Obwohl EtG seit dem Jahr 2000 intensiv als Alkoholmarker in Haaren beforscht wird, bietet die Thematik weiterhin Raum für Forschung, insbesondere im Bereich der instrumentellen Analytik. Ziel der vorliegenden Arbeit ist die Beleuchtung dieser und weiterer Aspekte. Die Extraktion erfolgte überwiegend mittels der sogenannten Mikropulverisierung. Sie ermöglichte die simultane Mahlung der Haarmatrix und Extraktion des EtGs mit einem hohen Probendurchsatz. Die Selektion und anschließende Detektion erfolgte überwiegend durch HPLC-MS/MS. Die Sicherheit bei der Bestimmung des Analyten wurde durch die erfolgreiche Teilnahme an drei Ringversuchen der Society of Hair Testing (SoHT) belegt. Wiederholbedingungen wurden durch Herstellung von eigenen Haarreferenzmaterialien und die Verwendung von homogenen Fremdhaarmaterialien sichergestellt. Zur Evaluierung der Stabilität von EtG wurden zwei Haarmaterialien unter thermischen Stressbedingungen eingelagert und mit dem Gehalt von Referenzproben verglichen. Der Analyt zeigte außergewöhnliche Stabilität unter den gewählten Bedingungen. Ebenso erfolgte eine Beurteilung des Zerstörungsgrads von EtG im Haar durch oxidierende Substanzen, einhergehend mit der Entwicklung eines zerstörungsfreien Schnelltests mittels FTIR zur Detektion von oxidierten Cysteinspezies in Haaren. Das Modellsystem Barthaar wurde für zwei Experimentreihen etabliert: die Korrelation des EtG-Gehaltes im Barthaar nach Aufnahme definierter Alkoholmengen und den Nachweis von glucuronidierten Spezies im Barthaar nach Aufnahme der korrespondierenden Muttersubstanzen. Während keine eindeutige Korrelation zwischen aufgenommener Alkoholmenge und EtG-Gehalt im Barthaar hergestellt werden konnte, war es durchaus möglich, zwei glucuronidierte Metabolite von Arzneistoffen im Barthaar nach Konsum der Ausgangssubstanzen nachzuweisen. / Although EtG is subject to extended research since the year 2000, the topic still holds headroom for further experiments, especially when it comes to the field of instrumental analysis. The goal of the present thesis was the clarification of crucial analytical and further aspects. The extraction was mostly carried out using the so-called micropulverisation. It rendered the simultaneous milling of the hair matrix and extraction of EtG possible with a high sample throughput. Selection of the analyte and following detection was mainly carried out using HPLC-MS/MS. The quality of analysis was ensured by the successful participation in three interlaboratory tests carried out by the Society of Hair Testing (SoHT). Repetitive conditions were ensured by manufacturing of own hair reference materials as well as by the usage of homogeneous external hair materials. Two hair materials were treated under thermal stress conditions and the EtG values were compared to reference samples to verify the analytes stability. EtG showed extraordinary stability under the chosen conditions. Likewise, an assessment of the degree of EtG decay after oxidative treatment as well as the development of a nondestructive assay via FTIR to detect oxidized cysteine species were established. The model system beard hair was arranged for the conduction of two experimental series: the correlation of the EtG content in beard hair after defined oral consumption of ethanol and the detection of glucuronidation of the corresponding parent substances after consumption. Whilst no distinct correlation could be observed for the ethanol experiment, it was possible to provide evidence for the existence of two glucuronized metabolites of drugs after consumption of the parent compounds.

Die missbräuchliche Anwendung von anabolen Substanzen erfolgt mit dem Ziel eines verstärkten Muskelaufbaus - im Sport zur Leistungsverbesserung, in der Tierzucht zum Erreichen von Zuchtidealen oder bei der Masttierhaltung zur Produktivitätssteigerung. Bisher wurden Doping- oder Medikationskontrollen zum Nachweis von anabolen Steroidhormonen üblicherweise im Urin bzw. im Blut durchgeführt. Für bestimmte Fragestellungen kann der analysierbare Zeitraum allerdings unzureichend sein oder aber die Untersuchungsmaterialien sind unter praktischen Gegebenheiten nur eingeschränkt verfügbar. Das Sammeln von Urinproben ist beispielsweise bei Zuchthengsten nur mit einem unverhältnismäßig hohen Aufwand realisierbar. Haare stellen in solchen Situationen eine Alternative dar, da sich das Entnahmeverfahren unkompliziert gestaltet und bei einer entsprechenden Haarlänge die eingelagerten Fremdstoffe länger als in Urin- oder Blutproben detektierbar sein sollten. In der vorliegenden Arbeit wurde ein effektiver Langzeitnachweis für insgesamt 11 anabole Substanzen in Pferdehaar-Proben mittels GC-HRMS und GC-MS/MS entwickelt (Nachweisgrenzen zwischen 0,1 und 5,0 pg/mg). Dabei können zum einen körperfremde anabole Wirkstoffe (z. B. Steroidester in Depotpräparaten) und zum anderen körper-eigene Steroide analysiert werden (z. B. Testosteron und Nandrolon beim Hengst). In verschiedenen Applikationsversuchen wurde gezeigt, dass durch eine Haaranalyse der Nachweis bis zu einem Jahr möglich ist. Für die endogene Nandrolonmenge in Schweifproben von unbehandelten Hengsten wurde eine signifikante Altersabhängigkeit festgestellt. Die ermittelten physiologischen Höchstkonzentrationen für Nandrolon betragen zwischen 1,1 pg/mg bei Junghengsten (1-3 Jahre) und 3,1 pg/mg bei Althengsten (11-20 Jahre). Die Bestimmung von Nandrolon in Haarproben erwies sich für die Körungskontrollen bei Junghengsten als ein geeignetes Verfahren zur Detektion einer exogenen Zufuhr. Die Untersuchung von Haaren ist zum Langzeitnachweis als Alternative gegenüber Blut- und Urinanalysen vorzuziehen, auch wenn sich retrospektiv nicht alle Fragen zum Behandlungsablauf präzise klären lassen (z. B. Angaben zur Dosierung oder zum genauen Applikationszeitpunkt). Das neu etablierte Verfahren ist außerdem die Methode der Wahl, wenn die Verfügbarkeit der übrigen Probematerialien eingeschränkt bzw. eine einfache und schnelle Beprobung erforderlich ist. Es wird bereits zur Medikationskontrolle bei Zuchthengsten sowie bei speziellen forensischen Untersuchungen eingesetzt.

Thesis (Ph.D. Communication Studies)) -- University of Limpopo, 2020 / Hair has been a marker of identity that communicates issues of race, acceptability, class and beauty. Evidence of this was during colonialism and apartheid where South African identities were defined by physical characteristics such as the texture of one’s hair, and the colour of one’s skin. Whiteness was the epitome of beauty which came with certain privileges. Non-White bodies were defined as part of a particular narrative that saw them as well as their hair as inferior to that of White bodies. Academic literature continues to engage African hair from the perspective of a colonial legacy through a postcolonial lens. This study, however, asserts a shift in engaging African hair and introduces an African identity which is re-empowered and liberated through agency and choice, and active participation in the construction of its own identity. This shift in engagement also relinquishes the African identity’s association with the dominant narrative of its conformity to a single European ideology of beauty and identity by introducing a (post)colonial, postmodern theory of a Multi-flex, Neo-hybrid identity which forms part of the theoretical framework of this study. This study draws on the theoretical positions of postmodern theory about the concepts of ‘self’ and identity. It engages interpretations of postmodernism and ‘self’ through the works of Kenneth Gergen and Robert Lifton who provide critical theoretical insight into postmodernism and identity. It also engages critical scholars such as Homi Bhabha, Franz Fanon, Kwame Appiah, Charles Ngwenya and Achille Mbembe, amongst others. Through this theoretical lens, I examine the role of the media in the presentation of the panoply of hair (styles) to South African women in the process of constructing a fluid, flexible and hybrid identity that decentres the ideology of rigid racial identity. I also critically investigate whether non-White women who lived during the colonial-apartheid era and those born in a free democratic era share this multi-flex, neo-hybrid identity of the postmodern woman. Thus this study aims to critically explore social narratives of South African women’s hair and how the media perpetuate the construction of a new postmodern African female identity within the backdrop of the commodification of hair and identity in a globalised market and media environment. Coupled with an interpretivist paradigm, a phenomenological v approach was adopted for this study. Data was collected from print media content material namely, DRUM Hair magazine (editions 2014-2019) due to the assortment of hairstyles and identities it provides for African women. Data was also collected in the form of semi-structured interviews/personal accounts/stories presented as phenomenological narratives from colonial-born Coloured and colonial-born Black female participants. Focus group interviews were conducted on post-apartheid/born-free Coloured and Black female South African participants to understand how these women construct their identities through hairstyle choices and the impact this has on the (re)presentation of their identities within the global beauty market environment. These diverse participants aged from 18 to 104 allow me to trace, if any, the changes in perception of hair and hairstyles from colonial-apartheid South Africa to the new and free post-apartheid South Africa. The results of the study show that media enable the African woman to construct a postmodern identity through the multiplicity of hairstyles/identities available to her. It also provides the African woman with the tools to create various identities for herself through the diversity of hairstyles available to her. The African woman who is exposed to an assortment of hairstyles can navigate from one identity to the next without being loyal to one identity which is typical of the postmodern self. Another finding is that coloniality seems to continue to shape the identities of women born during the colonial apartheid era. But for those born during the (post)colonial and post-apartheid era, they embrace a navigatory form of hybridity that is not loyal to one identity but explores various forms of identity, which the market place affords them and the media perpetuate in the construction of multi-flex, neo-hybrid and postmodern identities. The implication of this study is that it is liberating since it allows us to critically review our identity and what we deem as beautiful and to question the daily choices we make not only with our hairstyles but with fashion, food and other cultural elements that shape our performance of identities. / National Institute for the Humanities and Social Sciences (NIHSS) and South African Humanities Deans Association (SAHUDA)

[pt] No presente trabalho é proposto o desenvolvimento de um método analítico para determinação de S por espectrometria de absorção molecular de alta resolução com fonte contínua e forno de grafite (HR-CS GF MAS). As amostras foram preparadas por dissolução ácida e os padrões de calibração, assemelhados à matriz da amostra dissolvida, contendo sulfato, tioureia ou L-cisteína foram estudados em função de suas diferentes estabilidades térmicas. A técnica de HR-CS GF MAS é uma alternativa interessante para determinação de S, pois apresenta alta resolução espectral que minimiza interferências espectrais, pelo uso de um monocromador de alta resolução que permite a separação das linhas de absorção molecular do analito e da matriz, pelo uso do forno de grafite como fonte de atomização, que permite a separação da matriz e do analito antes da etapa de medida do sinal analítico. Com isso, este trabalho tem por objetivo desenvolver um método analítico para determinação de S em amostras de cabelo por HR-CS GF MAS, a fim de avaliar os níveis deste elemento no organismo e compará-los com os resultados obtidos por ICP OES. As condições escolhidas para temperatura de pirólise e de vaporização foram 1000 graus C e 2400 graus C, respectivamente, utilizando 800 microgramas de W, como modificador permanente, e 15 microgramas e 10 microgramas, respectivamente, de uma mistura de Pd(mais)Mg, como modificador em solução. O valor determinado para a concentração de S no material certificado de referência NCS DC73347a (cabelo humano) está de acordo com o descrito em seu certificado, bem como as concentrações de S determinadas em 14 amostras de cabelo, que estão em concordância com as determinadas por ICP-OES de acordo com teste t-pareado (95 por cento de confiança), o que comprova a boa exatidão do método proposto. / [en] In the presented work it is proposed the development of an analytical method for sulfur determination by high-resolution continuum source graphite furnace molecular absorption spectrometry (HR-CS GF MAS). The samples were prepared by acid dissolution and the calibration standards containing sulfate, thiourea, L-cysteine were studied as a function of their different thermal stabilities and its capability for matrix matching. The HR-CS GF MAS technique is an interesting alternative for sulfur determination, since its capability to perform an interference-free analysis due to its high resolution monochromator that allows to overcome the spectral overlapping and by the use of the graphite furnace as atomizer which minimizes the matrix effects before the analytical measurement. The aim of this work is to develop an analytical method for sulfur determination in hair samples by HR-CS GF MAS, in order to evaluate the levels of this element in the human body and to compare them with the results obtained by ICP OES. The chosen conditions for pyrolysis and vaporization temperatures were 1000 C degrees and 2400 C degrees, respectively, using 800 micrograms of W as permanent modifier combined with 15 micrograms and 10 micrograms, respectively, of Pd(plus)Mg mixture as modifier in solution. The value determined for S concentration in the certified reference material NSC DC73347a (human hair) was in agreement with those reported in its certificate, as well as sulfur concentrations determined in 14 hair samples, which are in agreement with those determined by ICP-OES according to the t-paired test (95 percent level of confidence), which proves the good accuracy of the proposed method.

In der vorliegenden Arbeit wurde ein analytisches Verfahren zur quantitativen Bestimmung von Fettsäureethylestern (FSEE) im Haar und in Hautoberflächenlipiden mittels Headspace-Festphasenmikroextraktion (HS-SPME) und Gaschromatographie-Massenspektrometrie (GC-MS) sowie eine auf Hochleistungs-Flüssigchromatographie mit Photodiodenarray-Detektion (HPLC-DAD) basierende Methode zur Bestimmung der Squalenkonzentrationen in Lipidextrakten entwickelt. Die bei Untersuchung von Proben verschiedener Konsumentengruppen erhaltenen Konzentrationswerte wurden hinsichtlich ihrer Eignung als Marker für chronisch exzessiven Alkoholkonsum untersucht. Aus den Ergebnissen lässt sich schließen, dass Fettsäureethylester im Haar als Alkoholmarker den bisher üblicherweise genutzten Markern wie GGT, CDT oder MCV bezüglich Sensitivität und Spezifität mindestens ebenbürtig sind. Es wurden die folgenden vorläufige Cut-off-Werte festgelegt: wenn sich im Haar für die Summenkonzentration der vier in der höchsten Konzentration vorkommenden FSEE (Ethylmyristat, Ethylpalmitat, Ethyloleat und Ethylstearat) ein Wert > 1 ng/mg ergibt, kann mit hoher Sicherheit von chronisch exzessivem Alkoholkonsum ausgegangen werden, für Abstinenzler werden typischerweise Werte < 0,4 ng/mg gefunden. Durch Bildung des Quotienten der FSEE-Konzentrationen und der Squalenkonzentrationen wurden relative FSEE-Konzentrationen erhalten, die im Falle der Haaranalyse zu einer Verbesserung der Zuordnungssicherheit zu den entsprechenden Konsumentengruppen führten bzw. bei der Analyse von Hautoberflächenlipiden einen sinnvollen Vergleich der Werte erst ermöglichten. Als vorläufiger Cut-off-Wert für die relativen FSEE-Konzentrationen wurde ein Wert von 2 ng/µg vorgeschlagen. Als weiteres wichtiges Ergebnis der Arbeit wurde der Einlagerungsmechanismus der FSEE ins Haar aufgeklärt. Es konnte gezeigt werden, dass Fettsäureethylester in erster Linie über das Sebum ins Haar gelangen. / The current doctoral thesis presents the development of an analytical procedure for the quantitative analysis of fatty acid ethyl esters (FAEE) in hair and in skin surface lipids using headspace solid phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS) as well as a method based on high-performance liquid chromatography with photodiode array detection (HPLC-DAD) to determine squalene concentrations in lipid extracts. The results obtained from analysis of samples from different alcohol consuming groups showed that FAEE are suitable markers for long-term alcohol misuse. Concerning sensitivity and specifity they are at least as good as other commonly used markers like GGT, CDT or MCV. The following provisional cut-off values were established: for chronically excessive alcohol consumption, the sum of the four FAEE (ethyl myristate, ethyl palmitate, ethyl oleate and ethyl stearate) found in the highest mean concentrations should be > 1 ng/mg in hair; for non-drinkers, concentrations < 0,4 ng/mg are typical. The quotient obtained by dividing the FAEE concentration by the squalene concentration was defined as the relative FAEE concentration, which provides a better classification of the samples regarding the consumer groups through hair analysis. Relative FAEE values also allow a reasonable comparison in the case of skin surface lipid concentrations for the first time. 2 ng/µg is suggested as a preliminary cut-off value. As a further important result of the current work, the mechanism of incorporation of FAEE into hair was clarified. It was shown that fatty acid ethyl esters are incorporated into hair mainly through sebum.

O consumo dos diferentes tipos de drogas está associado a problemas sociais, econômicos e de saúde pública, em todas as regiões no mundo. Dentre os problemas de saúde pública, podemos destacar a alta prevalência de comorbidade entre o uso de drogas e os transtornos mentais. A Cannabis, a cocaína e o crack são as drogas ilícitas mais consumidas no Brasil. A utilização do cabelo como matriz biológica para determinação destas drogas permite avaliar o uso crônicos pelos indivíduos, uma vez que o cabelo é uma matriz estável, de fácil manipulação e a janela de detecção depende apenas do comprimento do cabelo. Entretanto, a análise em cabelo ainda representa um desafio analítico. Foram desenvolvidos dois métodos para a detecção das diferentes drogas no cabelo, com diferentes enfoques analíticos. O primeiro método (desenvolvido durante o estágio de doutorado sanduíche na Itália) identificou e quantificou cocaína e metabólitos usando a técnica de column switching e detecção por LC-MS/MS. O segundo método foi desenvolvido para determinação de canabinóides nas amostras de cabelo utilizando GC-MS. O diferencial deste método foi a utilização de um novo dispositivo de extração em fase sólida (as ponteiras DPX) para concentração e purificação do extrato, utilizando menor quantidade de solventes. A determinação dos canabinóides e cocaínicos foi realizada nas amostras de cabelo da população atendida no CAPS - AD de Ribeirão Preto, São Paulo. Além da coleta da amostra de cabelo, o sujeito foi submetido a uma entrevista, onde os seguintes instrumentos de avaliação foram aplicadas: Questionário sobre a saúde do Paciente 9, Inventário de fobia social, Self Report Questionnaire, Questionário de Ansiedade de Beck, Inventário de Depressão de Beck e Questionário sobre o uso da Cannabis, bem como um questionário elaborado pelo pesquisador para coleta de dados sociodemográficos, consumo de substâncias e dados sobre a amostra de cabelo, como comprimento, cor, tintura ou coloração. As amostras de cabelo foram analisadas e a média das concentrações de cada droga encontrada no cabelo foi correlacionada com os indicadores clínicos de transtorno mentais, obtidos através dos instrumentos de avaliação psiquiátrica. A maior prevalência de indicadores clínicos positivos para transtornos psiquiátricos entre a população estudada foi de transtornos mentais comuns, entre eles a ansiedade e depressão. A comparação da média de concentração de Cannabis, cocaína e crack no cabelo com os indicadores clínicos positivos para os transtornos não apresentou resultados estatisticamente significantes. Entretanto, podemos inferir que os sujeitos que apresentaram maior concentração média de Cannabis e cocaína no cabelo possuíam mais indicadores clínicos positivos para sintomas mentais comuns e depressão maior enquanto que os sujeitos usuários de crack possuíam mais indicadores clínicos positivos para sintomas ansiedade. Apesar de algumas limitações, podemos concluir que o estudo possibilitou estimar a prevalência da morbidade entre abuso de drogas ilícitas e transtornos psiquiátricos na população atendida no Centro de Atenção Psicossocial Álcool e drogas de Ribeirão Preto. / Different kinds of drug use have been associated to social, economic and health public problems worldwide. Among the high prevalent public health problems is the comorbidity between drug abuse and psychiatric disorders. Cannabis, cocaine and crack are the most consumed illicit drugs in Brazil. Hair use as the biological matrix for the determination of these drugs allows to evaluate chronic use, once hair is a stable matrix, easy to manipulate and the window detection only depends on the size of the hair. However, hair analysis still represents an analytical challenge. It was developed two methods for the detection of the drugs in hair, with different analytical approach. The first method (developed during doctoral stage in Italy) had identified and quantified cocaine and metabolites using column switching technique and LCMS/ MS detection. The second method was developed for determination of cannabinoids in hair samples using GC-MS. Decontamination procedure was the same cited above. The differential of this method was the use of a new device in solid phase extraction (DPX tips) for the extracts concentration and purification, using less solvents volumes. Cannabinoids and cocaine analysis were performed in hair samples from people who were enrolled in the CAPS - AD of Ribeirão Preto, São Paulo. Besides hair collection, the individual was submitted to an interview, where it was applied the following evaluation scales: Patient health questionnaire - 9, Social phobia inventory, Self report questionnaire, Beck anxiety inventory, Beck depression inventory and Cannabis research questionnaire as well as a questionnaire made by the author to collect sociodemographic data, substance consume and hair data. Hair samples were analyzed and the concentrations were correlated with positive clinical factors of mental disorders obtained through evaluation scales. The highest prevalence of positive clinical indicators for psychiatric disorders among the population studied was of common mental disorders, including anxiety and depression. The comparison of the average concentration of Cannabis, cocaine and crack in the hair with the positive clinical indicators for the disorders did not show statistically significant results. However, we can infer that the subjects who had higher average concentration of Cannabis and cocaine in hair had showed positive indicators for common mental symptoms and major depression as well as the subjects who had higher average concentration of crack in hair had showed positive indicators for anxiety. Despite of some limitations, we can conclude that the study had allowed estimating the prevalence of morbidity among illicit drugs abuse and psychiatric disorders in the population enrolled in the psychosocial care center in Ribeirão Preto.

Este trabalho propõe o uso de microfrascos de polipropileno adaptados a um forno de microondas focalizadas como um procedimento alternativo para a preparação de amostras. O pré-tratamento de amostras em microfrascos digestores agrega algumas características importantes como aumento da freqüência analítica, pequena massa de amostra e baixo consumo de reagentes. A eficiência do sistema de digestão foi verificada com o desenvolvimento de metodologia para a determinação de cobre, ferro, manganês, selênio e zinco em cabelo por espectrometria de absorção atômica com atomização por chama ou eletrotérmica em forno de grafite. Os elementos selecionados são essenciais para os seres humanos e são indicadores nutricionais e do bom funcionamento enzimático. O sistema de digestão é constituído de um forno de microondas focalizadas e um tubo de vidro com 30 cm de comprimento e 4 cm de largura, ao qual são colocados quatro ou cinco microfrascos de polipropileno com capacidade para respectivamente 4,0 mL e 2,0 mL. Esses microfrascos foram adaptados a um suporte de Teflon&#174; e fixado a uma haste de vidro, facilitando a introdução e retirada do interior do tubo de vidro. O sistema proposto possibilitou uma drástica redução no tempo de preparo de amostra e melhor eficiência de decomposição (menor teor de carbono residual) em comparação com os procedimentos convencionais. O sistema \"quase fechado\" associado a baixas temperaturas atingidas evitou perdas de elementos por volatilidade, além de apresentar uma ótima homogeneidade de aquecimento entre os microfrascos. A exatidão da metodologia foi verificada através de ensaios de recuperação da análise de um material de referência certificado (IAEA-086) e da análise de amostra com adição e recuperação dos analitos apresentando recuperações de 90 a 103%. / In this work the use of polypropylene vials adapted at focused m1crowaves, as alternative method for sample preparation is proposed. The sample pre-treatment in digestion vials include some desirable characteristics like increase of analytical frequency, low sample mass and low reagents consumption. To check the efficiency of the digestion system the development of a methodology for copper, iron, manganese, selenium and zinc determination using graphite furnace or flame atomic absorption spectrometry was performed. The selected elements are essential for human individual, nutritional indicators and required for enzymatic working. The digestion system is constituted of a focused microwave oven, a glass tube with 30 cm length and 4 cm width, where are setting four or five polypropylene vials with capacity for 4.0 mL and 2.0 mL, respectively, through a Teflon&#174; support assisted by glass haste. The proposed system allowed a drastic reduction of sample preparation time and improved the decomposition efficiency (lower carbon residual content) comparing with conventional methods. The \"almost closed\" system associated with the low temperature avoids elements losses and improve heating homogeneity among the vials. The accuracy of the methodology was ascertained through good recoveries for a certificate reference material (IAEA-086) analysis and good recovery of spiked sample analysis, presenting recovery 90 to 103%.

A presente dissertação expositiva teve por objetivo o desenvolvimento de metodologia para análise forense de fios de cabelos. Considerado um microvestígio comum de ser encontrado em locais de crime contra pessoa (DOREA, 2010), fios de cabelo são capazes de fornecer informações úteis na identificação da autoria do crime, ou a entender a dinâmica de um crime violento (ROBERTSON, 1999). As fibras compostas por fio de cabelo deterioram-se lentamente (ROBBINS, 2012), e podem ser analisadas mesmo transcorrido longo período de tempo, tornando-se ainda mais relevante em locais de crime que são examinados tardiamente. Os equipamentos utilizados no presente estudo são de uso comum em laboratórios, permitindo que a metodologia seja amplamente empregada. O presente estudo buscou desenvolver metodologias para análise por microscopia ótica de fios de cabelo, identificando as características de interesse forense passíveis de serem estudadas. Utilizaram-se amostras de fios de cabelo para análise das seções transversais e longitudinais, de forma destrutiva e não destrutiva, com preparação de lâminas de forma permanente e não permanente. Como resultado obteve-se uma metodologia de baixo custo descrita para aplicações forenses em vestígios coletados em locais de crime, em armas de crimes ou em suspeitos, de forma a combater a criminalidade face o poder probatório da prova material. Constatou-se a possibilidade de identificação de características macroscópicas e microscópicas de fios de cabelo, que revelam atributos do doador e, em alguns casos, auxiliar no entendimento da dinâmica do crime. A agilidade observada no método permite ainda a obtenção de informações durante a fase preliminar ou de investigação em curtos espaços de tempo. / This monographic dissertation aimed to develop standards of microscopic forensic hair analysis. A very common trace to be found in certain crimes (DOREA, 2010), hair can be helpful to provide information regarding the perpetrator or the way that the crime was committed (ROBERTSON, 1999). Once hair is a low degradation fiber (ROBBINS, 2012), it can be analyzed long after the fact, becoming even more relevant in crime scenes processed after elapse time. The equipment’s used for this study are commonly found in forensic labs, allowing broad use. The study was restricted to literature review and further elaboration of preparation and analysis by optical microscopy of hairs methods, identifying the characteristics of forensic interest that can be studied. Samples of hair for cross section and longitudinal sections analysis had been used. Destructive and non-destructive methods in permanent and non-permanent blades where tested. As a result a low cost methodology was obtained for forensic applications in traces collected from crime scenes, weapons used in crimes or suspects, in order to combat crime by using the probative power of physical evidence.

A presente dissertação expositiva teve por objetivo o desenvolvimento de metodologia para análise forense de fios de cabelos. Considerado um microvestígio comum de ser encontrado em locais de crime contra pessoa (DOREA, 2010), fios de cabelo são capazes de fornecer informações úteis na identificação da autoria do crime, ou a entender a dinâmica de um crime violento (ROBERTSON, 1999). As fibras compostas por fio de cabelo deterioram-se lentamente (ROBBINS, 2012), e podem ser analisadas mesmo transcorrido longo período de tempo, tornando-se ainda mais relevante em locais de crime que são examinados tardiamente. Os equipamentos utilizados no presente estudo são de uso comum em laboratórios, permitindo que a metodologia seja amplamente empregada. O presente estudo buscou desenvolver metodologias para análise por microscopia ótica de fios de cabelo, identificando as características de interesse forense passíveis de serem estudadas. Utilizaram-se amostras de fios de cabelo para análise das seções transversais e longitudinais, de forma destrutiva e não destrutiva, com preparação de lâminas de forma permanente e não permanente. Como resultado obteve-se uma metodologia de baixo custo descrita para aplicações forenses em vestígios coletados em locais de crime, em armas de crimes ou em suspeitos, de forma a combater a criminalidade face o poder probatório da prova material. Constatou-se a possibilidade de identificação de características macroscópicas e microscópicas de fios de cabelo, que revelam atributos do doador e, em alguns casos, auxiliar no entendimento da dinâmica do crime. A agilidade observada no método permite ainda a obtenção de informações durante a fase preliminar ou de investigação em curtos espaços de tempo. / This monographic dissertation aimed to develop standards of microscopic forensic hair analysis. A very common trace to be found in certain crimes (DOREA, 2010), hair can be helpful to provide information regarding the perpetrator or the way that the crime was committed (ROBERTSON, 1999). Once hair is a low degradation fiber (ROBBINS, 2012), it can be analyzed long after the fact, becoming even more relevant in crime scenes processed after elapse time. The equipment’s used for this study are commonly found in forensic labs, allowing broad use. The study was restricted to literature review and further elaboration of preparation and analysis by optical microscopy of hairs methods, identifying the characteristics of forensic interest that can be studied. Samples of hair for cross section and longitudinal sections analysis had been used. Destructive and non-destructive methods in permanent and non-permanent blades where tested. As a result a low cost methodology was obtained for forensic applications in traces collected from crime scenes, weapons used in crimes or suspects, in order to combat crime by using the probative power of physical evidence.

Este trabalho propõe o uso de microfrascos de polipropileno adaptados a um forno de microondas focalizadas como um procedimento alternativo para a preparação de amostras. O pré-tratamento de amostras em microfrascos digestores agrega algumas características importantes como aumento da freqüência analítica, pequena massa de amostra e baixo consumo de reagentes. A eficiência do sistema de digestão foi verificada com o desenvolvimento de metodologia para a determinação de cobre, ferro, manganês, selênio e zinco em cabelo por espectrometria de absorção atômica com atomização por chama ou eletrotérmica em forno de grafite. Os elementos selecionados são essenciais para os seres humanos e são indicadores nutricionais e do bom funcionamento enzimático. O sistema de digestão é constituído de um forno de microondas focalizadas e um tubo de vidro com 30 cm de comprimento e 4 cm de largura, ao qual são colocados quatro ou cinco microfrascos de polipropileno com capacidade para respectivamente 4,0 mL e 2,0 mL. Esses microfrascos foram adaptados a um suporte de Teflon&#174; e fixado a uma haste de vidro, facilitando a introdução e retirada do interior do tubo de vidro. O sistema proposto possibilitou uma drástica redução no tempo de preparo de amostra e melhor eficiência de decomposição (menor teor de carbono residual) em comparação com os procedimentos convencionais. O sistema \"quase fechado\" associado a baixas temperaturas atingidas evitou perdas de elementos por volatilidade, além de apresentar uma ótima homogeneidade de aquecimento entre os microfrascos. A exatidão da metodologia foi verificada através de ensaios de recuperação da análise de um material de referência certificado (IAEA-086) e da análise de amostra com adição e recuperação dos analitos apresentando recuperações de 90 a 103%. / In this work the use of polypropylene vials adapted at focused m1crowaves, as alternative method for sample preparation is proposed. The sample pre-treatment in digestion vials include some desirable characteristics like increase of analytical frequency, low sample mass and low reagents consumption. To check the efficiency of the digestion system the development of a methodology for copper, iron, manganese, selenium and zinc determination using graphite furnace or flame atomic absorption spectrometry was performed. The selected elements are essential for human individual, nutritional indicators and required for enzymatic working. The digestion system is constituted of a focused microwave oven, a glass tube with 30 cm length and 4 cm width, where are setting four or five polypropylene vials with capacity for 4.0 mL and 2.0 mL, respectively, through a Teflon&#174; support assisted by glass haste. The proposed system allowed a drastic reduction of sample preparation time and improved the decomposition efficiency (lower carbon residual content) comparing with conventional methods. The \"almost closed\" system associated with the low temperature avoids elements losses and improve heating homogeneity among the vials. The accuracy of the methodology was ascertained through good recoveries for a certificate reference material (IAEA-086) analysis and good recovery of spiked sample analysis, presenting recovery 90 to 103%.