nephroprotective effect, normalizing the ultrastructural picture of the kidneys in rats with renal failure. This effect is most likely related to the presence of biologically active substances with a powerful antioxidant, anti-inflammatory, nephroprotective activity. The obtained results allow us to consider BNO 2103 as a promising nephroprotective agent for the treatment of chronic kidney disease.\u0000 ","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"73 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80295444","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Problematic aspects of modern professional training of pharmacy masters","authors":"N. Tkachenko, B. Hromovyk","doi":"10.14739/2409-2932.2022.2.258457","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.2.258457","url":null,"abstract":"The aim of the research is to analyze the process of professional training of pharmacy master’s in modern realities to identify problematic issues and find ways to solve them.\u0000Materials and methods. Critical analysis, content analysis, methods of generalization, and a combination of results were used in the work. Legal acts of the regulation of pharmaceutical education, data from the Unified State Database of education, 34 educational and professional programs for the preparation of pharmacy masters of 22 basic pharmaceutical institutions of higher education in the pharmaceutical direction were the material of the study.\u0000Results. The presence of a significant number of institutions of higher education was found. It leads to high costs per student due to the large volumes of their contingents in most institutions, as well as the likelihood of a slight global shortage and a decrease in the level of qualification. At the same time, there were no significant savings in training costs, which arises from the scale of activities. In addition, there is no proper state and public control over compliance with the institutions of higher education legal acts in the field of education and science. Analysis of the content of educational and professional programs revealed non-compliance with the legislation on the normative and variable part of the construction of the educational process and a significant variety of educational components. The existence of different approaches to the minimum number of credits for these components and graduation certification has been found. It will affect the process of integration of graduates into the international professional environment. It was shown that in a number of the institutions of higher education there was an inadequate qualification level of scientific and pedagogical workers in graduate departments and developers of the educational and professional programs.\u0000Conclusions. 78 institutions of higher education have been training pharmaceutical specialists on 23.02.2022. The proportion of part-time students among future specialists was characterized by an increase in the education level. Significant disagreements have been established among the cross-cutting educational and professional programs, according to which the training of Master of Pharmacy was carried out at the present stage. The ways of solving problematic issues of improving the educational space for the preparation of Master of Pharmacy were proposed.","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"15 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82636511","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yu. I. Korniievskyi, O. Panasenko, V. H. Korniievska, B. Varynskyi, M. M. Maletskyi
{"title":"Natural aspirin of some members of the Rosaceae and Salicaceae families","authors":"Yu. I. Korniievskyi, O. Panasenko, V. H. Korniievska, B. Varynskyi, M. M. Maletskyi","doi":"10.14739/2409-2932.2022.2.256639","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.2.256639","url":null,"abstract":"White willow Salix alba L., a member of the family Salicaceae is characterized by the presence of phenolic compounds and their glycosides (1.5–11.0 %), such as salicin, salicortin, salireposide, picein, triandrin, syringin, tremulacin, flavonoids (1–4 %) namely luteolin, apigenin, quercetin, quercimeritrin, cosmosin, diosmetin, tannins (8–20 %) i.e. catechins, anthocyanidins, halotanines of organic acids, ascorbic acid. Preparations of white willow bark are used as an antipyretic, anti-inflammatory, diaphoretic, analgesic, diuretic, and astringent. The rhizomes with roots of the commonly known dropwort or fern-leaf dropwort are Filipendula vulgaris Moench., member of the family Rosaceae are characterized by phenologicoside gaulterin, the hydrolysis of which produces salicylic aldehyde, tannins (up to 33 %), flavonoids, ascorbic acid, polysaccharides, starch. The herbs and flowers are used as anti-inflammatory, anti-rheumatic, vasodilator, gastric, and antiulcer agents.\u0000The aim of the work is to determine the composition of the white willow bark Salix alba L. tincture, a member of the willow family Salicaceae, using gas-liquid chromatography (GLC) and HPLC and to determine the composition of the tincture of the dropwort root Filipendula vulgaris Moench. family Rosaceae.\u0000Materials and methods. Raw materials (underground organs) of the dropwort Filipendula vulgaris Moench. and bark of the white willow Salix alba L., which were harvested in July 2020 at the ZSMU research site. Tinctures were prepared according to the production recipe (1:5) (extractant was 70 % ethanol), investigated by the gas chromatograph Agilent 7890B with mass spectrometric detector 5977B. The mass spectra library NIST 14 was used to identify the components. White willow bark tincture (70 % ethyl alcohol extractant) was used to determine the phenolic compounds content and salicylic acid derivatives. The study was performed by HPLC (high-performance liquid chromatography) and HPLC MS.\u0000Results. Qualitative and quantitative analysis of the components of Salix alba L. willow bark tincture was performed by gas-liquid chromatography, 39 components of different classes of biologically active compounds have been identified, among which the 10 components are predominated in quantitative content. The main one was Salicin (39.53 %). The GC analysis of the tincture of the dropwort roots, Filipendula vulgaris Moench., identified 34 components of different groups of biologically active compounds, dominated by 11 components, the main is Ethyl.alpha.-d-glucopyranoside (34.55 %). HPLC analysis confirmed the presence of phenolic compounds (flavonoids such as apigenin, and quercetin) and salicylic acid derivatives (glycoside salicin) in the tincture of white willow bark (Salix alba L.).\u0000Conclusions. By GC analysis the 39 components in tincture of white willow bark Salix alba L. were identified, 10 components were predominated, the main one was Salicin (39.53 %). The 34 components in the tincture o","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"7 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81821936","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Ye. O. Karpun, S. O. Borsuk, L. I. Kucherenko, V. Parchenko
{"title":"The study of the optical activity of some S-derivatives 4-R-5-((((3-(pyridin-4-yl)-1H-1,2,4-triazole-5-yl)thio)methyl)-4H-1, 2,4-triazole-3-thiols","authors":"Ye. O. Karpun, S. O. Borsuk, L. I. Kucherenko, V. Parchenko","doi":"10.14739/2409-2932.2022.2.255791","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.2.255791","url":null,"abstract":"About half of the drugs currently produced are chiral compounds, and about 90 % of these compounds are sold as racemates, consisting of an equimolar mixture of two enantiomers. Although they have the same chemical structure, most of the optical isomers of chiral substances show marked differences in biological activity. It is known that the presence of a single asymmetric atom has become almost an integral part of advanced drug design.\u0000The aim of this work was to determine the angle of rotation of the polarization plane of solutions of some S-derivatives of 4-R-5-((((3-(pyridin-4-yl)-1H-1,2,4-triazole-5-yl)thio)methyl))-4H-1,2,4-triazole-3-thiols and the establishment of regularities between the structure of the studied molecules and their optical activity.\u0000Materials and methods. The subject of the study was 2-[5-R1-4R2-1,2,4-triazole-3-ylthio]-1-aryletanols. The study of the angle of rotation of the plane of polarization of solutions of newly synthesized compounds was carried out using an Atago AP-300 polarimeter and the DFU 2.2.7 physical-chemical analysis method “Optical rotation”.\u0000Results. The results of the physical-chemical analysis were carried out that the studied compounds exhibit optical activity. The compound 1-((4-methyl-5-(((3-(pyridin-4-yl)-1H-1,2,4-triazole-5-yl)thio)methyl)-4H-1,2,4-triazole-3-yl)thio)-2-phenylethan-1-ol (+43° [deg∙g/cm3∙dm]). The only levorotatory substance was 1-(4-fluorophenyl)-2-((4-methyl-5-(((3-(pyridin-4-yl)-1H-1,2,4-triazole-5-yl)thio))methyl)-4H-1,2,4-triazole-3-yl)thio)ethan-1-ol with specific rotation [α]D20 = -43° [deg∙g/cm3∙dm].\u0000Conclusions. Studies had shown that 1-(4-fluorophenyl)-2-((4-methyl-5-(((3-(pyridin-4-yl)-1H-1,2,4-triazole-5-yl))thio)methyl)-4H-1,2,4-triazole-3-yl)thio)ethan-1-ol was able to rotate the light polarization plane to the left, which was evidence of the advantage of the S-enantiomer in the racemic mixture, and therefore this compound was considerable interest for further preclinical research. Also, all other analyzed compounds behave as optical isomers.","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88310280","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Heterocyclizations based on N-(R-hydrazine-1-carbonothioyl)cycloalkancarboxamides: functionalized azoles and their antimicrobial activity","authors":"О. V. Kholodniak, Yu. V. Shubina, S. I. Kovalenko","doi":"10.14739/2409-2932.2022.1.252037","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.1.252037","url":null,"abstract":"Synthesis and structural modification of azoles remains an important area of medical chemistry and allows to obtain new compounds with a wide range of biological activity. Among the significant number of azoles, 1,3,4-thiadiazoles and 1,2,4-triazoles attract special attention, among which are known drugs, larvicides, insecticides, growth regulators, etc. Even though heterocyclizations of functionally substituted hydrazines for their synthesis are well studied, N-(R-hydrazine-1-carbonothioyl)cycloalkanecarboxamides, and nowadays, remain reagents with undiscovered potential. Moreover, the introduction of lipophilic “pharmacophore” fragments (cycloalkanes) in the structure of 1,3,4-thiadiazoles and 1,2,4-triazoles is a promising direction for their modification. That should provide additional intermolecular interactions with enzymes and may lead to enhancement or alteration of the biological activity vector. Thus, the synthesis of new derivatives of this class of compounds and the study of their antibacterial properties remains an urgent problem of medical and organic chemistry.\u0000Aim. To investigate the heterocyclization of N-(R-hydrazine-1-carbonothioyl)cycloalkanecarboxa-mides, to establish the structure and antibacterial activity of the synthesized compounds.\u0000Materials and methods. Methods of organic synthesis, physical and physical-chemical methods of analysis of organic compounds (NMR 1H-spectroscopy, chromato-mass spectrometry, elemental analysis). The antimicrobial activity of the synthesized compounds was studied according to the generally accepted method for standard strains of microorganisms and fungi.\u0000Results. The peculiarities of heterocyclization of N-(R-hydrazine-1-carbonothioyl)cycloalkanecarboxamides have been studied and the factors influencing this reaction have been elucidated. It was shown that these compounds under the conditions of the heterocyclization reaction in concentrated mineral acids form 5-R-2-amino-1,3,4-thiadiazoles. The intermediate undergoes additional hydrolysis by cleavage of the cycloalkanecarboxyl fragment. Alternative methods for the synthesis of 5-R-2-amino-1,3,4-thiadiazoles were proposed. For the first time, the original 4-cycloalkanecarbonyl-3-(amino-,phenyloxo-(thio)methyl-1,5-dihydro-4H-1,2,4-triazole-5-thiones were synthesized by prolonged heating of the corresponding disubstituted thiosemicarbazides. It was not possible to extend this reaction to other diacylthiosemicarbazides, the latter undergo heterocyclization in the presence of sodium hydroxide with the formation of the known 5-R-2,4-dihydro-3H-1,2,4-triazole-3-thiones. 1H NMR spectra were studied, analyzed, and regularities of splitting of characteristic protons in functionalized azoles were established. Conducted microbiological screening was showed that 5-R-2-amino-1,3,4-thiadiazoles, 4-cycloalkanecarbonyl-3-(amino-,phenyloxo-(thio)methyl-1,5-dihydro-4H-1,2,4-triazole-5-thiones and 5-R-2,4-dihydro-3H-1,2,4-triazole-3-thione were less effective a","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"100 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"73608315","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Y. Serdiukova, O. Kolisnyk, Т. О. Tomarovska, S. M. Poluian, Z. Shovkova, O. H. Pohosian
{"title":"Validation of Amoxicillin iodometric procedure in quantitative analysis of pure substance and medical preparation","authors":"Y. Serdiukova, O. Kolisnyk, Т. О. Tomarovska, S. M. Poluian, Z. Shovkova, O. H. Pohosian","doi":"10.14739/2409-2932.2022.1.251985","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.1.251985","url":null,"abstract":"The aim of the work is to validate a simple and rapid iodometric procedure for the quantitative determination of amoxicillin in pure substance and medicinal preparation using potassium caroate as analytical reagent.\u0000Materials and methods. The procedure involves the use of potassium caroate (KHSO5) as an oxidant. The assay is based on the quantitative penicillin oxidation by KHSO5 to the corresponding S-oxide. The interaction between amoxicillin and analytical reagent is stoichiometric. Indirect iodometric method is used for the quantitative determination of amoxicillin main substance. The validation procedure was performed according to the State Pharmacopeia of Ukraine.\u0000Results. The precision, accuracy, limit of detection (LOD), and limit of quantitation (LOQ) are accepted over the concentration range of 80–120 % with a correlation coefficient of 0.999. LOD and LOQ were found to be 4.91 % and 14.73 % for amoxicillin pure substance respectively. The precision calculated as the relative standard deviation (RSD) was less than 0.8 % and accuracy (δ, relative error) was better than 0.4 %. The proposed method was validated statistically and through recovery studies. For Amoxicillin medical preparation RSD ≥1.93 % and δ ≥ 1.62 %.\u0000Conclusions. The obtained data showed acceptable agreement with the certificate results, so the proposed procedure can be used for the assay of amoxicillin in medicinal preparation.","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"48 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90734561","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Clinical and pathogenetic aspects of formation, early diagnosis, and medicated correction of cardiorenal disorders in men with hypertension against the background of purine metabolism disturbance","authors":"O. Dudko","doi":"10.14739/2409-2932.2022.1.246775","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.1.246775","url":null,"abstract":"Aim: to review literary sources and analyse the modern view of the mechanisms of development of kidney and heart damage in patients with combination of hypertension (HP) and hyperuricemia and methods of their medicated correction.\u0000Materials and methods. A review of the scientific literature for the last 10 years was done. It demonstrates that today high levels of uric acid (UA) are considered not only as a consequence of deteriorating renal function, but also as one of the factors of renal damage. The role of the kidneys in the pathogenesis and development of hypertension is the subject of a lively debate, whose significance is determined by the presence of a long period of latent renal dysfunction. According to the literature, in patients with essential hypertension, a direct correlation was found between the uric acids level and the left ventricular diastolic dysfunction (LVDD). Early diagnosis of heart lesions is possible using speckle-tracking echocardiography, which is an innovative technology for studying myocardial deformation, allowing subclinical diagnosis of heart muscle lesions. This technique is informative in hypertension even in the absence of hypertrophy and LVDD. The article also elucidates modern methods for diagnosing kidney damage against the background of hypertension, in particular, lipocalin associated with neutrophil gelatinase (NGAL). However, the significance of this biomarker in impaired renal function under conditions of hyperuricemia has not been studied. According to the literature, cystatin C is a marker of early diagnosis of cardiovascular events and a marker of renal glomerular function in the absence of an increase in serum creatinine levels. The role of this marker has been proven for many diseases of the kidneys and the cardiovascular system; however, there are no data on their definition as markers of damage to the heart and kidneys in hypertension in conditions of hyperuricemia.\u0000Conclusions. The identification of causal relationships and mechanisms of complications in hypertensive patients with purine metabolism disturbance needs further study. Therefore, early diagnosis of structural and functional changes in the main target organs (in particular, the heart and kidneys) and the determination of biochemical markers (NGAL, cystatin C) to identify their functional disturbances at the preclinical stage are important.","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"28 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75024075","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Ozonation of 4-aminotoluene as a new method of synthesis of 4-aminobenzaldehyde – an intermediate for the production of anti-tuberculosis drugs","authors":"A. Halstian, A. S. Вushuiev, Ye. Yu. Vasylenko","doi":"10.14739/2409-2932.2022.1.249620","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.1.249620","url":null,"abstract":"Solutizon is an original anti-TB drug that is effective in resisting mycobacteria to other anti-TB drugs, which is obtained by the interaction of thiosemicarbazone 4-aminobenzaldehyde and sodium oxymethylene sulfonate. 4-Aminobenzaldehyde is synthesized by redox conversion of 4-nitrotoluene in the presence of sodium polysulfide. The reaction is carried out in boiling alcohol, and 4-aminobenzaldehyde is separated after steam distillation with a yield of 40–50 %. However, today this method loses its practical, environmental and economic attractiveness, as it has significant disadvantages – low product yield, high reaction temperature (80–120 °C), the formation of sulfur-containing wastewater. Therefore, the development of low-temperature, environmentally friendly methods for obtaining 4-aminobenzaldehyde is an urgent task.\u0000The aim of the work is to study the kinetic features and mechanism of the liquid-phase reaction of ozone with 4-aminotoluene to create a new low-temperature, environmentally friendly method for the synthesis of 4-aminobenzaldehyde.\u0000Materials and methods. Sigma acetic anhydride of сh.р. qualification was used for the experiments. 4-Aminotoluene company “Sinbias” qualification “сh.р.”; 4-Acetamidotoluene and its derivatives were used chromatographically pure. Acetates of metals of qualification “сh.р.”, potassium bromide of qualification “pharmacopoeial” were used without additional purification. Continuous control of the current ozone concentration and recording the results in the form of a kinetic curve was carried out when passing ozone-containing gas through the container of the spectrophotometer “SF-46 LOMO” at a certain wavelength of a monochromatic light source. The results of the analysis were recorded using the KSP-4 potentiometer included in the spectrophotometer optical density reference circuit. This device automatically compensated the photocurrent by recording its value. The scale KSP-4 was calibrated in units of optical density, and the conversion into absolute ozone concentration was carried out according to the Lambert-Ber equation using molar extinction coefficients. Relative analysis error ≤5 %. At the optical stroke length of the container 10 ÷ 100 mm, the sensitivity of the device was ~10-7mol·l-1 ozone.\u0000Results. The kinetic features and mechanism of the liquid-phase reaction of ozone with 4-aminotoluene have been studied. It is shown that the developed catalytic system Mn(II)-KBr-H2SO4-Ac2O significantly increases the depth, rate, and selectivity of oxidation of 4-aminotoluene and the main reaction product is 4-aminobenzaldehyde in the form of the corresponding benzylidenediacetate with a yield of 69.5 %. The active particle responsible for the inclusion of the substrate in the oxidation of the methyl group in the presence of manganese (II) acetate and potassium bromide is manganese bromide ion radical (Mn(II)Br•), which is more active than Mn (III) and therefore more high-speed initiates oxidation by the meth","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"18 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81904030","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
{"title":"Detection of atomoxetine and its metabolites in the urine by thin-layer chromatography and mass spectrometry","authors":"S. A. Karpushyna, S. V. Baiurka, T. Tomarovska","doi":"10.14739/2409-2932.2022.1.252070","DOIUrl":"https://doi.org/10.14739/2409-2932.2022.1.252070","url":null,"abstract":"The aim of the study was the detection of atomoxetine and its biotransformation products in the urine under TLC screening conditions and identification of the metabolites using mass spectrometry method.\u0000Materials and methods. The volunteer’s urine samples after taking a single therapeutic dose of atomoxetine (2 capsules of 60 mg each of Strattera®) were studied. Sample preparation included diluting acid hydrolysis followed by the native compound and metabolites extraction with chloroform from the saturated solution of ammonium sulfate at pH of 11–12. Thin-layer chromatography studies of the extracts were carried out in 18 mobile phases including those proposed by The International Association of Forensic Toxicologists for general drug screening, and those widely used in forensic toxicological studies. The color reactions were carried out using a range of chromogenic reagents. A Varian 1200 L mass spectrometer (Netherlands) equipped with a dual quadrupole mass analyzer was applied for analysis of the eluates from chromatograms. Identification was undertaken at the direct introduction of the sample into the ion chamber, electron-impact ionization (70 eV), and full ion scanning mode.\u0000Results. The spot of the native drug on the chromatogram was identified by the Rf, value. Two atomoxetine biotransformation products were identified by the molecular weights that correspond to the molecular ion peaks in the mass spectra.\u0000Conclusions. Atomoxetine and its biotransformation products were detected in the urine under TLC screening conditions and identified using mass spectrometry method. Chromatographic mobility of the native compound, hydroxyatomoxetine, and dihydroxyatomoxetine in the TLC screening systems as well as the results of their visualization using chromogenic reagents applied for toxicological drug screening in the systematic toxicological analysis have been determined.","PeriodicalId":10800,"journal":{"name":"Current issues in pharmacy and medicine: science and practice","volume":"76 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2022-03-15","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"83850195","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}