This master thesis deals with the assessment of selected fragrant substances in cosmetic products. At the beginning the occurrence, methods of acquiring and application of these substances is described. They are essential components primarily in cosmetic products, however they can cause an allergic reaction in sensitive individuals. The theoretical part of this thesis also describes the cause and the progress of these undesirable effects. There are several hundreds, up to thousands fragrant substances used in the perfume industry, from which 26 was designated by the European regulations as potential allergenic fragrant substances and their content is regulated. Legislative standards as well as the overview of the methods used to determine these fragrances are given here. The experimental part is focused on the development and validation of the separation methods for determining of the selected and potentially allergenic fragrant substances. The method used was a solid phase microextraction using Carboxen/Polydimethylsiloxane fiber combined with a gas chromatography coupled to a flame ionization detector (SPME-GC-FID). Amylcinnamyl alcohol, benzyl alcohol, cinnamyl alcohol, coumarin, lyral, ?-isomethyl ionone were among the determined allergenic substance. Consequently, this method was also applied on 10 selected cosmetic products specimens, in which the linalool and geraniol were identified as the most common allergenic substances.

This diploma thesis is focused on aromatic substances occurring in food. The theoretical part describes their characteristics, the use of fragrances of plant origin for flavoring of food and points to their possible negative effects on the human organism. Twenty six potentially allergenic fragrances are thus identified in European legislation and an overview of their physical properties, occurrence and use is also processed in this work.The aim of the experimental part was to develop and validate a method for assessment of fragrances using headspace solid phase microextraction combined with gas chromatography (HS-SPME-GC-FID). The following parameters have been validated : repeatability, linearity, limits of detection (LOD) and limits of quantification (LOQ). The HS-SPME-GC-FID method was finally applied to selected samples of foods commonly available on the market.

This diploma thesis is focused on the problematic of assessment of 26 most important allergenic aroma compounds in foods, flavoured herbal teas were chosen as the model samples. Aroma is the one of the main characteristics of tea, which is closely linked to taste and odour. The theoretical part of this work is focused on the characteristics of tea, tea types, producing technology, classification according to the fermentation and also their undeniable impact on the human organism. In the experimental part, the allergenic aroma compounds in 10 chosen samples of flavoured tea were identified and quantified using the solid phase microextraction (SPME-GC-FID) in conjunction with gas chromatography. The work also includes sensory evaluation of taste and smell of tea samples by qualified assessors.

Ce travail décrit les équilibres gaz-liquide lors des fermentations alcooliques en conditions œnologiques, en se focalisant sur les composés d'arôme les plus abondants : isobutanol, alcool isoamylique, acétate d'éthyle, acétate d'isoamyle et hexanoate d'éthyle. Les coefficients de partage à l'équilibre (ki) de ces molécules sont quantifiés, grâce à la méthode PRV (Phase Ratio Variation), en précisant l'effet de la composition du milieu et de la température. Grâce à la mise en œuvre de fermentations spécifiques pendant lesquelles la vitesse de dégagement de CO2 est contrôlée (grâce à une perfusion d'azote ammoniacal), il a été montré que le dégagement de CO2 n'avait pas d'effet sur le rapport de concentrations entre phase gaz et liquide et pouvait être assimilé au ki. Une démarche de modélisation est ensuite effectuée, pour estimer la valeur du rapport de concentrations entre phase liquide et gaz pour ces composés (à l'exception de l'acétate d'éthyle et de l'alcool isoamylique), à tout moment de la fermentation et quelle que soit la température, y compris en conditions de non isothermie. Le modèle, basé sur l'équilibre des phases gaz et liquide, conduit à une erreur moyenne d'estimation inférieure à 10%. Grâce à ce modèle, il devient possible de réaliser des bilans de production des différents composés tout au long de la fermentation, à partir de leur seule mesure dans la phase gaz. Ces bilans permettent de différencier (i) la quantité globale produite, représentative des potentialités de la levure (intérêt microbiologique), (ii) la quantité restant dans la phase liquide (intérêt organoleptique) et (ii) la quantité perdue dans le gaz effluent (intérêt technologique). Il est ainsi mis en évidence que les pertes d'esters sont très importantes. Par exemple, à 20°C, elles atteignent respectivement 44 % et 25 % pour l'hexanoate d'éthyle et l'acétate d'isoamyle. Grâce à un dispositif de suivi en ligne permettant des mesures très fréquentes (une par heure), les vitesses - et les vitesses spécifiques - de production et de pertes sont calculées. Elles constituent de nouvelles informations utiles à la fois pour l'étude du métabolisme (suivi de la dynamique de flux métaboliques) et pour mieux raisonner les conduites de fermentation, notamment le régime de température. L'impact de ce régime de température est étudié plus en détail en réalisant des bilans de production lors de fermentations conduites avec la même souche de levure et le même moût. Les résultats obtenus montrent que si l'on ne prend en compte que les concentrations dans la phase liquide - généralement les seules informations disponibles - on surestime fortement l'impact de la température sur le métabolisme de composés fortement volatils, tels que les esters / The gas-liquid partitioning during winemaking fermentations was studied, with a focus on the main aroma compounds: isobutanol, isoamyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate. The partition coefficients (ki) of these molecules were quantified, using the PRV (Phase Ratio Variation) method. The influence of the must composition and temperature was assessed. The absence of any effect of CO2 production on gaz-liquid ratio compared to ki value was established by running specific fermentations in which the rate of CO2 production was kept constant by perfusion with assimilable nitrogen. A model was then elaborated to calculate gaz-liquid ratio of these molecules (excepted ethyl acetate and isoamyl alcohol) at any fermentation progress and at any temperature, including anisothermal fermentations. The model based on the equilibrium between the gas and liquid phases predicted ki with less than 10% error. Using this model, balances were c alculated, with a differentiation between (i) the total production, representative of the yeast potential (microbiological interest), (ii) the amount remaining in the fermenting must (organoleptic interest) and (iii) the amount lost in the exhaust CO2 (technological interest). High losses of esters were observed. For example, at 20°C, they represented 44% and 25 % for ethyl hexanoate and isoamyl acetate, respectively. Using an on line monitoring with a high frequency of measurements (one per hour), rates and specific rates of production were calculated. These new data are useful both for studies on metabolism (dynamics of metabolic fluxes) and for improving fermentation control, in particular temperature profile. The impact of temperature was assessed in more detail by comparing balances of production during fermentations run with the same yeast strain and must. These experiments demonstrated that the effect of temperature on the yeast metabolism was highly overestimated whe n only considering the concentrations in the liquid, i.e. usually the only available information.

Orientador: Glaucia Maria Pastore / Tese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia de Alimentos / Made available in DSpace on 2018-08-06T19:14:01Z (GMT). No. of bitstreams: 1 MarosticaJunior_MarioRoberto_D.pdf: 758713 bytes, checksum: a3f5c7bf4942f073b9a52b841245b3e6 (MD5) Previous issue date: 2006 / Resumo: Este trabalho teve por objetivos o estudo da biotransformação de terpenos e avaliação de suas propriedades biológicas. A biotransformação de limoneno foi realizada por uma linhagem de Fusarium oxysporum cultivada em manipueira e transferida para meio mineral, sendo o óleo essencial de laranja, um resíduo da indústria do suco de laranja, a fonte do limoneno. Rendimentos da ordem de 450 mg/L de a-terpineol, o principal produto obtido, foram alcançados. Da mesma forma, a biotransformação do citronelol foi conduzida por uma linhagem de Penicillium sp. cultivada em manipueira e transferida para meio mineral. O principal produto obtido foi o cis-óxido de rosa em concentrações da ordem de 70 mg/L. A seleção de microrganismos biotransformadores de limoneno (cuja fonte foi óleo essencial de laranja) a- e b-pinenos (cuja fonte foi terebentina, resíduo industrial da indústria de papel) foi realizada por microextração em fase sólida (MEFS). A técnica mostrou-se eficaz para a recuperação de voláteis presentes no 'heapspace¿ de culturas esporuladas de superfície para a biotransformação. Os microrganismos selecionados por MEFS foram submetidos à biotransformação em cultura líquida e produção da ordem de 50 mg/L de verbenol por Mucor sp. 2276 e 70 mg/L de verbenona resultaram da biotransformação de a- e b-pinenos. Aspergillus sp. 2357 e Penicillium sp. 2360 produziram aproximadamente 90 e 10 mg/L de a-terpineol e álcool perílico respectivamente. A biotransformação de a-farneseno por linhagens de Aspergillus niger gerou compostos nunca relatados anteriormente na literatura. Quatro produtos principais foram obtidos. Apenas um composto pôde ser identificado por meio de CG-EM como 6-OH-farneseno. Análises de CG-olfatometria descreveram 6-OH-farneseno como aroma cítrico impactante. Estudos 'in vitro¿ e 'in vivo¿ com extrato da biotransformação de limoneno por Fusarium oxysporum e com padrões de monoterpenos revelaram o potencial desses compostos em atuarem como antioxidantes, gerando uma possibilidade para esses compostos serem utilizados industrialmente como aromas funcionais / Abstract: The biotransformation of terpenes and their functional properties were investigated in this study. The biotransformation of limonene was done by a Fusarium oxysporum strain grown in cassava waste water and transferred into a mineral medium for biotransformation. The limonene source was an orange essential oil from a orange juice industry. The main biotransformation product was a-terpineol, reaching around 450 mg/L. Similarly, biotransformation of citronellol was conducted by a Penicillium sp. strain grown also in cassava waste water and transferred into a mineral medium. The main product was cis-rose oxide, reaching concentrations higher than 70 mg/L. The screening of microrganisms for biotransformation of limonene (from orange essential oil) and a-, b-pinenes (from turpentine oil, residue from pulp industry) was done by solid phase microextraction (SPME). The technique was effective for the recovery of the volatiles from the headspace of sporulated surface biotransformation cultures. Liquid culture biotransformation experiments performed with the SPME screened strains resulted in the production of 50 mg/L of verbenol by Mucor sp. 2276 and 70 mg/L of verbenone form a-, b-pinenes and 90 mg/L of a-terpineol by Aspergillus sp. 2357 and 10 mg/L of perillyl alcohol by Penicillium sp. 2360. The biotransformation of a-farnesene by Aspergillus niger strains resulted in compounds never described in the literature before. Four main new compounds were obtained. Only one of them could be identified by GC-MS as 6-OH-farnesene. CG-O experiments revealed the impactant citrus aroma of 6-OH-farnesene. 'In vitro¿ and 'in vivo¿ experiments with the limonene biotransformation extract by Fusarium oxysporum and with the monoterpene standards present in the extract revealed the antioxidant potential of these compounds, which open a new perspective for the utilization of these compounds as functional aroma compounds / Doutorado / Doutor em Engenharia de Alimentos

The aim of this diploma thesis was to determine the optimal extraction conditions for obtaining an extract from the plant Plectranthus amboinicus. Plectranthus amboinicus is an aromatic herb of the Lamiaceae family containing a large number of bioactive compounds. Because of this, it has a number of biological effects – antimicrobial, anti-inflammatory, antioxidant, analgesic, etc. To maintain the maximum of sensory and nutritionally valuable components of P. amboinicus, a simple maceration of fresh chopped herb was chosen. Maceration was performed under the following conditions: 40 minutes at 40 ° C, solvent 40% ethanol, weight 20 g of herb per 100 ml of solvent. The extract prepared under these optimal conditions was comprehensively characterized in terms of the content of total polyphenols, their concentration was determined to 0,08 ± 0,02 mgGEA·ml-1, which corresponds to 0,40 ± 0,07 mgGEA·g-1 of the plant. The antioxidant activity of the extract was 241,24 ± 29,24 µgTEAC·ml-1 and the radical scavenging activity of ABTS•+ was determined to be 49,29 ± 5,97 %. The antimicrobial activity was verified by the agar well diffusion method. Two types of bacteria were selected for the determination – gram-positive Bacillus cereus, gram-negative Escherichia coli and yeast Candida glabrata. The results showed that the extracts have the highest antimicrobial activity against B. cereus. There were 64 volatile aromatic compounds identified in the extract, with monoterpenes and sesquiterpenes dominating. The obtained results confirm that P. amboinicus, or its prepared extract, has a good potential for use as a new and non-traditional flavor in various foods and delicacies, which can also increase their nutritional value.

Tetradenia spp. is herb naturally growing in Africa and is part of family called Lamiaceae. The herb is used in traditional medicine to cure malaria, angina or as treatment for tropical skin diseases. Maceration was chosen from number of extraction methods, to obtain bioactive compounds from this plant. Optimization was performed with aim to retrieve as much of bioactive compounds as possible. Optimal conditions chosen were: temperature 60 °C, extraction time 40 minutes, solvent 40% ethanol and solid-solvent ratio 1:5. In total 63 aromatic active compounds were found in optimal extract. Terpenes were the most abundant (88,60 %), from them oxygenated monoterpenes (55,65 %) and monoterpenes (29,52 %). Compounds with highest percentage quantity were camphor (51,76 %), cis--ocimene (8,17 %), 3-octyl acetate (7,71 %), trans--ocimene (6,76 %), -terpinene (4,93 %), o-cymene (3,81 %), terpinolene (1,33 %), limonene (1,33 %), camphene (1,19 %) and borneol (1,20 %). Further, total phenolic content was 0,31 ± 0,02 mgGAEml-1, which equals 1,52 ± 0,11 mgGAEg-1 of plant. Antioxidant activity was 417,56 ± 32,84 gTEACml-1 and percentage of radical scavenging activity ABTS•+ was 88,99 ± 7,00 %. Finally antimicrobial activity was determined against bacteria Bacillus cereus, Escherichia coli and yeast Candida glabrata. Against E. coli and C. glabrata there was no inhibition exhibited. Against B. cereus there was seen mild inhibition activity. The results confirm that Tetradenia spp. contain a number of interesting aroma active compounds, which shows antioxidant and antimicrobial activity. The herb has a good potential as natural source of nutritious and sensory active compounds to be used into various foods.

This master´s thesis deals with production and characterization of fresh cheese with addition of herb extracts, specifically extracts from Plectranthus amboinicus and Echinacea purpurea. The purpose of this thesis was to prepare samples with higher sensory quality and nutritional value. Produced cheeses were characterized in terms of volatile (aroma) substances, fatty acid content, total phenolic substances, antioxidant activity and sensory quality. Cheese sample with added extract from E. purpurea reached the highest value of total phenolic compounds (0,172 ± 0,019 mgGAEg-1 of cheese) and antioxidant activity (91,2 ± 2,2 gTEACg-1 of cheese). Cheese sample with added extract from P. amboinicus, compared to standard cheese sample (without added extract) also reached higher values of total phenolic compounds and antioxidant activity. 43 volatile (aroma) compounds were identified in both samples with added extracts (P. amboinicus, E. purpurea), in standard cheese sample it was 33. In sample with E. purpurea camphor was present in high amount (15,23 %) responsible for the camphor aroma, camphor was also identified in small amount in sample with P. amboinicus. Highest volatile matter content was identified in sample with P. amboinicus. Standard cheese sample was rated as the best from the sensory perspective. Addition of extracts had negative effect on color, taste, and aroma perception of cheese. Strongest herbal taste was identified in sample with E. purpurea, brownish color of this sample manifested in lower pleasantness of color. Obtained results show, that extract addition increases the nutritional value of cheese (higher content of aromatic substances and phenolic compounds, higher antioxidant activity), but lowers sensory quality and overall consumer acceptability.

This diploma thesis deals with the optimization of jelly candies production, application of herbal extract to produced candies, and subsequent characterization of produced samples in terms of volatile (aromatic) substances, total phenolic substances, antioxidant aktivity, and sensory quality. Optimization parameters – the amount of gelatin and the addition of citric acid, were selected based on the sensory analysis. Additions of 7,5 % gelatin and 2 % acid were proven to be optimal. The sources for the production of herbal extracts were the plants Aronia melanocarpa and Echinacea purpurea, which are known for their high content of bioactive substances. The further sensory analysis determined the optimal amount of extract added to jelly candies samples – in the case of chokeberry it was 4 % and in the case of echinacea it was 1 % of the extract. In the sample with chokeberry extract of optimal composition, ie 7,5 % gelatin, 2 % citric acid, and 4 % extract, 46 volatile substances were determined, of which nonanal (12,17 %) and thymol (8,70 %) were the most represented, the total polyphenol content was 472.88 ± 8.02 gGAEg-1 of the sample and the antioxidant activity was determined to be 828.99 ± 17.74 gTEACg-1 of the sample. The sample with echinacea extract of optimal composition, ie 7,5 % gelatin, 2 % citric acid and, 1 % extract, contained 56 volatile substances, the most represented being nonanal (12,08 %), thymol (6,19 %), and decanal (5,52 %). The total polyphenols in this sample were determined to be 291.09 ± 10.17 gGAEg-1 of the sample and its antioxidant activity was determined to be 850.91 ± 30.29 gTEACg-1 of the sample. Samples with the addition of chokeberry extract, which gave the confectionery a fruity, slightly sour taste and a pink to dark purple color, were considered more pleasant/acceptable; samples with echinacea had an herbal aroma and taste and orange color.

This master thesis deals with preparation of extracts from fruits of aronia, optimization of conditions for extraction and subsequent characteristics of the obtained optimal extract. In the theoretical part information about the botanical characteristics of Aronia melanocarpa and about its utilization are mentioned. Furthermore, the chemical composition of aronia fruits is described and the main biologically active substances contained in the plant are described. At the end of the theoretical part extraction and separation techniques, determination methods of antioxidant, antimicrobial activity and determination of aromatic active compounds are described. The experimental part describes the optimization of maceration so that the macerate contains as much polyphenolic substances as possible, as well as aromatic active substances. 40% ethanol, at a temperature of 60 ° C, with a weight solvent ratio of 1: 5, for 40 minutes proved to be optimal for the maceration of aronia fruits. The total polyphenol content of the optimal extract was determined to be 5237.2 ± 40.7 mgGAEkg-1 and the antioxidant activity by TEAC to be 512.5 ± 5.04 gml-1. 24 aromatic active compounds were identified in the extract, with the largest percentage being monoterpenes and aldehydes. Furthermore, it was found that the extract did not show antimicrobial activity against the microorganisms used (Bacillus cereus, Escherichia coli and Candida glabrata). The obtained results confirm that aronia extracts are an important source of many biologically active compounds and can be used in food as a natural source of nutritionally and sensory valuable substances.