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This diploma thesis deals with the retrieval of the content of tin in environmental media, the circulation in them and possibilities of the determination of tin in the environment. Summarizes available information on the properties of tin and its compounds, the occurrence and circulation of tin in environmental and determination of tin in environmental media, attention is paid to the determination of total tin content using method of ET-AAS. The experimental part is focused on optimization methods of determination for the ET AAS and selection of a suitable extraction procedure for determination of total tin content in soils and sediments. The best procedure for the determination of tin in the ET-AAS was applied to samples of soil, sediment and water. As the optimum matrix modifier was chosen the solution of Pd (NO3)2 in 5% ascorbic acid, the optimum pyrolysis temperature was 1400 °C and atomization temperature 2400 ° C. Neither of extraction procedures examined were found to be an appropriate procedure for the determination of tin in environmental samples and further work is necessary to optimize the method of separation.

This diploma thesis is focused on changes in the content of ?-glutamyl- S-vinylcysteine (GVC), the anti-nutritional factor present in narbon beans (Vicia narbonensis). The samples were collected at different stages of growth and separated into individual parts. There were prepared 32 extracts after freeze-drying and homogenisation in which it was determined the quantity of GVC by HPLC. The levels of GVC at different developmental stages were influenced by climatic conditions during growth, mainly by temperature and precipitation. The results obtained were compared with data published previously in the literature. The highest content of GVC was found in the seeds of narbon beans, especially at early stages of growth. Surprisingly, no GVC was detected in other parts of narbon beans (stems, leaves, beans, and roots).

The theoretical part of this master’s thesis is mainly focused on the physical and chemical properties of chromium, its toxicity and possibility of entering of various forms of chromium into the environment. There are also described the most common analytical methods for determination of chromium in water, including ways of modification and preconcentration water samples. The aim of experimental part is the optimalization and assessing the conditions spectrophotometric determination of Cr(III) by selected organic reagents (chromazurol S, eriochromcyanine R, 4-(2-thiazolylazo)resorcinol) and their comparison with the determination of total chromium, as Cr(III), using atomic absorption spectrometry with electrothermic atomization. The analytical procedure for spectrophotometric determination of chromium with chromazurol S, which was found to be most suitable and ET-AAS, were applied to real water samples.

Объектами исследования служили фармацевтическая субстанция «Аргамид» и готовая лекарственная форма 1% крем «Аргамид» на основе серебряной соли сульфадимидина (Приоритетная справка на выдачу патента № 2015153574 от 14.12.2015). Данная соль и лекарственные средства на ее основе были разработаны на базе кафедры фармации УГМУ с целью обеспечения российского фармацевтического рынка эффективными антибактериальными и ранозаживляющими лекарственными препаратами отечественного производства согласно стратегии развития фармацевтической промышленности «ФАРМА-2020». Цель работы: разработка и валидация методик количественного определения серебра в исследуемых лекарственных средствах. Анализ литературных данных показал, что оптимальным методом определения серебра является метод осадительного титрования с потенциометрической индикацией конечной точки титрования. При этом, учитывая содержание серебра в анализируемых лекарственных средствах, для его определения в субстанции был выбран метод роданометрического, а в готовой лекарственной форме – йодометрического титрования. Для анализируемых лекарственных средств были подобраны оптимальные условия пробоподготовки: масса навески, концентрация растворителя; время и температура обработки пробы. В качестве индикаторного вместо дорогостоящего импортного серебряного дискового электрода использовали отечественный толстопленочный серебросодержащий электрод. Положительные результаты валидационной оценки разработанных методик, проведенной согласно требованиям Государственной Фармакопеи РФ XIII изд., позволяют считать их приемлемыми и рекомендовать для включения в проекты фармакопейных статей на исследуемые лекарственные средства. Контроль содержания серебра по разработанным методикам не требует дорогостоящего оборудования, привлечения высококвалифицированного персонала, отличается относительно коротким временем анализа, а, следовательно, может применяться испытательными лабораториями предприятия в процессе производства и центрами контроля качества во время обращения на фармацевтическом рынке исследуемых лекарственных средств. / The objects of study were pharmaceutical substance "Argamid" and finished dosage form of 1% cream "Argamid" based on silver salt sulfadimidine (Priority reference patent number 2015153574 from 14.12.2015). This salt and drugs based on it have been developed at the Department of Pharmacy UGMU to ensure that the Russian pharmaceutical market effective antibacterial and wound healing medicines domestic production according to the strategy of development of the pharmaceutical industry "Pharma 2020". Objective: Development and validation of methods of quantitative determination of silver in the investigational medicinal product. Analysis of published data shows that the best method of determining silver is the method of precipitation titration with potentiometric indication end point. However, given the content of silver in the analyzed medicaments for identification substance rodanometricheskogo method was selected, and in the final dosage form - iodometric titration. optimal conditions for sample preparation were selected to be analyzed drugs: sample weight, the concentration of solvent; Sample processing time and temperature. As an indicator instead of expensive imported silver disk electrode used domestic thick-film silver-electrode. Positive results validation assessment developed techniques conducted in accordance with the requirements of the RF State Pharmacopoeia XIII ed., Allow us to consider them acceptable and recommended for inclusion in the draft articles on the pharmacopoeia investigational medicinal products. Control of the silver content by developed techniques does not require expensive equipment, highly skilled personnel, has a relatively short analysis time, and, therefore, can be applied testing laboratories of the enterprise in the production process and quality control center during handling in the pharmaceutical market of investigational medicinal products.

Die Systematische Toxikologische Analyse (STA) stellt auf Grund der großen Vielfalt und der ständigen Zunahme an toxikologisch relevanten Substanzen eine der größten Herausforderungen in der chemischen Analyse dar. In der vorliegenden Arbeit wurde daher die Eignung der Flüssigchromatographie in Kombination mit der Hybrid-Quadrupol-Flugzeitmassenspektrometrie (LC-QTOF-MS) für diesen Zweck untersucht. Dazu wurden eine Datenbank mit über 7360 und eine CID-Spektrenbibliothek mit mehr als 2720 toxikologisch relevanten Substanzen erstellt und geeignete Probenvorbereitungsmethoden entwickelt. Die Erprobung der Methoden erfolgte an dotierten Blut- und Haarproben. Hierbei zeigte sich, dass die Analyse im Auto-MS/MS-Modus (Messzyklen von MS- und MS/MS-Spektren) eine Identifizierung basischer Substanzen mittels CID-Spektren zwischen 0,5 und 2 ng/ml im Blut ermöglichte. Die Nachweisgrenzen der für 24 Wirkstoffe validierten Methode in Haaren lagen bei 3 bis 15 pg/mg. Die Eignung der LC-QTOF-MS zur STA von Haarproben wurde an 30 Drogentodesfällen und 60 Todesfällen mit bekannter chronischer Medikamenteneinnahme zu Lebzeiten sowie an 77 Blutproben nachgewiesen. Für die Suche nach Metaboliten wurde ein Metaboliten-Tool entwickelt. In der praktischen Anwendung auf Datenfiles von Blut- und Haarproben erwies sich das Tool als wertvolles Hilfsmittel zur Identifizierung unbekannter Peaks und zur Bestätigung von Suchergebnissen in der Datenbank. Zur automatischen Konzentrationsabschätzung identifizierter Substanzen wurde ein Tool „Estimate Concentration“ geschaffen. Die Überprüfung des Verfahrens an realen Blut- und Haarproben durch Vergleich mit HPLC-DAD- und GC-MS-Ergebnissen wies eine gute Übereinstimmung der Konzentrationen auf. Insgesamt zeigten die Untersuchungen, dass die LC-QTOF-MS zurzeit die am besten geeignete Methode für die STA darstellt. Auch bei einem erst später aufkommenden Verdacht kann eine gezielte Suche in dem bereits gemessenen Datenfile durchgeführt werden. / Due to the large variety and the steady increase of toxicologically relevant substances, systematic toxicological analysis (STA) is one of the most difficult tasks in analytical chemistry and, therefore, a steady topic of research and methodical improvement. For this reason, the suitability of liquid chromatography in combination with hybrid quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) for STA was investigated. For this purpose, a database of more than 7360 and a CID spectra library of more than 2720 toxicologically relevant substances and suitable methods for sample preparation were developed. The application was evaluated at spiked blood and hair samples. It was found that the analysis in Auto-MS/MS mode (alternating measurement cycles of MS and MS/MS spectra) allowed substance identification in blood using CID spectra between 0.5 and 2 ng/ml for basic substances. The detection limits of the validated method in hair ranged from 3 to 15 pg/mg for 24 drugs. The suitability of LC-QTOF-MS for STA was tested for hair samples from 30 drug-related death cases and from 60 death cases with known chronic medication as well as for 77 blood samples. For the search of metabolites, a metabolite tool was developed. In the practical application to data files from blood and hair samples, the tool proved to be very helpful for identification of unknown peaks and for confirmation of results obtained only from the database without CID spectra. A tool "Estimate Concentration" was created for automatic estimation of concentrations of identified substances. The application to real blood and hair samples and the comparison of the concentrations with results from HPLC-DAD and GC-MS showed good agreement. Overall, these investigations showed that LC-QTOF-MS is currently the most favorable method for STA. Because of the comprehensive registration of all substances in a sample, the data files can be checked for the presence of certain poisons even later without new measurements.