CROMATOGRAFIC ANALYSIS (2)

Author: Rodriguez Avila José Antonio.
Year: 2004.
University: VALLADOLID [www.uva.es].
Place of defense: Sala de Grados, Facultad de Ciencias.
Place of preparation: Universidad de Valladolid.

Summary: This paper describes the synthesis of new materials by the sol-gel route, including iron oxides, in order to potentiate the effect of the compounds adsorbent separately (silica-gel and iron oxides), as well as take advantage of advantages of magnetic properties, in the case of Fe3O4. The compounds were characterized by chemical analysis, X-ray Diffraction (XRD), infrared spectroscopy (FTIR-ATR), Laser Scattering, Micro-Raman, thermal analysis (DSC) and scanning electron microscopy (SEM-EDX), may established you get oxihidróxido iron embedded in silica gel in one case and silica gel embedded in magnetite in another. The first material (FeOOH.SiO2) is a material that has a high affinity toward retention arsenate ion, which has allowed it to incorporate material in the development of an electrode potenciométrico selective As (V) and conventional tubular geometry easily plug in a system in flow injection analysis. The evaluation of the variables that affect the response generated by the electrodes are optimized through different procedures optimization. It is used as an objective function, obtaining adequate sensitivity and reproducibility. The results obtained using the devices and proposed methodologies are compared with those obtained by a referral process. In all assays are encuentró that the results provided by the two methods are comparable, highlighting the advantages of the procedures developed, as are possible in situ analysis, economics, sampling rate and the possibility of automation. For its part the material composed of silica gel embedded in magnetite was used as a packing material for HPLC column chromatography, a technique for generating separation novel called Magneto-Cromatografía of Liquid High Resolution (HPLMC by its acronym in English), which proved useful in the separation of analytes in the paramagnetic dissolution. This technique has been successfully used in the analysis of eight different amino acids in wine. Finally, using discriminant analysis of the results, it was possible to classify the wines according to their origin.

Author: COMAS LOU ENRIC.
Year: 2004.
University: ROVIRA I VIRGILI [www.urv.cat].
Place of defense: FACULTAT DE QUÍMICA.
Place of preparation: FACULTAT DE QUÍMICA.

Author: MARTÍ BORRAS M. PILAR.
Year: 2004.
University: ROVIRA I VIRGILI [www.urv.cat].
Place of defense: FACULTAT DE QUIMICA.
Place of preparation: FACULTAT DE QUIMICA.

Summary: ABSTRACT work in this thesis deals with the study and characterization of the aroma of wine through the implementation of two important techniques in this field such as chromatography gases-olfatometría (GCO) and the electronic nose based on mass spectrometry. The former has developed a method that uses microextracción in solid phase (SPME) to obtain aromatic extracts wine and which determines the potency of aromatic compounds odoriferous through a new modality of technical Aroma Extract Dilution Analysis (AEDA). In the case of the electronic nose has been studying the application of this technique to different aspects related to the determination of the quality aromatic wine such as quality control from different wine parameters (range, origin and time of aging) process control ripening grapes and winemaking and determination of 2,4,6-tricloroanisol, the main aromatic compound responsible for the defect "like to cork." On the other hand technique has been applied successfully to the determination of time of aging spirits sugarcane, as well as the determination of aromatic intensities of different descriptors that are evaluated in the sensory analysis of this kind of drinks.

Author: CARO RUBIO ESTER.
Year: 2004.
University: ROVIRA I VIRGILI [www.urv.cat].
Place of defense: FACULTAT DE QUIMICA.
Place of preparation: FACULTAT DE QUIMICA.

Author: BUSTOS VÁZQUE GUADALUPE.
Year: 2004.
University: VIGO [www.uvigo.es].
Place of defense: FACULTAD DE CIENCIAS DE OURENSE.
Place of preparation: FACULTAD DE CIENCIAS DE OURENSE (UNIVERSIDAD DE VIGO).

Summary: This thesis has tried to seize two residues from agro-industrial sector in wine for obtaining important additives in the food industry, such as lactic acid and biosurfactantes. On the one hand have been used lees or sludge from different stages of wine from white wine and red wine (distilled and distilled without) for use as a source of nutrients for the biotechnological production of ác. Lactic by lactic acid bacteria. The biotechnological production of acid usually takes place with lactic acid bacteria, but the species of Lactobacillus have high nutritional requirements, it is necessary to find new nutrients as well as low-cost sources of carbon alternatives to synthetic glucose. This marked the lees and used as a source of nutrients. Once evaluated the lees as nutrients, we proceeded to break pruning of optimal spirits are suplementaron with nutrients and fermentaron with L. Pentosus (one of the few strains of Lactobacillus capable of fermenting pentosas). In order to increase the concentration of hidrolizdos to increase the amount of sugars initials. Experiments were carried out additional ocn synthetic sugars to study the possible inhibition that the concentration of hydrolysates could exert on the L. Pentosus. In addition, depending on the results related potential metabolic pathways used by L. Pentosus with the consumption of different sugars hemicelulósicos. During the prehidrólisis generates a solid waste with a high cellulose content. This waste is treated with NaOH to increase the digestibility of the cellulose and studied the effects of temperature, reaction time and concentration of NaOH in the composition and sensitivity of the hidróliisis enzyme of solid waste. The cellulose obtained in optimum conditions of treatment, passed for a statistical model, underwent SSF processes for the biotechnological production of lactic acid with L. Rhamnosus. As an industrial level are more effective processes carried out in continuous processes in batch, we proceeded to explore obtaining continuous lactic acid and biosurfactantes extra and intracellular, from liquor hemicelulósicos and using different flows operation. To estimate the potential problems that could result lees of winemaking in the recovery of lactic acid in the media fermentativos using lees vinification as nutrients, lactic acid, recovered from the middle of fermentation using an ion exchange resin (Amberlite IRA 400) .

Author: SANCHEZ RABANEDA FERRAN.
Year: 2004.
University: BARCELONA [www.ub.es].
Place of defense: FACULTAD DE FARMACIA.
Place of preparation: FACULTAD DE FARMACIA.

Summary: With the aim of being able to recycle waste from agricultural and food industries of agricultural surpluses to obtain plant extracts with a possible industrial application has been evaluated yields extraction (using different organic solvents) and the antioxidant activity of different materials raw vegetable. Extracts of greatest interest to the industries that produce plant extracts were selected on the basis of the results obtained in the various tests conducted antioxidant activity, but also in terms of different factors, related to the process of obtaining the plant material, its subsequent treatment in the extractive industries, and the potential commercialization of final statement. In the first phase have been selected waste of pear, apple, artichoke, tomato and golden rod. These materials are extracted again with mixtures of agua - etanol and agua-acetona, and then were purified with butanol and butanona. The most promising extracts obtained in this first phase (excerpt apple made with acetana of 80% and purified with butanona, artichoke extract made from 50% ethanol and purified with butanona and extract gold stick made with acetone for 80% and purified with butanol) have been performed later at plant pilito, again subject to the tests of antioxidant activity. In order to relate the antioxidant activity of the extracts with its content in phenolic compounds, it has successfully developed a method of analysis by liquid chromatography coupled with mass spectrometry, which has identified a large number of phenolic compounds presentaes in the extracts, both minority and majority.

Author: Concha Herrera Victoria.
Year: 2004.
University: VALENCIA [www.uv.es].
Place of defense: Facultat de Química.
Place of preparation: Facultat de Química.

Summary: The primary protein amino acids are a particularly complex set of compounds under the analytical point of view. Their role as essential constituents of living matter implies that the analysis should always extend to the entire series, which concludes the need for separation techniques powerful, able to conveniently isolate signals of each and every one of the 19 analytes potentially in any sample. This explains the prevalence of chromatographic methods for analysis. Both the primary amino acid protein as its derivatives are particularly under various chromatographic perspective, making separations based on the elution isocrática in virtually inapplicable. This ineffectiveness emerge as alternatives, either using gradient elution, or chromatographic methods capable of attenuating the differences polarity. To date, there has been fully resolved in a manner satisfactory to the various problems posed by the analysis of these compounds. This thesis is trying to answer some of them, especially the improvement of chromatographic separations, with the help of mathematical techniques. The Memory Doctoral Thesis consists of three parts: The first part examines the reaction derivatizante more prevalent in reverse phase liquid chromatography for the analysis of amino acids, which form isoindoles using a mixture of o-ftaldehido and a thiol. These derivatives can be separated and detected easily. However, the nature of thiol heavily influence on the kinetics of formation and degradation, resulting in a first study examined the characteristics of the reaction with 10 thiol. Colateralmente, an application was developed in which the analyte was himself thiol, instead of the amino acid. The second part focuses on improving the chromatographic separation techniques quimiométricas. On the one hand, sought to reduce the errors produced in the modeling retention due to problems in the preparation and storage of mobile phases. To make the correction has proposed the use of reference compounds, thereby errors usually below 1%. The availability of very precise predictions led to the optimization of the separation gradient multilineal with high reliability. It proposed a measure that predicts the maximum capacity resolutiva chromatographic system, and that can be used to determine how long it is worth increasing the complexity of the gradient. However, there is no point in proposing conditions of separation impossible to reproduce in the chromatograph. In response, it was proposed a measure robust resolution, which includes errors propagated by the model of retention. The thesis concludes by comparing the procedures completed for chromatographic analysis of the primary amino acid protein, in all cases based on elution phase reverse. These procedures were implemented with the same instrumentation and applying the same techniques of optimization. First, we studied in detail the most widespread chromatographic procedure, which uses phases acuo-orgánicas. Specifically, comparing the characteristics of the two most common solvents: methanol and acetonitrile. For his greatest strength eluent (which makes it possible to reduce the consumption of solvent), and greater efficiencies (which translates into slightly higher resolutions), acetonitrile is preferable, in combination with a gradient trilinear. This chromatographic procedure is then compared with four other alternative. The study took into account the fact that outside the detection, there are other issues of great practical significance, such as the use of experimental conditions too firm (which reduce the life of colu 8 mnas), and 53e l risk to produce serious damage to the instrumentation, obtaining improper deductions (too short or too long, either for all or only for some compounds), or insufficient resolution. The procedures were considered: the elution of free amino acids forming ionic pairs with acids trifluoroacético and pentadecafluorooctanoico detection evaporative light scattering, and the elution with half micelar hybrid dodecilsulfato sodium and propanol derivatization with pre - and post-columna and UV detection. The procedure conventional acuo-orgánico with a gradient multilineal acetonitrile was the one who showed better overall performance.

Author: Ventura Benítez Meritxell.
Year: 2004.
University: RAMÓN LLULL [www.url.edu].
Place of defense: Escuela Técnica Superior IQS.
Place of preparation: Escuela Técnica Superior IQS.

Summary: This thesis focuses on the study of toxins produced by fungi of the genus Aspergillus and Penicillium, more specifically aflatoxins B1, G1, B2, G2 and ochratoxin A. The work focuses on two areas of activity: production and analysis of mycotoxins, both within the framework of food security. From the standpoint of production, we want to know the factors influencing the development of ochratoxin A by a strain micotoxigénica so as to minimize the impact of this toxin in food. Within this field of research, which studies the influence exercised A. And A. parasiticus Ochraceus on its production of aflatoxins B1, G1, B2, G2 and ochratoxin A, respectively. To do so, their behavior is evaluated when both strains were incubated separately and together in the same substrate for different days of incubation. From the analytical standpoint, we want to have a method for the simultaneous analysis of toxins interest in arrays of plant origin, and which are the most commonly presented this pollution. First, it develops a methodical analysis for the determination of aflatoxins B1, G1, B2 and G2 in a medicinal plant, Rhamnus purshiana by solid phase extraction and filling polymeric high performance liquid chromatography with a reverse-phase column ultra - quickly. It uses a mass spectrometer for cuadrupolo simple as detector. The method is applied to the analysis of samples of R. Purshiana inoculated with a strain aflatoxigénica to assess whether this is a good substrate for the development and subsequent fungal toxin production. Subsequently, it optimizes the analysis of ochratoxin A in coffee through two analytical techniques, thin layer chromatography and high performance liquid chromatography with fluorescence detector reverse-phase column and small diameter. The confirmation of the toxin is carried out by mass spectrometry of cuadrupolo simple. In the latter method, the sample preparation stage is performed by solid phase extraction in cushioning polymer. Furthermore, it evaluates the production capacity of ochratoxin A strains of Aspergillus and Penicillium isolated from samples of coffee. Finally, we have developed two methods that allow simultaneous analysis of aflatoxines B1, G1, B2, G2 and ochratoxin A in samples of beer. One of the methods used high performance liquid chromatography coupled with a mass spectrometer of cuadrupolo simple. The other method, applied a new chromatographic technique called liquid chromatography coupled to an ultra-resolution mass spectrometer triple cuadrupolo. Both methods use the same development stage shows, a solid phase extraction in cushioning polymer. On the other hand, evaluates the production capacity of aflatoxins B1, G1, B2, G2 and ochratoxin A by strains of Aspergillus and Penicillium previously isolated from samples of maize, rice, barley and malt, used in brewing

Author: SANTOS SANZ MARÍA.
Year: 2004.
University: VALLADOLID [www.uva.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: By-products from processing plants plant products for food and drinks represent a major problem for the industry because of the high volume of waste generated and its high moisture content makes them highly perishable. These residues are bagasse brewer and the by-products of processing industry apple and peach juice. With a view to obtaining industrial value-added products from waste bagasse malt barley, there has been a partnership between the Department of Analytical Chemistry, Faculty of Sciences, the Institute of Industrial fermentation CSIC And the company Mahou SA to explore the influence of two processes of eliminating moisture (drying and freeze-drying) bagasse in its overall composition and obtain at laboratory level, two items of interest in industry, arabinose and xylose through a commercial enzyme hydrolysis with low cost. The result of this collaboration is the work that is presented, which performs a characterization of bagazos generated in the industry following a series of basic parameters (moisture, ash, fat, protein, reducing sugars and metals), it determines the number of arabinose and xylose that contain, we studied the influence of drying and freeze-drying in the value of these parameters, and assesses the production of arabinose and xylose with different enzyme preparations, all of which has been necessary to adapt and verify the corresponding analytical methods. It is also reflected in this report obtaining value-added products through enzymatic hydrolysis from bagazos apple and melocotó1l supplied by Indulérida SA, which is also seen as a procedure for removing moisture. This will determine the concentration of its major monosaccharides: glucose and fructose in addition to the minority: xylose and arabinose and the estimated. Capacity release of monosaccharides besides arabitol and inositol, with antioxidant activity by the same enzyme preparations. Thus, we obtain that bagazos brewers contain, as expressed on average dry weight: 3.4% ash, 4.4.% Matería fat, a 24.2% protein, 8.3% of arabinose and a 15.6% xylose. The processes tested to reduce moisture bagasse reduce the fat and protein at a level close to 2%, was observed large variations in the content of arabinose and xylose according to the m090 to retain bagasse. The mineral content of lots of bagasse is the most distinguishing feature among them. Enzymes Ultraflo L Lallzyme MP and Lallzyme OE are most appropriate to release pentosas of bagazos brewers, providing more than 26% and 45% of the total content of xylose and arabinose, respectively. By enzymatic hydrolysis with 130 mU of Ultraflo Ly 16 hours of incubation, it gets rid between 0.2% and 0.4% of xylose of bagazos fruit, and approximately 4.0% and 2.6% of arabinose of apple products and peach respectively. The concentration of glucose in the enzyme hydrolyzed fruit is high, ranging between 8.3% bagasse Peach and 17.0% in dietary fiber apple. To obtain xylose and arabinose by enzymatic hydrolysis, the largest concentrations are achieved in bagasse malt barley. While in obtaining glucose is preferable to the use of dietary fiber apple. The bagasse and dietary fiber, 8 melo 495 cotón there is a 5.4% and 10.3% fructose in a free, respectively, which represents a share of 46% and 67% of the total content. However, the by-products of the apple fructose concentration is 8%, which represents a percentage from 1 00% of the total content. The hidrolízados enzymatic of bagazos fruit of apple and peach contain small amounts of arabitol and inosítol, less than 0.2%, which were not detected in bagazos brewers.

Author: PADRÓN SANZ CAROLINA.
Year: 2004.
University: LAS PALMAS DE GRAN CANARIA [www.ulpgc.es].
Place of defense: FACULTAD DE CIENCIAS DEL MAR.
Place of preparation: FACULTAD DE CIENCIAS DEL MAR.

Summary: In this Doctoral Thesis arises as objective optimization and development of new methodologies and extraction preconcentration of two families of compounds pollutants: Dioxins of, and organophosphate pesticides present in environmental samples of a different nature, using the media micelares as extractantes. The use of the means micelares is a highly desirable alternative to conventional methods employed for the analysis of such substances because it is faster methodologies, simple economic and less damaging to the environment because of their biodegradability. In the development and optimization of these methodologies (Point Cloud for the extraction of compounds from liquid samples) and (Microwave Assisted Extraction for the extraction of compounds from solid samples) determining the most suitable conditions for the extraction of these substances and their chromatographic separation technique using as the high performance liquid chromatography reversed phase. It identifies the analytical parameters of the proposed methodologies, and are validated by comparing the results with those found by other extraction techniques, or through their application to the collection and analysis of mixtures certified. From the results of various studies conducted in this PhD thesis demonstrates that the methodologies developed extraction procedures are perfectly valid for the extraction and preconcentration of dioxins and pesticides present in both liquid and solid samples. Moreover, the results that are obtained are comparable to those of other traditional methods of extraction. And, have shown their great applicability, being equally efficient in extracting and preconcentrar the analytes in the study, samples of different characteristics and / or treatment.

Author: JARAUTA GURRÍA IDOIA.
Year: 2004.
University: ZARAGOZA [www.unizar.es].
Place of defense: FACULTAD.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: The work of this report has attempted to combine the results of practical interest for the winemaker and the world of oenology with the generation of scientific knowledge. To achieve this it is working on three levels. Firstly the launch of two analytical methods for determination of original components of importance in the aroma of wine and parenting as are aliphatic lactones and enolonas (sotolón, furaneol and maltol). Both methods are based on using solid phase extraction with subsequent determination by gas chromatography coupled with mass spectrometry. Second is trying to understand the basic chemistry of the perception addressed in a simple study of the role played by certain groups of aromatic compounds in the aroma of wine aging checking the sensory effect of the interaction between some aromatic compounds and studied the effect the existence of complex non-volatile aromatic characteristics. And finally analyzed the volatile aromatic composition of a large number of samples established patterns of behavior associated with the process of aging in barrels and the use of different oak barrels.

Author: Bagó Lacida Bárbara.
Year: 2005.
University: RAMÓN LLULL [www.url.edu].
Place of defense: Escuela Técnica Superior IQS.
Place of preparation: Escuela Técnica Superior IQS.

Summary: TITLE: ANALYSIS OF VARIOUS ORGANIC POLLUTANTS IN FANGO OF DEPURADORA AND STUDY OF ITS STATUS IN THE PROCESS OF POSTTRATAMIENTO SUMMARY: We have developed and optimized different methods for the analysis of various organic pollutants (biogenic amines, NPEOs, PAHs, LAS, DEHP, dinitroacetaphenone HHCB and AHTN) in samples of sludge from wastewater treatment plant. In most cases, the methods proposed and validated improve time analysis over previous methods, both from the point of view chromatographic, as in the development stage shows. The results show that, in some cases, the values of pollutants studied are above the limit proposed in the draft European legislation, as well as composting and drying heat are two effective mechanisms to reduce the level of pollutants in these products. KEYWORDS: FANGO OF DEPURADORA, PROCESSES OF POSTTRATAMIENTO OF FANGOS, COMPOST, HRGC, HPLC.

Author: Quiñones Torrelo María del Carmen.
Year: 2005.
University: VALENCIA [www.uv.es].
Place of defense: Facultad de Química.
Place of preparation: Facultad de Química.

Summary: In the development of new drugs application of combinatorial chemistry allows optimization of the pharmacokinetic and pharmacodynamic characteristics of the compounds "seed" of the various therapeutic groups. In this process, the pharmaceutical industry faces the need to assess quickly and inexpensively a large number of molecules with potential biological activity for decisions regarding what should be excluded molecules in the early stages and which compounds should be developed. The evaluation of new molecules is based on the results of the tests "in vivo", but for ethical reasons and practices, recently being developed new methodologies and the tests in vitro, mathematical models such as those based on quantitative relationships Structure "QSAR models" or quantitative relationships retención-actividad "models QRAR" intended to replace or at least reducing the use of experimental animals. This dissertation is framed in the area QRAR, with an incursion into the area QSAR using neural networks, and focuses on the drugs to action at the central nervous system, CNS. To measure the retention of drugs neuroactivos using a chromatographic system based on liquid chromatography micelar. The stationary phase is a column octadecilsilano and as a mobile phase used dissolutions surfactant Brij35 in terms of pH, ionic strength, temperature and osmotic pressure that reproduce physiological conditions in which the division takes place when a drug is administered to a living organism. In this chromatographic technique we called chromatography Micelar of Bio-reparto (CMB). The work carried out was part of a line of investigation, Department of Analytical Chemistry focuses on the development and evaluation systems "in vitro" based on chromatography techniques as an alternative to animal experiments for the evaluation of new drugs. In this context the objeticos it seeks to achieve in this thesis are: Â evaluate the efficacy of chromatography micelar of bio-reparto (CMB) as a technique in vitro alternative to traditional methods to estimate pharmacokinetic and pharmacodynamic properties of different families of compounds that act on central nervous system, such as antidepressants, antihistamines and opioid analgesics. Â Get general models retención-actividad provide useful qualitative information on issues relating to the toxicity, efficacy in blocking the reuptake of biogenic amines or affinity for the various recipients of these compounds for various therapeutic groups (anxiolytic and antipsychotics, in addition to the above). Â set the limits of applicability of the models and statistically validated. From the results the following conclusions are drawn:. The CMB system allows strict control of the experimental conditions which provides data retention reproducible. The use of a single descriptor in the development of the models have advantages from the point of view, especially with small series of data. The successful implementation of the proposed regression models is limited by the lack of parameter values bibliographic descriptor associated with the activity. Â The retention of the compounds measured in a system chromatography micelar of bio-reparto is a parameter that adequately describes the pharmacokinetic and pharmacodynamic behavior of different groups of drugs with action at CNS. Whereas retention measure using a mobile phase of Brij35 0.04M, in general, the models obtained, 8 itself as d46 ratios are the same, are significant with a confidence level of more than 95% and explain between 67 and 97 % of the variance in the data of the activity in question. Similar patterns were obtained from a statistical point of view the various phases mobile Brij35 tested. Â models QRAR developed showed good predictive capability for both extrapolation by interpolation, with the exception of models developed for some of the pharmacodynamic parameters in the data predicted by extrapolation should be considered with caution. The models are valid for predicting the activity of compounds having the same molecular features and estereoquímicas as those used in developing the model and the farmacóforo corresponding to the biological tissues in question. Â Among the different types of antidepressants considered in this argument, most compounds withheld CMB (k> 75 for a mobile phase of Brij35 0.04M) are the most potent inhibitor of the reuptake of serotonin, on the contrary compounds less held in CMB (k <50) are the most potent inhibitor of the reuptake of norepinephrine. Therefore, the CMB will be able to provide information on the selectivity of inhibiting the reuptake of NA/5-HT of a compound with proven therapeutic action but whose data relating to the activity are not known. Â The general models obtained with compounds belonging to different therapeutic groups (antidepressants, antihistamines, and anxiolytics neuroleptics), indicate that there is a range of retention (50 <k <150 for a mobile phase of Brij35 0.04M) in the drugs which have a higher affinity for the receptors of monoaminas considered; these compounds also found to be the most toxic. Â models QRAR developed that are better suited QSAR models using logPapp as independent variable to describe the pharmacokinetic and pharmacodynamic behavior of CNS drugs. This is due to the retention CMB not only depends on the characteristics of hydrophobic compounds but also of their electronic properties and estéricas, which determine the strength of the link between the drug and its corresponding biological tissues. . QSAR models based on the model codes / Neuronal Network are valid for predicting the long half-life of antihistamines and to determine their therapeutic group (antagonists H1 or H2). These models demonstrate the effectiveness of the program structures CODES encoder for generating molecular descriptors that can be used in QSAR studies.

Author: ARTMANN MARISA.
Year: 2005.
University: SANTIAGO DE COMPOSTELA [www.usc.es].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: , UNIVERSIDAD SANTIAGO (ESPAÑA)..

Summary: The long and persistent record of the conduct of the investigation shows the interest that centralizo towards the study of the chemical composition of the sap of copaifera, from its use of different técnicasa of extraction and separacción per column, it succeeded in isolating a compound Crystal extract a Copaífera langsdorfil. Finally our assumptions structural acid 19-kaurenoico was confirmed for the first time through studies of X-ray diffraction Comparing compounds oil of copaífera isolated by other researchers with acid 19-kaurenico, it is concluded that there is a structural similarity of the same.

Author: RODRIGUEZ ROBLEDO VIRGINIA.
Year: 2005.
University: CASTILLA-LA MANCHA [www.uclm.es].
Place of defense: INSTITUTO DE INVESTIGACIÓN EN RECURSOS CINEGETICOS.
Place of preparation: FACULTAD DE CIENCIAS QUIMICAS.

Summary: The aim of the thesis is to establish and validate analytical methods using new techniques electroforéricas and chromatographic separation and allowing the determination of antidepressants most important and some of its metabolites in pharmaceutical formulations and biological fluids. The proposed methods are intended to enable determinations quick, simple, sensitive, robust and allow the use of them both in controlling hot formulations as in the forensic or clinical study of biological samples.

Author: RODRIGUEZ CUESTA MARIA JOSÉ.
Year: 2005.
University: ROVIRA I VIRGILI [www.urv.cat].
Place of defense: FACULTAT DE QUIMICA.
Place of preparation: UNIVERSITAT ROVIRA I VIRGILI.

Author: EZQUERRO ROYO ÓSCAR.
Year: 2005.
University: LA RIOJA [www.unirioja.es].
Place of defense: UNIVERSIDAD DE LA RIOJA.
Place of preparation: UNIVERSIDAD DE LA RIOJA.

Summary: The aim of the thesis was the development of different methods based on the microextracción in solid phase in space head coupled to gas chromatography (HS-SPME-GC) for the determination of volatile organic compounds (VOCs) in various solid samples (materials flexible packaging, contaminated soils and cork stoppers). The importance of these methods is its applicability in the industrial sector of the flexible packaging, in cellars or companies corcheras and environment. The extraction technique employed has been the microextracción in solid phase (SPME), which allows direct analysis of volatile organic compounds by avoiding the use of organic solvents, it is easily automatable and can be combined in line with the gas chromatography. Furthermore, it has been developed for the first time the theory of microextracción in solid phase in the space of multiple head (MHS-SPME). This technique allows direct quantification in solid samples by removing the effect matrix, and is repeatedly drawn the same sample using HS-SPME.

Author: Pacheco Martínez M. Cristina.
Year: 2005.
University: ALICANTE [www.ua.es].
Place of defense: Facultad de Ciencias.
Place of preparation: Universidad de Alicante.

Summary: The present research work addresses the problem of N-nitrosamines in natural rubber. These are a family of carcinogenic substances that are formed during the curing of the material, by the decomposition of additives to high temperatures process. Among all the articles manufactured from natural rubber, rubber teats for infant use are those that have aroused greater interest in the type of consumer target. These are items directly to the baby's mouth and his sensitivity to carcinogenic substances is much greater than that of an adult. This has led to the creation of the European Directive 93/11/EEC, which regulates through standard EN 12868, the level of N-nitrosamines released by the teats of caucho.En this research work has been studied issues N-nitrosamines in the teats, from three points of view. First, it has studied the method for determination of N-nitrosamines, detectors and proposing alternative extraction methods to improve the measurement and recovery of the analytes. On the other hand, it is necessary to assess the risk exposure of the baby in terms of the migration levels of N-nitrosamines in saliva, in different conditions of use of a teat. It has been observed that the material washed prior to the use of the teat, reduce migration levels, and therefore the risk of exposure of the baby. Finally, it has addressed the manufacturing process of teats to study the problem from the standpoint of the formation of N-nitrosamines in the rubber. The formation of N-nitrosamines given by the presence of secondary amines (decomposition of the remains of vulcanization accelerators) nitrosating and in the atmosphere of vulcanization and in the midst of látex.Este work has resulted in a comprehensive study of the problem of N-nitrosamines in natural rubber teats, bringing conclusions as to the identification, migration and the formation of these substances.

Author: HLABANGANA LEAH.
Year: 2005.
University: BARCELONA [www.ub.es].
Place of defense: FACULTAD DE BARCELONA.
Place of preparation: UNIVERSITAT DE BARCELONA.

Summary: The amines are the natural constituents of many foodstuffs and their presence may be related to the degree of fermentation or putrefaction of the same. Also, some amines are impurities from outside activities or antropogénics such as packaging, product development and so on. Therefore, to establish effective methods for the determination of these substances is a priority in the fields biochemical, clinical and food products. In this thesis, have been studied two different groups of amino compounds. On the one hand, certain contaminants amines and / or impurities in sweeteners and, secondly, the amines biógenas that are generated from the amino acid protein. The analytical methodologies employed have been in flow injection analysis (FIA) and liquid chromatography (HPLC) high resolution in both cases detection has been based on the absorption molecular UV-visible of analytes. Methods (FIA) can be an alternative to the chromatographic methods and electroferéticos for determining multi certain analytes. In this thesis were established FIA different methods for the simultaneous determination of aniline and cyclohexylamine in commercial sweeteners containing cyclamate using 1,2-naftoquinona-4-sulfonato sodium (NQS) as reagent derivatizante. It has also established a method for determining rapid FIA histamine in wines. For optimzación of experimental conditions have been used techniques quimiométricas such as factorial design and optimization multi. On the other hand, when it has not been possible to reach a total selectivity, methods have been used quimiométricos for data analysis. Finally, we propose an HPLC method with derivatization post-columna with the reagent NQS for determining amines biógenas wine. This method is based on the separation of amines using ion chromatography pairs using a gradient elution of acetonitrile mobile phase and an aqueous phosphate buffer (pH = 2.5) containing surfactant heptanosulfanato sodium. This chromatographic method has been applied to the analysis of red wines from different regions of Spain.

Author: ROSELL LINARES MÓNICA.
Year: 2005.
University: BARCELONA [www.ub.es].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: DEPARTAMENTO DE QUÍMICA AMIENTAL, INSTITUTO DE INVESTIGACIONES QUÍMICAS Y AMBIENTALES DE BARCELONA (IIQAB-CSIC).