The aim of the diploma thesis was the aroma active compounds assessment and sensory profile determination of various types of sea buckthorn (Hippopha rhamnoides L.). The theoretical part provides the detailed description of this plant, comprising the occurence, taxonomy, chemical composition and use. Experimental part summarizes the data obtained: identification and quantification of aroma compounds using the SPME – GC –FID and GC-MS method and evaluation of complete sensory profile. Various cultivars of sea buckthorn harvested in 2009-2012 were analysed. In total 23 various types of sea buckthorn were measured, 23 alcohols, 10 aldehydes, 11 esters, 14 ketones and 5 acids were found.

This thesis deals with the assessment of aroma active compounds in gooseberry and sensory analysis of it focusing on flavour. The theoretical part describes general characteristics, biological marks and properties of selected varieties, healing abilities, the active substances contained in gooseberry fruits and their use. The aim of the experimental part was to determine aroma-active substances contained in fruits of nineteen selected cultivars of gooseberry using SPME-GC-FID method. In total 45 volatile compounds were identified, among them 17 alcohols, 11 aldehydes, 6 ketones, 9 esters and 2 acids. For a better identification one sample (Captivátor variety) was also analysed using GC-MS with purge and trap extraction. Pentan-1-ol, hexanal, pentanal, ethylethanoate, ethylbutanoate, methylethanoate, methylbutanoate and ethanol were confirmed using mass spectra. Only several cultivars were selected for the assessment of overall sensory quality and palatability of fruits. Karmen and Remarka varieties were considered as the best samples by assessors.

A Aniba canelilla (H.B.K.) Mez é uma planta aromática proveniente da região amazônica cujo óleo essencial apresenta como componentes majoritários o 1-nitro-2-feniletano e o metileugenol. Apesar das atividades antifúngicas e anti-inflamatórias cientificamente comprovadas e do uso popular do óleo para o tratamento de dermatites, acnes e feridas, não existe até o momento um estudo que verse sobre a quantificação desses compostos na pele. O objetivo deste trabalho foi a validação de um método bioanalítico otimizado por microextração em fase sólida no modo headspace em cromatógrafo gasoso com detector de ionização de chama (HS-SPME-GC-FID) para a determinação do 1-nitro-2-feniletano e metileugenol a partir do óleo essencial em diferentes amostras de estudo de permeação cutânea in vitro. Uma metodologia foi desenvolvida e validada por HS-SPME-GC-FID. A faixa da curva de calibração foi de 2,08 - 207,87 μg.mL-1 para o 1-nitro-2-feniletano e de 0,40-40,41 μg.mL-1 para o metileugenol. A presença de matriz e as características intrínsecas da metodologia de HS-SPME requereram uma transformação da curva de calibração. A transformação logarítmica (Log10) foi então aplicada aos dados e os resultados apresentaram homocedasticidade, resíduos dispersos, coeficiente de determinação (r²> 0,99) e recuperação adequados. Estudos de permeação cutânea foram realizados em células de Franz com diferentes quantidades (20, 100 e 200 μL) de óleo essencial de A. canelilla para avaliar o perfil de permeação e retenção em pele de orelha suína e fluido receptor. A análise das amostras nas condições validadas mostrou uma grande permeação e retenção dos compostos na seguinte ordem: fluido receptor >> derme >> epiderme >> estrato córneo. Verificou-se um aumento progressivo e dependência na retenção com base na quantidade aplicada no compartimento doador e grande retenção principalmente no fluido receptor e derme, resultado este compatível com as características físico-químicas de Log P, afinidade ao ambiente hidrofílico e lipofílico, tamanho e peso molecular do 1-nitro-2-feniletano e metileugenol. Em conclusão, o método proposto por HS-SPME-GC-FID para quantificar os compostos majoritários do óleo essencial de A. canelilla em amostras de pele de orelha suína e fluido receptor foi seletivo, preciso, exato e adequado, e pode ser utilizado em análises futuras. / Aniba canelilla (H.B.K.) Mez is an aromatic plant from the Amazon region whose essential oil has 1-nitro-2-phenylethane and methyleugenol as major compounds. Despite of the scientifically proved antifungal and anti-inflammatory activities and the popular use of oil for the treatment of dermatitis, acnes and wounds, there is no study up to date about the quantification of these compounds in skin samples. The aim of this study was the validation of an optimized bioanalytical method by solid phase microextraction on headspace mode in gas chromatograph with flame ionization detector (HS-SPME-GC-FID) for the determination of 1-nitro-2-phenylethane and methyleugenol from the essential oil in different samples of in vitro cutaneous permeation study. A methodology was developed and validated by HS-SPME-GC-FID. The ranges of calibration curves were 2.08 - 207.87 μg.mL-1 for 1-nitro-2-phenylethane and 0.40 - 40.41 μg.mL-1 for methyleugenol. The presence of matrix and the intrinsic characteristics of the HS-SPME methodology required a transformation to the calibration curves. The logarithmic transformation (Log10) was then applied to the data and the results showed homoscedasticity, dispersed residues, and adequate coefficient of determination (r²> 0.99) and recovery. Skin permeation studies were performed on Franz cells with different amounts (20, 100 and 200 μL) of A. canelilla essential oil to evaluate the skin permeation and retention profile in porcine ear skin and receptor fluid. The analysis of the samples under the validated conditions showed a high permeation and retention of the major compounds in the following order: receptor fluid >> dermis >> epidermis >> stratum corneum. A progressive increase and retention dependence were observed based on the amount applied in the donor compartment, and large retention mainly on the receptor fluid and dermis was observed, in accordance with the physicochemical characteristics of Log P, affinity to the hydrophilic and lipophilic environment, size and molecular weight of 1-nitro-2-phenylethane and methyleugenol. In conclusion, the method proposed by HS-SPME-GC-FID to quantify the major compounds of A. canelilla essential oil in porcine ear skin and receptor fluid samples was selective, accurate, precise and adequate, and can be used in future analyzes.

A Aniba canelilla (H.B.K.) Mez é uma planta aromática proveniente da região amazônica cujo óleo essencial apresenta como componentes majoritários o 1-nitro-2-feniletano e o metileugenol. Apesar das atividades antifúngicas e anti-inflamatórias cientificamente comprovadas e do uso popular do óleo para o tratamento de dermatites, acnes e feridas, não existe até o momento um estudo que verse sobre a quantificação desses compostos na pele. O objetivo deste trabalho foi a validação de um método bioanalítico otimizado por microextração em fase sólida no modo headspace em cromatógrafo gasoso com detector de ionização de chama (HS-SPME-GC-FID) para a determinação do 1-nitro-2-feniletano e metileugenol a partir do óleo essencial em diferentes amostras de estudo de permeação cutânea in vitro. Uma metodologia foi desenvolvida e validada por HS-SPME-GC-FID. A faixa da curva de calibração foi de 2,08 - 207,87 μg.mL-1 para o 1-nitro-2-feniletano e de 0,40-40,41 μg.mL-1 para o metileugenol. A presença de matriz e as características intrínsecas da metodologia de HS-SPME requereram uma transformação da curva de calibração. A transformação logarítmica (Log10) foi então aplicada aos dados e os resultados apresentaram homocedasticidade, resíduos dispersos, coeficiente de determinação (r²> 0,99) e recuperação adequados. Estudos de permeação cutânea foram realizados em células de Franz com diferentes quantidades (20, 100 e 200 μL) de óleo essencial de A. canelilla para avaliar o perfil de permeação e retenção em pele de orelha suína e fluido receptor. A análise das amostras nas condições validadas mostrou uma grande permeação e retenção dos compostos na seguinte ordem: fluido receptor >> derme >> epiderme >> estrato córneo. Verificou-se um aumento progressivo e dependência na retenção com base na quantidade aplicada no compartimento doador e grande retenção principalmente no fluido receptor e derme, resultado este compatível com as características físico-químicas de Log P, afinidade ao ambiente hidrofílico e lipofílico, tamanho e peso molecular do 1-nitro-2-feniletano e metileugenol. Em conclusão, o método proposto por HS-SPME-GC-FID para quantificar os compostos majoritários do óleo essencial de A. canelilla em amostras de pele de orelha suína e fluido receptor foi seletivo, preciso, exato e adequado, e pode ser utilizado em análises futuras. / Aniba canelilla (H.B.K.) Mez is an aromatic plant from the Amazon region whose essential oil has 1-nitro-2-phenylethane and methyleugenol as major compounds. Despite of the scientifically proved antifungal and anti-inflammatory activities and the popular use of oil for the treatment of dermatitis, acnes and wounds, there is no study up to date about the quantification of these compounds in skin samples. The aim of this study was the validation of an optimized bioanalytical method by solid phase microextraction on headspace mode in gas chromatograph with flame ionization detector (HS-SPME-GC-FID) for the determination of 1-nitro-2-phenylethane and methyleugenol from the essential oil in different samples of in vitro cutaneous permeation study. A methodology was developed and validated by HS-SPME-GC-FID. The ranges of calibration curves were 2.08 - 207.87 μg.mL-1 for 1-nitro-2-phenylethane and 0.40 - 40.41 μg.mL-1 for methyleugenol. The presence of matrix and the intrinsic characteristics of the HS-SPME methodology required a transformation to the calibration curves. The logarithmic transformation (Log10) was then applied to the data and the results showed homoscedasticity, dispersed residues, and adequate coefficient of determination (r²> 0.99) and recovery. Skin permeation studies were performed on Franz cells with different amounts (20, 100 and 200 μL) of A. canelilla essential oil to evaluate the skin permeation and retention profile in porcine ear skin and receptor fluid. The analysis of the samples under the validated conditions showed a high permeation and retention of the major compounds in the following order: receptor fluid >> dermis >> epidermis >> stratum corneum. A progressive increase and retention dependence were observed based on the amount applied in the donor compartment, and large retention mainly on the receptor fluid and dermis was observed, in accordance with the physicochemical characteristics of Log P, affinity to the hydrophilic and lipophilic environment, size and molecular weight of 1-nitro-2-phenylethane and methyleugenol. In conclusion, the method proposed by HS-SPME-GC-FID to quantify the major compounds of A. canelilla essential oil in porcine ear skin and receptor fluid samples was selective, accurate, precise and adequate, and can be used in future analyzes.

A Aniba canelilla (H.B.K.) Mez é uma planta aromática proveniente da região amazônica cujo óleo essencial apresenta como componentes majoritários o 1-nitro-2-feniletano e o metileugenol. Apesar das atividades antifúngicas e anti-inflamatórias cientificamente comprovadas e do uso popular do óleo para o tratamento de dermatites, acnes e feridas, não existe até o momento um estudo que verse sobre a quantificação desses compostos na pele. O objetivo deste trabalho foi a validação de um método bioanalítico otimizado por microextração em fase sólida no modo headspace em cromatógrafo gasoso com detector de ionização de chama (HS-SPME-GC-FID) para a determinação do 1-nitro-2-feniletano e metileugenol a partir do óleo essencial em diferentes amostras de estudo de permeação cutânea in vitro. Uma metodologia foi desenvolvida e validada por HS-SPME-GC-FID. A faixa da curva de calibração foi de 2,08 - 207,87 μg.mL-1 para o 1-nitro-2-feniletano e de 0,40-40,41 μg.mL-1 para o metileugenol. A presença de matriz e as características intrínsecas da metodologia de HS-SPME requereram uma transformação da curva de calibração. A transformação logarítmica (Log10) foi então aplicada aos dados e os resultados apresentaram homocedasticidade, resíduos dispersos, coeficiente de determinação (r²> 0,99) e recuperação adequados. Estudos de permeação cutânea foram realizados em células de Franz com diferentes quantidades (20, 100 e 200 μL) de óleo essencial de A. canelilla para avaliar o perfil de permeação e retenção em pele de orelha suína e fluido receptor. A análise das amostras nas condições validadas mostrou uma grande permeação e retenção dos compostos na seguinte ordem: fluido receptor >> derme >> epiderme >> estrato córneo. Verificou-se um aumento progressivo e dependência na retenção com base na quantidade aplicada no compartimento doador e grande retenção principalmente no fluido receptor e derme, resultado este compatível com as características físico-químicas de Log P, afinidade ao ambiente hidrofílico e lipofílico, tamanho e peso molecular do 1-nitro-2-feniletano e metileugenol. Em conclusão, o método proposto por HS-SPME-GC-FID para quantificar os compostos majoritários do óleo essencial de A. canelilla em amostras de pele de orelha suína e fluido receptor foi seletivo, preciso, exato e adequado, e pode ser utilizado em análises futuras. / Aniba canelilla (H.B.K.) Mez is an aromatic plant from the Amazon region whose essential oil has 1-nitro-2-phenylethane and methyleugenol as major compounds. Despite of the scientifically proved antifungal and anti-inflammatory activities and the popular use of oil for the treatment of dermatitis, acnes and wounds, there is no study up to date about the quantification of these compounds in skin samples. The aim of this study was the validation of an optimized bioanalytical method by solid phase microextraction on headspace mode in gas chromatograph with flame ionization detector (HS-SPME-GC-FID) for the determination of 1-nitro-2-phenylethane and methyleugenol from the essential oil in different samples of in vitro cutaneous permeation study. A methodology was developed and validated by HS-SPME-GC-FID. The ranges of calibration curves were 2.08 - 207.87 μg.mL-1 for 1-nitro-2-phenylethane and 0.40 - 40.41 μg.mL-1 for methyleugenol. The presence of matrix and the intrinsic characteristics of the HS-SPME methodology required a transformation to the calibration curves. The logarithmic transformation (Log10) was then applied to the data and the results showed homoscedasticity, dispersed residues, and adequate coefficient of determination (r²> 0.99) and recovery. Skin permeation studies were performed on Franz cells with different amounts (20, 100 and 200 μL) of A. canelilla essential oil to evaluate the skin permeation and retention profile in porcine ear skin and receptor fluid. The analysis of the samples under the validated conditions showed a high permeation and retention of the major compounds in the following order: receptor fluid >> dermis >> epidermis >> stratum corneum. A progressive increase and retention dependence were observed based on the amount applied in the donor compartment, and large retention mainly on the receptor fluid and dermis was observed, in accordance with the physicochemical characteristics of Log P, affinity to the hydrophilic and lipophilic environment, size and molecular weight of 1-nitro-2-phenylethane and methyleugenol. In conclusion, the method proposed by HS-SPME-GC-FID to quantify the major compounds of A. canelilla essential oil in porcine ear skin and receptor fluid samples was selective, accurate, precise and adequate, and can be used in future analyzes.

This thesis is focused on potentially allergenic substances (PASs) in cosmetics. Their specific features, methods of control and observation are described. There are also mentioned dermatology problems connected with usage of perfumed cosmetic products in which the allergenic ingredients can be found and possibilities of their regulation. Fragrances are mixtures of natural or synthetic character which give the aroma. In nature, fragrances are produced mainly by plants. More than one hundred fragrances have been identified as allergens. Twenty six of them were declared as PASs. Allergenic components of perfume compositions are the main cause of allergic contact dermatitis. Experimental part of the thesis is focused on the procedure of analysis of specific allergenic fragrances (?-Amylcinnamaldehyde, Anisealcohol, Benzylsalicylate, Cinnamaldehyde, ?-Hexylcinnamaldehyde, 7-Hydroxycitronellal and Methyl-2-octynoate). Headspace-Solid Phase Microextraction connected with Gas Chromatography-Flame Ionisation Detector (HS-SPME-GC-FID) was used for extraction, analysis and identification of these substances. The method was validated and applied on the spectrum of real samples of cosmetic products.

This master thesis deals with the assessment of aroma active compounds in fruits of currant (Ribes spp.). The theoretical part was focused on basic characteristics and chemical composition of currants, as well as the basic principles of techniques used: solid phase micro extraction (SPME), gas chromatography (GC) and sensory analysis. The main aim of the experimental part was to determine aroma active compounds in currants using SPME-GC-FID method. The profile and scale tests were used for assessment of sensory quality and tastiness of fruits. In total 18 varieties, among them 6 white, 6 red and 6 black currants, were evaluated. Fifty aroma active compounds were identified including 21 alcohols, 10 aldehydes, 2 acids, 8 ketones and 9 esters. The results were statistically evaluated using principal component analysis (PCA) to investigate the influence of single compounds on sensory quality of fruits.

L'évaluation de l'inertie des matières plastiques au contact de denrées alimentaires est régie par le règlement européen N°10/2011. Au Liban, l'absence de législations relatives à l'usage des matières en plastiques a conduit à des emballages non contrôlés au niveau de la production et du stockage, ce qui peut induire un risque sanitaire pour le consommateur. L'objectif de ce travail a été d'apprécier les phénomènes de migration des contaminants du PET vers l'eau. Pour cela, l'analyse de certains migrants potentiels a été initiée tels que des COV et des SV afin de vérifier la conformité de leur teneur par rapport aux LMA dans les règlementations internationales. Le dosage des aldéhydes dans l'eau a été effectué par dérivation avec la 2,4-DNPH, suivie d'une étape de préconcentration sur une cartouche en C18, puis séparation et quantification par HPLC-UV. L'analyse des composés SV a été réalisée par SPME-GC-FID sur une fibre en PDMS/DVB. L'analyse des BTEX et du styrène a été réalisée par HS-Trap-GC-FID. Ces méthodes ont été validées conformément à la norme NF T 90-210 avec des LQ inférieures aux LMA. L'analyse des COV dans l'eau embouteillée et dans le PET a été réalisée par HSTrap- GC-MS. La présence de FA, d'AA, de DEP et des BTEX dans l'eau embouteillée en PET a été confirmée. Il a été mis en évidence que la température et l'exposition solaire influencent la migration des aldéhydes. Les concentrations d'AA trouvées après incubation à 40ºC ne sont pas négligeables et peuvent modifier les propriétés organoleptiques de l'eau. L'analyse du PET montre la présence des hydrocarbures, des aldéhydes, des alcools, et des cétones / The inertness’ value of plastics that are on contact with foodstuffs is governed by the European rule N°10/2011. In Lebanon, the lack of the Rules and Regulations of plastics’ usage led for a non-controlled packing in production as in storage, which will cause a sanitary risk to the consumer and to the population. The purpose of this research was to appreciate the migration’s phenomena of contaminants from the PET to the water. For this, there was an analysis of potential migrants such as VOC and SV to verify their tenor’s conformity relative to the MCL in international regulations. The aldehydes’ dosage in the water was performed by the derivation with the 2,4-DNPH, followed by a concentration on a C18 cartridge, then separation and quantification was done by HPLC-UV. The SV compounds’ analysis was realized by SPME-GC-FID method on a PDMS / DVB fiber. The BTEX and the styrene’s analysis was done by HS-trap-GC-FID method. These methods were validated in accordance with standard NF T 90-210 with a LQ less than the MCL. The volatile compounds in the bottled water and in the PET were analyzed by HS-trap-GC-MS method. The presence of FA, AA, DEP and BTEX in the bottled water with the PET was confirmed. It was highlighted that temperature and sun exposition influence the aldehydes’ migration. The acetaldehyde’s concentration after incubation at 40ºC wasn’t negligible and can modify the water’s organoleptic properties. The PET’s analyze reveals the presence of hydrocarbons, aldehydes, alcohols and ketones

The aim of this master‘s thesis was to determine the aroma active compounds and monitor the sensory quality of apples. The theoretical part deals with the description, composition and properties of apples, information about the aroma compounds, their determination and possibilities for sensory evaluation of apples is also given. The gas chromatography method combined with the solid-phase microextraction, utilized for the specification of aroma compounds, is described. In the experimental part, the SPME-GC-FID method was applied on selected cultivars of apples specially cultivated against apple scab (Venturia inaequalis), i.e. 24 genotypes and Golden Delicious as the control variety. In total 60 various aroma compounds were identified, 22 alcohols, 12 aldehydes, 11 ketones, 10 esters and 5 organic acids. The number and concentration of compounds identified differed according to the cultivars. Sensory analysis was performed using category ordinal scales and the profile test.