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Polybrominated diphenyl ethers belong among the persistent compounds, which have been classified as priority organic pollutants. In environmental compartments are observed in the past decade. Polybrominated diphenyl ethers are detected in abiotic and biotic matrices. For this dissertation were chosen the matrixes from seats of fire, taken in various localities of the Czech Republic and Slovakia. Their analysis should demonstrate whether they in these specific matrices remain. There were examined following polybrominated diphenyl ether congeners: BDE- 28, 47, 99, 100, 153, 154, 183. For their isolation from the matrix were used three different extraction techniques, namely ultrasonic extraction, microwave extraction and pressurized solvent extraction. For the determination was chosen method of GC / ECD. In this dissertation are also described basic chemical, physical and environmental properties of BDE, including other analytical methods that can be used to determine polybrominated diphenyl ethers in environmental compartments.

The compound 3-quinuclidinyl benzylate (agent BZ) belongs to the group of incapacitating warfare agents with anticholinergic activity. Today, for its ability to induce functional cognitive impairment (i.e. coordination and memory disorders), the agent BZ is used mainly for scientific purposes in the study of Alzheimer's disease. Despite this fact, its pharmacokinetics has not been fully examined yet. In order to determine the agent BZ in biological material, LC-MS / MS method and sample preparation procedure for body fluids (plasma, bile) and tissues (brain, liver, kidneys) were developed, optimized and validated. The sample preparation procedure for body fluid employed solid phase extraction using a C18 column eluted with methanol and for body tissues it was precipitation with acetonitrile. The chromatographic separation was performed on Gemini NX-C18 reverse phase column (150 × 4.6 mm, 5 μm). The mobile phase consisted of a 10mM solution of ammonium acetate at pH 11 and methanol in a ratio of 30 : 70. Elution of the analytes was performed under isocratic elution. The total analysis time was 5 minutes. Mass spectrometric detection was performed by a linear ion trap using electrospray ionization. Sample preparation procedure and chromatographic analysis methods were successfully applied to real...

<p>Glavni cilj istraživanja ove doktorske disertacije je bio valorizacija sporednog proizvoda žalfije (Salvia officinalis L.) iz fabrike čaja za dobijanje visoko-vrednih ekstrakata željenih osobina koji bi imali primenu u gotovim proizvodima prehrambene, kozmetičke i farmaceutske industrije.<br />U cilju ekstrakcije polifenolnih jedinjenja su primenjene konvencionalne (maceracija) i savremene (ultrazvučna ekstrakcija, mikrotalasna ekstrakcija i ekstrakcija subkritičnom vodom) ekstrakcione tehnike. U postupaku maceracije je optimizovana koncentracija etanola u ekstragensu, dok je za optimizaciju savremenih ekstrakcionih tehnika primenjen eksperimentalni dizajn i metoda odzivne povr&scaron;ine. Prinos polifenola (ukupnih fenola i ukupnih flavonoida) i antioksidativna aktivnost određena različitim in vitro testovima su bili ispitivani odzivi. Za svaki od navedenih ekstrakcionih postupaka je ispitivan uticaj glavnih ekstrakcionih parametara: ultrazvučna ekstrakcija (temperatura, vreme ekstrakcije i snaga ultrazvuka), mikrotalasna ekstrakcija (koncentracija etanola, vreme ekstrakcije i odnos rastvarač-droga) i ekstrakcija subkritičnom vodom (temperatura, vreme ekstrakcije i koncentracija HCl u ekstragensu). Tečni ekstrakti dobijeni ultrazvučnom, mikrotalasnom i subkritičnom ekstrakcijom su pokazali izuzetno visoku antioksidativnu aktivnost određenu &bdquo;hvatanjem&ldquo; DPPH i O2∙- radikala i kapacitetom redukcije Fe3+ jona i imali su znatno veći sadržaj polifenola u odnosu na ekstrakte dobijene maceracijom.<br />U cilju ekstrakcije terpenoidnih jedinjenja su primenjeni postupci Soxhlet ekstrakcije, destilacije vodenom parom i ekstrakcije superkritičnim CO2. Postupak superkritične ekstrakcije je optimizovan metodom odzivne povr&scaron;ine i optimalni uslovi ekstrakcije su bili pritisak 290 bar, temperatura 55˚C i protok CO2 od 0,4 kg/h, dok su predviđene i eksperimentalne vrednosti prinosa ekstrakcije bile 8,90 i 8,84%. Hemijskom analizom lipofilnih ekstrakata i etarskog ulja je utvrđeno da su oksidovani monoterpeni (&alpha;-tujon i kamfor), oksidovani seskviterpeni (viridiflorol) i polifenolni diterpeni (epirosmanol) dominantna jedinjenja prisutna u ovim uzorcima.<br />Tečni ekstrakti žalfije dobijeni konvencionalnim i savremenim ekstrakcionim tehnikama su spray drying tehnikom osu&scaron;eni u cilju prevođenja u stabilniju formu suvog ekstrakta. Suvim ekstraktima su određene fizičko-hemijske osobine (hemijski sastav, sadržaj vlage, higroskopnost, moć rehidratacije, WAI i WSI) i biolo&scaron;ka aktivnost (antimikrobna i antioksidativna aktivnost) i procenjena je njihova mogućnost primene u prehrambenoj i farmaceutskoj industriji.</p> / <p>The main aim of this dissertation was valorization of sage (Salvia officinalis L.) by-product from filter-tea factory for recovery of high-value extracts with desirable properties for application in food, cosmetics and pharmaceutical products.<br />Conventional (maceration) and novel (ultrasound-assisted, microwave-assisted and subcritical water extraction) extraction techniques were applied for polyphenols recovery. Ethanol concentration was optimized in maceration process, while experimental design and response surface methodology were applied for optimization of novel extraction techniques. Polyphenols yield (total phenols and total flavonoids) and antioxidant activity, determined by various in vitro assays, were investigated responses. Influence of main process parameters was determined for each technique: ultrasound-assisted extraction (temperature, extraction time and ultrasonic power), microwave-assisted extraction (ethanol concentration, extraction time and sample-solvent ratio) and subcritical water extraction (temperature, extraction time and HCl concentration in solvent). Liquid extracts obtained by novel extraction technique exhibited higher antioxidant activity determined by scavenging of DPPH and O2∙- radicals and reduction of Fe3+ and also provided higher polyphenols yield comparing to extracts obtained by maceration. Soxhlet extraction, hydrodistillation and supercritical fluid extraction were applied for terpenoids recovery. Supercritical fluid extraction process was optimized by response surface methodology and optimal conditions were pressure of 290 bar, temperature of 55˚C and CO2 flow rate of 0.4 kg/h, while predicted and experimentally obtained values of total extraction yield at these conditions were 8.90 i 8.84%, respectively. According to chemical analysis, the most abundant compounds in lipid extracts and essential oil were oxygenated monoterpenes (&alpha;-thujone and camphor), oxygenated sesquiterpenes (viridiflorol) and diterpene polyphenols (epirosmanol).<br />Sage liquid extracts obtained by conventional and novel extraction techniques were spray dried in order to obtain dry extract form. Physico-chemical properties (chemical profile, moisture content, hygroscopicity, rehydratation time, WAI and WSI) and biological activity (antimicrobial and antioxidant activity) were determined in dry extracts and their potential application in food and pharmaceutical formulations was discussed.</p>

The impact and dynamics of Internet-based resources for Arabic-speaking users is increasing in significance, depth and breadth at highest pace than ever, and thus requires updated mechanisms for computational processing of Arabic texts. Arabic is a complex language and as such requires in depth investigation for analysis and improvement of available automatic processing techniques such as root extraction methods or text classification techniques, and for developing text collections that are already labeled, whether with single or multiple labels. This thesis proposes new ideas and methods to improve available automatic processing techniques for Arabic texts. Any automatic processing technique would require data in order to be used and critically reviewed and assessed, and here an attempt to develop a labeled Arabic corpus is also proposed. This thesis is composed of three parts: 1- Arabic corpus development, 2- proposing, improving and implementing root extraction techniques, and 3- proposing and investigating the effect of different pre-processing methods on single-labeled text classification methods for Arabic. This thesis first develops an Arabic corpus that is prepared to be used here for testing root extraction methods as well as single-label text classification techniques. It also enhances a rule-based root extraction method by handling irregular cases (that appear in about 34% of texts). It proposes and implements two expanded algorithms as well as an adjustment for a weight-based method. It also includes the algorithm that handles irregular cases to all and compares the performances of these proposed methods with original ones. This thesis thus develops a root extraction system that handles foreign Arabized words by constructing a list of about 7,000 foreign words. The outcome of the technique with best accuracy results in extracting the correct stem and root for respective words in texts, which is an enhanced rule-based method, is used in the third part of this thesis. This thesis finally proposes and implements a variant term frequency inverse document frequency weighting method, and investigates the effect of using different choices of features in document representation on single-label text classification performance (words, stems or roots as well as including to these choices their respective phrases). This thesis applies forty seven classifiers on all proposed representations and compares their performances. One challenge for researchers in Arabic text processing is that reported root extraction techniques in literature are either not accessible or require a long time to be reproduced while labeled benchmark Arabic text corpus is not fully available online. Also, by now few machine learning techniques were investigated on Arabic where usual preprocessing steps before classification were chosen. Such challenges are addressed in this thesis by developing a new labeled Arabic text corpus for extended applications of computational techniques. Results of investigated issues here show that proposing and implementing an algorithm that handles irregular words in Arabic did improve the performance of all implemented root extraction techniques. The performance of the algorithm that handles such irregular cases is evaluated in terms of accuracy improvement and execution time. Its efficiency is investigated with different document lengths and empirically is found to be linear in time for document lengths less than about 8,000. The rule-based technique is improved the highest among implemented root extraction methods when including the irregular cases handling algorithm. This thesis validates that choosing roots or stems instead of words in documents representations indeed improves single-label classification performance significantly for most used classifiers. However, the effect of extending such representations with their respective phrases on single-label text classification performance shows that it has no significant improvement. Many classifiers were not yet tested for Arabic such as the ripple-down rule classifier. The outcome of comparing the classifiers' performances concludes that the Bayesian network classifier performance is significantly the best in terms of accuracy, training time, and root mean square error values for all proposed and implemented representations.

<p>Glavni cilj istraživanja ove doktorske disertacije je bio ispitivanje hemijskog sastava lista koprive (Urtica dioica L.), primena različitih ekstrakcionih tehnika radi izolovanja aktivnih jedinjenja iz lista, ispitivanje njihovog hemijskog sastava, kao i formulacija prehrambenog proizvoda dodavanjem ekstrakta lista.<br />U cilju ispitivanja sastava lista primenjene su različite analitičke tehnike kao &scaron;to su GC/MS, GC/FID, UHPLC-DAD/MS/MS, ICP-OES, živin analizator, AAS i spektrofotometrija. Pri tome je dokazano prisustvo različitih klasa hemijskih jedinjenja među kojima su pigmenti (hlorofil i karotenoidi), terpenoidi, fenolni i polifenolna jedinjenja, vitamini (vitamin C i vitamini B grupe) i masne kiseline.<br />Za izdvajanje biolo&scaron;ki aktivnih jedinjenja primenjene su različite tehnike ekstrakcije, kao &scaron;to<br />su: maceracija, Soxhlet ekstrakcija, ultrazvučna (UAE), mikrotalasna (MAE) i superkritična<br />ekstrakcija (SFE). Preliminarne UAE ekstrakcije su pokazale da je voda bila najpogodnija kao rastvarač, odnosno da su vodeni ekstrakti pokazali najveću antioksidativnu aktivnost, kao i najveći sadržaj ukupnih fenola (TPC) i flavonoida (TFC). Pripremljeni vodeni ekstrakti su dalje ispitivani u pogledu sastava, antioksidativne, citotoksične i antimikrobne aktivnosti, gde su rezultati međusobno poređeni kako bi se odabrala najpogodnija ekstrakciona tehnika. Kod SFE je ispitan uticaj uslova ekstrakcije, odnosno pritiska i temperature na<br />sastav dobijenih ekstrakata i njihovu biolo&scaron;ku aktivnost (antioksidativna i citotoksična). Iscrpljeni list korpive je nakon SFE bio ekstrahovan primenom UAE i MAE tehnika, gde su dobijenim ekstraktima utvrđeni sastav i biolo&scaron;ka aktivnost. Nakon svih ispitivanja, MAE ekstrakt i suvi list koprive su dalje primenjeni u formulaciji prehrambenog proizvoda (hleba), gde je variran njihov sadržaj, dok su analizirani sastav, tehnolo&scaron;ki kvalitet hleba, kao i biolo&scaron;ka aktivnost (antioksidativna i citotoksična).</p> / <p>The main goals of this PhD thesis were investigation<br />of chemical composition of stinging nettle leaves<br />(Urtica dioica L.), application of different extraction<br />techniques for isolation of biologically active<br />compounds from leaves, investigation of their<br />chemical composition and formulation of food<br />product with addition of dried leaves and/or its extract.<br />For those purposes, different analytical techniques<br />were applied, i.e. GC/MS, GC/FID, UHPLCDAD/<br />MS/MS, ICP-OES, direct mercury analyzer,<br />AAS and spectrophotometry. Different classes of<br />chemical compounds were detected and identified,<br />such as: pigments (chlorophylls and carotenoids),<br />terpenoids, phenolic and polyphenolic compounds,<br />vitamins (vitamin C and B group) and fatty acids.<br />For the purpose of isolation of biologically active<br />compounds, different extraction techniques were<br />applied: maceration, Soxhlet extraction, ultrasound<br />(UAE), microwave (MAE) and supercritical (SFE)<br />extraction. Preliminary conducted extraction, as well<br />as total phenolics (TPC) and flavonoids (TFC)<br />contents, showed that water was the most suitable<br />solvent for further course of investigation. Water<br />extracts were further analyzed regarding their<br />chemical composition, antioxidant, cytotoxic and antimicrobial activities. Obtained result were<br />compared in order to select the most efficient<br />extraction technique. In the case of SFE, influence of<br />pressure and temperature on extraction yield,<br />composition and biological activity of prepared<br />extracts were monitored. Exhausted plant material<br />after SFE was used for further MAE extraction, while<br />obtained extracts were analyzed to investigate<br />chemical composition and biological activity.<br />After conducted experiments and analysis, MAE<br />extract was used for formulation of food product<br />(bread) where it was added in different amounts in<br />combination of without dried leaves. Obtained<br />products were analyzed regarding their chemical<br />composition, technological requirements and<br />biological activity.</p>

O objetivo do presente deste trabalho foi avaliar a toxicidade aguda, crônica e a genotoxicidade sobre E. andrei causadas por solo recém-contaminado com óleo lubrificante usado e após biorremediação por diferentes estratégias, após 22 meses, e paralelamente ao estudo de ecotoxicidade, foi conduzida uma investigação comparativa de três métodos de extração de HTP e HPA de solos para análise cromatográfica. A comparação das técnicas de extração evidenciou que para HTP, a técnica de extração acelerada por solvente-ASE foi a que melhor recuperou n-alcanos; já para as frações HRP e MCNR as técnicas soxhlet e micro-ondas-MARS não apresentaram diferenças significativas e foram melhores que ASE. Para HPA, a técnica de extração por soxhlet foi a que apresentou melhor recuperação em todos os solos. O teste de mortalidade apresentou, aos 14 dias, taxas crescentes de mortalidade de 10 6%, 20 0%, 73 25%, 93 12% e 100 0% para amostras de CONT (solo controle, sem contaminação artificial), BIOS (solo contaminado com 5% de OLU e biorremediado por bioestimulo), BIOA1 (solo contaminado com 5% de OLU e biorremediado por bioestimulo + bioaumento com adição de 10% de RSU maturado), e BIOA2 (solo contaminado com 5% de OLU e biorremediado por bioestimulo + bioaumento com adição de 10% de RSU semi-maturado) e OLU (solo contaminado com 5% de OLU), respectivamente. Aos 28 dias, entretanto, BIOS e OLU apresentaram taxas de mortalidade de 97 % 6 % e de 100 % 0 % respectivamente, valores estes significativamente superiores ao CONT. Foram observadas deformações anatômicas nos indivíduos mantidos em BIOS e OLU, assim como diminuição da biomassa em todas as amostras, evidenciando efeitos crônicos. O teste de reprodução, aos 28 dias, foram observadas grandes quantidades de indivíduos jovens nos solos biorremediados e recém-contaminado. No entanto, aos 56 dias houve uma diminuição dessas formas e o controle (CONT) exibiu uma quantidade maior de formas juvenis. O teste de densidade e viabilidade celular mostrou ser indicador sensível para toxicidade crônica apresentando queda nos solos BIOS e OLU em relação ao CONT com diferenças significativas (p <0.05). Não foram observados micronúcleos nos solos em estudo. Tal observação reforça a necessidade de testes de ecotoxicidade para avaliar a real eficácia de tecnologias de tratamento. / The aim of this study was to evaluate this acute toxicity, chronic and genotoxicity on E. andrei caused by freshly contaminated soil with used lubricating oil and after bioremediation by different strategies, after 22 months, and alongside ecotoxicity study, we conducted a comparative study of three methods of extraction and HTP HPA soil for chromatographic analysis. Comparison of extraction techniques for HTP showed that the technique of accelerated solvent extraction-ASE had the best recovery of n-alkanes, whereas for fractions and HRP MCNR soxhlet techniques and microwave-MARS and no significant differences were better than ASE. For HPA, the soxhlet extraction technique showed the best recovery in all soils. The mortality test showed , at the 14th day, growing mortality rates of 10 6% 20 0%, 73 25% 93 12% and 100 0% for samples CONT (ground control without contamination artificial ), BIOS (soil contaminated with 5% of OLU and bioremediated for biostimulation) BIOA1 (soil contaminated with 5% of OLU and bioremediated for biostimulation + bioaugmentation by adding 10% of MSW matured) and BIOA2 (soil contaminated with 5% bioremediated of OLU and for biostimulation + bioaugmentation by adding 10% of MSW semi-matured) and OLU (soil contaminated with 5% OLU), respectively. At the 28th day, however, OLU BIOS and mortality rates were 97% 6% and 100% 0%, respectively, values which are significantly higher than CONT. Anatomical deformations have been observed in individuals kept in BIOS and OLU, as well as decreased biomass in all samples, suggesting chronic effects. The reproduction test, at the 28th day, were found large quantities of juveniles in bioremediated soils and freshly contaminated soil. However, at the 56th day there was a decrease of these forms and control (CONT) exhibited a greater amount of juveniles. The >test> density and cell viability test showed to be a sensitive indicator for chronic toxicity in soils having decrease BIOS and OLU compared to CONT with significant differences (p <0.05). No micronuclei were observed in soils under study. This observation reinforces the need for ecotoxicity tests to assess the true efficacy of treatment technologies.

O objetivo do presente deste trabalho foi avaliar a toxicidade aguda, crônica e a genotoxicidade sobre E. andrei causadas por solo recém-contaminado com óleo lubrificante usado e após biorremediação por diferentes estratégias, após 22 meses, e paralelamente ao estudo de ecotoxicidade, foi conduzida uma investigação comparativa de três métodos de extração de HTP e HPA de solos para análise cromatográfica. A comparação das técnicas de extração evidenciou que para HTP, a técnica de extração acelerada por solvente-ASE foi a que melhor recuperou n-alcanos; já para as frações HRP e MCNR as técnicas soxhlet e micro-ondas-MARS não apresentaram diferenças significativas e foram melhores que ASE. Para HPA, a técnica de extração por soxhlet foi a que apresentou melhor recuperação em todos os solos. O teste de mortalidade apresentou, aos 14 dias, taxas crescentes de mortalidade de 10 6%, 20 0%, 73 25%, 93 12% e 100 0% para amostras de CONT (solo controle, sem contaminação artificial), BIOS (solo contaminado com 5% de OLU e biorremediado por bioestimulo), BIOA1 (solo contaminado com 5% de OLU e biorremediado por bioestimulo + bioaumento com adição de 10% de RSU maturado), e BIOA2 (solo contaminado com 5% de OLU e biorremediado por bioestimulo + bioaumento com adição de 10% de RSU semi-maturado) e OLU (solo contaminado com 5% de OLU), respectivamente. Aos 28 dias, entretanto, BIOS e OLU apresentaram taxas de mortalidade de 97 % 6 % e de 100 % 0 % respectivamente, valores estes significativamente superiores ao CONT. Foram observadas deformações anatômicas nos indivíduos mantidos em BIOS e OLU, assim como diminuição da biomassa em todas as amostras, evidenciando efeitos crônicos. O teste de reprodução, aos 28 dias, foram observadas grandes quantidades de indivíduos jovens nos solos biorremediados e recém-contaminado. No entanto, aos 56 dias houve uma diminuição dessas formas e o controle (CONT) exibiu uma quantidade maior de formas juvenis. O teste de densidade e viabilidade celular mostrou ser indicador sensível para toxicidade crônica apresentando queda nos solos BIOS e OLU em relação ao CONT com diferenças significativas (p <0.05). Não foram observados micronúcleos nos solos em estudo. Tal observação reforça a necessidade de testes de ecotoxicidade para avaliar a real eficácia de tecnologias de tratamento. / The aim of this study was to evaluate this acute toxicity, chronic and genotoxicity on E. andrei caused by freshly contaminated soil with used lubricating oil and after bioremediation by different strategies, after 22 months, and alongside ecotoxicity study, we conducted a comparative study of three methods of extraction and HTP HPA soil for chromatographic analysis. Comparison of extraction techniques for HTP showed that the technique of accelerated solvent extraction-ASE had the best recovery of n-alkanes, whereas for fractions and HRP MCNR soxhlet techniques and microwave-MARS and no significant differences were better than ASE. For HPA, the soxhlet extraction technique showed the best recovery in all soils. The mortality test showed , at the 14th day, growing mortality rates of 10 6% 20 0%, 73 25% 93 12% and 100 0% for samples CONT (ground control without contamination artificial ), BIOS (soil contaminated with 5% of OLU and bioremediated for biostimulation) BIOA1 (soil contaminated with 5% of OLU and bioremediated for biostimulation + bioaugmentation by adding 10% of MSW matured) and BIOA2 (soil contaminated with 5% bioremediated of OLU and for biostimulation + bioaugmentation by adding 10% of MSW semi-matured) and OLU (soil contaminated with 5% OLU), respectively. At the 28th day, however, OLU BIOS and mortality rates were 97% 6% and 100% 0%, respectively, values which are significantly higher than CONT. Anatomical deformations have been observed in individuals kept in BIOS and OLU, as well as decreased biomass in all samples, suggesting chronic effects. The reproduction test, at the 28th day, were found large quantities of juveniles in bioremediated soils and freshly contaminated soil. However, at the 56th day there was a decrease of these forms and control (CONT) exhibited a greater amount of juveniles. The >test> density and cell viability test showed to be a sensitive indicator for chronic toxicity in soils having decrease BIOS and OLU compared to CONT with significant differences (p <0.05). No micronuclei were observed in soils under study. This observation reinforces the need for ecotoxicity tests to assess the true efficacy of treatment technologies.

Conselho Nacional de Desenvolvimento Científico e Tecnológico / In this study, was optimization an analytical method for identification and quantification method of Polycyclic Aromatic Hydrocarbons (PAHs) in surface water and hospital effluent samples. High Performance Liquid Chromatography with Fluorescence Detection (HPLC-FLD), assisted by Solid Phase Extraction (SPE) and Dispersive Liquid-Liquid Microextraction (DLLME), was used. For SPE, the use of organic modifiers was necessary owing to the low solubility of PAHs, and employed 20% of acetonitrile as such. Factorial design was applied and the best results were: pH 5 for the samples and washing water. The SPE method was validated in Chromabond® C18 ec cartridges and recoveries ranged from 92.0 to 100.2% (RSD 0.2 to 5. 0%). The highest concentrations of PAHs using SPE were found in surface waters from the water course crossing the UFSM Campus (5.4 to 21.5 μg L-1). Using DLLME optimized by design of experiments, the best conditions were: pH 7, 0.2 mol L-1 NaCl, 100 μL of extractor solvent (carbon tetrachloride) and 500 μL of disperser solvent (acetone). The DLLME method was validated, providing recoveries ranging from 77.2 to 100.6% (RSD 0.9 to 10.2%) for surface water and 72.7 to 100.3% (RSD 1.9 to 8.9%) for hospital effluent samples. Using DLLME, the highest concentrations of PAHs were found in surface water samples (3.2 to 19.7 μg L-1). Employing both SPE and DLLME, the concentration of anthracene and pyrene were below the limit of quantification in all sampling points. By the environmental risk assessment naphthalene, 1-methylnaphthalene and phenanthrene showed moderate environmental risk. High environmental risk was found for fluorene, anthracene and pyrene. Heterogeneous photocatalysis and ozonation was examined as remediation method. A jacketed stirred tank reactor and ultraviolet irradiation were used for photocatalysis with TiO2 supported on polydimethylsiloxane. Owing to the low solubility of PAHs, it was necessary the addition of acetonitrile to the solutions (5% in aqueous solution, and 10% in surface water and hospital effluent). A factorial design was applied and the best rates of degradation was set as pH 9 and 35 °C (aqueous solution), and pH 7 and 30 °C (surface water and hospital effluent). First order kinetics was observed for photocatalytic degradation of PAHs in aqueous solution, and, zero order, in hospital effluent and surface water. The photocatalytic degradation subproducts were identified for anthracene, phenanthrene and naphthalene by GC-MS and the fragmentation routes were proposed. Semi-batch column type reactor was used by the ozonation. The best degradation rates of the analytes, in aqueous solution and in real samples, were observed at pH 9. The ozonation kinetics showed a first-order reaction for all samples and degradation times ranging from 5 to 15 minutes. / Neste trabalho fez-se a otimização de método analítico para identificação e quantificação de Hidrocarbonetos Policíclicos Aromáticos (HPAs) em amostras de águas superficiais e efluente hospitalar. Empregou-se Cromatografia Líquida de Alta Eficiência com detecção por Fluorescência (HPLC-FLD), Extração em Fase Sólida (SPE) e Microextração Líquido-Líquido Dispersiva (DLLME). Para a SPE, investigou-se o uso de modificadores orgânicos, devido a baixa solubilidade dos HPAs, e empregou-se 20% de acetonitrila como tal. Aplicou-se planejamento fatorial e os melhores resultados foram: pH 5 para amostras e água de lavagem. O método de SPE foi validado em cartuchos Chromabond® C18 ec e as recuperações variaram de 92,0 a 100,2% (RSD 0,2 a 5,0%). As maiores concentrações de HPAs, com SPE, foram em amostras de águas superficiais do córrego do Campus da UFSM (5,4 a 21,5 μg L-1). Para a DLLME, otimizada por planejamento de experimentos, as condições ótimas foram: pH 7, 0,2 mol L-1 de NaCl, 100 μL de solvente extrator (tetracloreto de carbono) e 500 μL de solvente dispersor (acetona). O método de DLLME foi validado e as recuperações variaram 77,2 a 100,6% (RSD de 0,9 a 10,2%) para amostras de água superficiais e, de 72,7 a 100,3% (RSD de 1,9 a 8,9%), para amostras de efluente hospitalar. As maiores concentrações de HPAs, por DLLME, obtiveram-se em amostras de águas superficiais (3,2 a 19,7 μg L-1). Empregando-se SPE e DLLME, as concentrações de antraceno e pireno ficaram abaixo do limite de quantificação em todos os pontos de amostragem. Na avaliação de risco ambiental, naftaleno, 1-metilnaftaleno e fenantreno apresentaram risco ambiental moderado. Alto risco ambiental foi evidenciado para fluoreno, antraceno e pireno. Como método de remediação aplicou-se fotocatálise heterogênea e ozonização. Na fotocatálise, empregou-se reator tanque agitado termostatizado, radiação ultravioleta e TiO2 suportado em polidimetilsiloxano. Devido à baixa solubilidade fez-se necessária a adição de acetonitrila à solução de HPAs (5% em solução aquosa e 10% em água superficial e efluente hospitalar). Aplicou-se planejamento fatorial e as melhores taxas de degradação obtiveram-se com pH 9 e 35 °C (solução aquosa) e, pH 7 e 30 °C (águas superficiais e efluente hospitalar). Foi observada cinética de primeira ordem para a degradação fotocatalítica dos HPAs em solução aquosa e de ordem zero em amostras de efluente hospitalar e águas superficiais. Os subprodutos de degradação fotocatalítica de antraceno, fenantreno e naftaleno foram identificados por GC-MS e propuseram-se rotas de fragmentação. Empregou-se um reator tipo coluna de semi-batelada no processo de ozonização de HPAs. As melhores taxas de degradação dos analitos em solução aquosa e em amostras reais foram observadas em pH 9. O estudo cinético evidenciou reações de primeira ordem para todas as amostras estudadas e os tempos de degradação variaram de 5 a 15 minutos nas condições otimizadas.

eDNA is a fast and popular method to collect information about species presence in the environment. eDNA is DNA that is collected from environmental samples, such as water, from DNA that is expelled from organisms interacting with their environment. eDNA is an effective way to find species with small populations and alien species. There are two ways to analyze eDNA, with high-throughput DNA sequencing methods and DNA metabarcoding or use of species-specific primers and PCR. In this study, we focus on the latter, designing species-specific primers for Burbot, Brown trout, and Atlantic Salmon, testing their validity in detecting eDNA of these species with functional PCR. We also evaluated eDNA collection methods, testing different scenarios in aquarium tanks with different number of dead and alive fishes. Primers and experimental setup such as use of different temperatures of the PCR reaction used in this study didn’t result in a functional PCR as determined by electrophoresis gel. There are some problems with the design of the PCR methods for eDNA since the purpose is to design methods that can identify certain species. However, future development of eDNA methods will probably include sequencing and not detection of PCR product sizes. eDNA methods will complete traditional trapping methods like net and electrofishing, but not replace them. / eDNA är en snabb och populär metod för att samla information om arters abundans i miljön. eDNA är DNA taget från miljö prover, så som vatten, från DNA som frigörs från organismer som intrigerar med deras miljön. eDNA är ett effektivt sätt att hitta arter med små populationer och främmande arter. De finns två olika sätt att analysera eDNA, med DNA-sekvenseringsmetoder med hög genomströmning och DNA-metabarkodning eller användning av artspecifika primrar och PCR. I denna studie fokuserade vi på den senare, designade artspecifika primers för lake, lax och öring, testa deras validitet vid detektering av eDNA hos dessa arter med funktionell PCR. Vi utvärderade också eDNA-insamlingsmetoder, testa olika scenarier i akvarietankar med olika antal döda och levande fiskar. Primers och experimentell uppställning, såsom användning av olika temperaturer för PCR-reaktionen som användes i denna studie, resulterade inte i en funktionell PCR såsom bestämd av elektroforesgel. Det finns några problem med utformningen av PCR-metoderna för eDNA, eftersom syftet är att utforma metoder som kan identifiera vissa arter. Emellertid kommer framtida utveckling av eDNA-metoder troligtvis att inkludera sekvensering och inte detektering av PCR-produktstorlekar. eDNA-metoder kommer att komplettera traditionella fångstmetoder som nät- och elektrofiske, men inte ersätta dem.