CROMATOGRAFIC ANALYSIS

Author: RIVERO MARABE JOSÉ JUAN.
Year: 2001.
University: EXTREMADURA [www.unex.es].
Place of defense: FACULTAD CIENCIAS.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: The power ioentificar inequivolamente the largest number of metabolites of each corticosteruides or esteruide anabolic, from which can be demonstrated using genetic themselves, both with the need for this identification through faster and more accurate methodology is a continuous goal analitico of doping control, becoming this objective in priority in regard to conduct research that will enable us to improve and perfeccipnear technically the methodology applied in the aforementioned control. Three main objectives. - Tuning methods analytical cromatugráficos for deteminación cuanti and cuali of anabolic steroids and corticosteroids. - Assessed on real samples empowerment analitaca of methodology used. - Evaluation and determination of the presence of anabolic steroids and cortcosteroides endeprotistas and sedentary people.

Author: ALEXANDRE FRANCO MARÍA.
Year: 2002.
University: EXTREMADURA [www.unex.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: This thesis has been carried out studies moving to the development of test procedures for tracking different compounds whose determination in fatty foods resulting from interes.Así, enracinamiento a genetic problems of these foods and cause deterioration of the same is averted by prosencia of antioxídantes either natural or sinteticos.en specific focoferoles and pupigralado, antiocianisol, pulibhoxitolmenco respectivamente.Se have developed a method for analyzing these compounds, beseros in the same character reducer, and tnato in the signals are obtained in its electrochemical oxidation in electodos coal vinified by a further analysis of multivariate techniques for the determination of mixtures of such compounds, otrolecto one of the fatty food whose pubdución be of greater interest in our region and with greater benefit is the healthy oil production of oliva.Su rebre increasing use of products fitosemiterios to optimize growing aceite.Entre these, the new groves are irrigated is very necessary utiliazación -- whose waste and weigh wing food chain, especially through the irrigation water. Therefore analytical methods have been proposed for cocitrol of such waste, in particular diquat and gletoseto.Y by recent examines the use is common in acetites, as acetites from our olive mazanilla, cacerenia for fipificación the provenance of these.

Author: GIMENO FERRERES ROSA ANA.
Year: 2003.
University: ROVIRA I VIRGILI [www.urv.cat].
Place of defense: QUÍMICA.
Place of preparation: FACULTAD DE QUÍMICA.

Summary: The aim of this thesis has been the development of analytical methods based on acomplamiento of high performance liquid chromatography at various extraction techniques for the detection and identification of various families of organic pollutants in water and sediment samples port. The pollutants studied were bencenosulfonatos and nafatalenosulfonatos, polycyclic aromatic compounds, phthalates and adipates and pesticides antialgas. As detectors, methods have been developed using the detector UV-visible and aque this detector is used on a regular basis. However, due to the low concentration levels to be determined in the analysis of environmental samples, it is preferable to the use of more sensitive detectors, such as fluorescence detector or mass spectrometry. That is why these detectors have also been selected for determining alglunos of the compounds studied. In the case of mass spectrometry, the interface has been used for the coupling liquid chromatography has been the interface at atmospheric pressure chemical ionization, which has been selected taking into account the characteristics of the compounds studied. In terms of extraction techniques for aqueous samples has been used in solid phase extraction coupled in some cases on-line liquid chromatography, assessing both the use of sorbents polymeric conveniconales, as PLRP-s, as the sorbents polymeric highly entrecruzados, as LioChrolut IN and Isolute ENV +. For samples sedimientos, the technique has uitilizado is in contact with the sample an organic solvent, in some cases favoring the extraction process using ultrasound. In some of the studies also include the use of two methods of calibration of the second order as mathematical tool apra resolving some of the problems encountered in the determination of the compounds studied, the less time analysis by quantifying the analytes from peaks cromatográicos partially resolved or the rapid quantification in complex samples presenting matrix effect. All methods developed have been used to assess the presence of the compounds studied in real samples taken at the expense of Tarragona (Spain), including monitorizaicón over a period of five months of the presence of pesticides antialgas.

Author: MATEU SÁNCHEZ MANUEL.
Year: 2003.
University: ALMERÍA [www.ual.es].
Place of defense: CIENCIAS EXPERIMENTALES.
Place of preparation: UNIVERSIDAD DE ALMERÍA.

Summary: The work contributes to several rigorous and reliable analytical methods to control the presence of pesticide residues in several cultivos.Los methods presented are based on the application of the technique chromatography gases-espectrometria mass to anilisis a high number of these compounds methods are framed in a context of quality assurance, traceability and control Statistical. Additionally were carried out studies calbración in different matrices and solvent in which test the ability of the methods desarrollandos to be applied to ls determination of the compounds studied in different cultures. Finally, multivariate calibration was applied successfully to resolve señáles overlapping obtained.

Author: PLAZA MEDINA MARÍA.
Year: 2003.
University: LA RIOJA [www.unirioja.es].
Place of defense: ENSEÑANZAS CIENTIFICAS Y TECNICAS.
Place of preparation: CIENTÍFICO Y TECNOLÓGICO DE LA UNIVERSIDAD DE LA RIOJA.

Summary: The project comprises three sections work done. I.-se studying the degradation of pesticides etiofencarb and ecefato in controlled laboratory conditions: hydrolytic degradation in the acidic, neutral and alkaline, at different pH; thermal degradation at temperatures of 4Â fourth (low), 20Â º (environment) and 50Â º ( elevated); photochemical degradation by radiation with solar simulator in different ways, aqueous methanol and hexane and xon oxidative degradation of hydrogen peroxide solutions at different concentrations in aqueous and non-aqueous media. In these studies have been obtained kinetics of degradation for each and every type of pesticide degradation. II .- A second paragraph has been desrrollado to identify the degradation products obtained allowing propose mechanisms degradativos for diferntes reactions. III. - Finally, a study has been made of pesticides applied field with the doses recommended by the manufacturers and the crop being selected manzano.Se tracks the evolution of etiofencarb and acephate, with the previously identified metabolites in diferntes fractions apple: fraction surface fración peeling internal. There are equilibriosde penetration to the interior of the fruit and effects degradativos, both external and internal.

Author: LORENZO GARCIA FERNANDO.
Year: 2003.
University: HUELVA [www.uhu.es].
Place of defense: FACULTAD CIENCIAS EXPERIMENTALES.
Place of preparation: FACULTAD CIENCIAS EXPERIMENTALES.

Summary: BE DEVELOPED AND OPTIMIZADO MISCELLANEOUS LINKS FOR THE DETERMINATION AND ESPECIACION OF MERCURY IN FISH AND SAMPLE BIVALVE. BE USED FOR THAT ONE SENSOR FLUORESCENCIA ATOMIC. FOR THE DETERMINATION OF TOTAL MERCURY HAS BEEN USED AN INJECTION OF DEVICE IN FLUJO-VAPOR FRIO-FLUORESCENCIA ATOMIC. FOR ESPECIACION MERCURY HAS BEEN USED THE ACOPLAMENTO CROMATOGRAFO OF GASES-PIROLISIS-FLUORESCENCIA ATOMIC. BE DESIGNED ANALYTICAL A STRATEGY FOR MAKING THE DETERMINATION OF METILMERCURIO IN THIS KIND OF SAMPLES, BASED ON AN DETMINACION STARTING FROM THE CONCENTRATION OF MERCURY TOTAL CHOICE FOR LATER THE METHODOLOGY FOR APPROPRIATE TREATMENT FOR EVERY KIND OF SHOW, PROCURANDO MAXIMIZE PRODUCTIVITY HEAD TO BE USED IN LABORATORIES OF ROUTINE. THE DETECTOR IS MODIFIED FOR ATOMIC FLUORESCENCIA COMMERCIAL, INCORPORÁNDOLE A CELL FOR QUARTZ WHAT PERMITIO INCREASE ABOUT HIS SENSITIVITY IN DOUBLE. AMENDMENT OF CELL FOR QUARTZ PERMITIO DEVELOPMENT OF LINKAGE FLUORESCENCIA-FLUORESCENCIA FOR THE DETERMINATION OF MERCURY AND A SECOND ELEMENT SUSCEPTIBLE OF GENERATING HIDRUROS IN THIS CASE, THE ARSENIC. LINKAGE FLUORESCENCIA-FLUORESCENCIA HE HAVE JOINTLY WITH LIQUID CHROMATOGRAPHIC FOR THE ESPECIACION MERCURY AND ARSENIC IN WATER SAMPLES OF NATURAL. FINALLY, HE DESARROLLARON LINKS BETWEEN CROMATOGRAFOS GAS AND LIQUID WITH DETERCCION BY ICP-MS, TO UNDERTAKE COMPARATIVE STUDY. THE DETECTOR FOR ATOMIC FLUORESCENCIA IS A GOOD ALTERNATIVE FOR THE DETERMINATION AND ESPECIACION MERCURY AND OTHER ELEMENTS OF ROUTINE IN LABORATORIES, DUE TO THE HIGH SENSITIVITY REACHED WITH THIS, AS WELL AS THE ROBUSTEZ OF EQUIIPO AND LOW COST OF ACQUISITION AND MAINTENANCE.

Author: QUINTANILLA LOPEZ JESUS EDUARDO.
Year: 2003.
University: COMPLUTENSE DE MADRID [www.ucm.es].
Place of defense: FACULTAD DE CIENCIAS QUMICAS.
Place of preparation: FACULTAD DE CIENCIAS QUIMICAS.

Summary: The anÃÂ ¡lisis multicomponent mixtures is happening at dÃÂa, one of the areas that enjoy greater growth within the QuÃÂmica AnalÃÂtica.En this field, CromatografÃÂa coupled to the EspectrometrÃÂa Mass is one of the tÃÂ © cnicas mÃÂ ¡s used at present, despite the relative slowness of the process cromatogrÃÂ traffic. The road mÃÂ ¡s obvious to solve the aforementioned slow serÃÂa dispense with separaciÃÂ ³ n cromatogrÃÂ ¡fica and perform anÃÂ ¡lisis ÃÂ eighth Only with the espectrÃÂ ³ meter masas.Para this serÃÂa needed mÃÂ © all regresiÃÂ ³ n multivariate the mass spectra of mixtures, but until now little has been achieved in this regard. Therefore, estableciÃÂ ³ as a key objective of this Doctoral Thesis developing a metodologÃÂa of anÃÂ ¡lisis rÃÂ We ask that allows cheaper and quantify the components of mixtures, using tÃÂ © cnicas of calibraciÃÂ ³ n multivariate the mass spectra obtained by introduciÃÂ charges directly in the sample. The work has focused primarily on evaluating the performance of different mÃÂ © all regresiÃÂ ³ n multivariate aplicaados to cuantificaiÃÂ ³ n mixtures by EspectrometrÃÂa of Masas.Para It has done a comprehensive job simulaciÃÂ ³ n, going after diseÃÂ ± ar y optimizing a system of allowing teams to adapt a conventional CromatografÃÂa of Gases-EspectrometrÃÂa Mass for introducciÃÂ ³ n direct mezclas.Por ÃÂ fourth last, was realizÃÂ ³ the anÃÂ ¡lysis samples of special interÃÂ © s, as drugs and aromas of plants, applying the system introducciÃÂ charges directly deseÃÂ ± ado and procedures regresiÃÂ ³ n multivariate. Ultimately, it has developed a metodologÃÂa analÃÂtica for undertaking the cuantificaciÃÂ ³ n component complex samples directly by EspectrometrÃÂa Mass without a separaciÃÂ ³ n cromatogrÃÂ ¡fica previa.El process can be done on computers conventional CromatografÃÂa of Gases-EspectrometrÃÂa Mass thanks to the system of introducciÃÂ ³ n direct sample development.

Author: NOGUEIRAS CARNERO M. JOSÉ.
Year: 2003.
University: VIGO [www.uvigo.es].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: FACULTAD DE CIENCIAS - UNIVERSIDAD DE VIGO.

Author: SANCHES SILVA ANA TERESA.
Year: 2004.
University: SANTIAGO DE COMPOSTELA [www.usc.es].
Place of defense: FACULTAD DE FARMACIA.
Place of preparation: FACULTAD DE FARMACIA.

Summary: The food preservation is essential to avoid natural disturbances, proliferation and contamination by microorganisms. One of the most common causes of food spoilage during storage is lipid oxidation. In recent years this phenomenon has aroused great interest among researchers and the general public because of their potential influence on the aging process and in several diseases such as arteriosclerosís and cancer. This phenomenon leads to the alteration of the components of the food and creates the formation of unpleasant tastes and odors. In addition to changes in sensory quality, nutritional value, safety and acceptability also shrinking. This thesis devotes most of its chapters to the study of the influence of storage conditions of the product packaging (eg time, light, atmosphere, temperature) in nutritional components susceptible to oxidation lipid (fatty acids), as well as the study of aromatic profile obtained in different storage conditions and the pursuit of an analytical tool that allows early detection and assessment of the extent of lipid oxidation processes. The last chapter has been devoted to the study of the migration of substances of packing material made food. Over the past few decades the concern over issues such as food safety, nutrition, additives and labeling of the product has been an increasing demand by consumers. Within this context, the packaging of foods is a technique essential to preserve the quality of services, minimize its damage and limit the use of additives. The materials intended to come into contact with food, such as plastics, fulfilling various functions much-containing foods, protecting the physical and chemical deterioration, and provide a practical means to inform consumers about the products. Also, the packaging preserves the shape and texture of the food it contains, avoided losing flavor or aroma, prolonged storage time and regulates the content of water or moisture of the food. In some cases, the material selected may even improve the quality of producto.Sin embargo there is a very important feature, and should require that all packaging, and that there are no interactions with the contents of it. Therefore, an important aspect of public health concern to the EU is the consumer exposure to chemicals in the undesirable dieta.La little information on the behavior of many substances potentially migrants and the growing importance of food safety , have attracted the interest of the European Union in terms of plastic materials in contact with food. Among the projects that the European Union has funded under this item is the "Foodmigrosure", which is being developed in several European centers of research. Included in this project, which has funded scholarship to the realization on the part of this thesis has been developed a method analitico, which allows eval 8 uar the 3e1 levels of migration of triclosan, antimicrobial chosen by the project as a model substance test Transport / partíción. The dissertation presents has allowed the development of seven articles, currently published in reputable international journals.

Author: CARPINTEIRO BOTANA JOSEFINA.
Year: 2004.
University: SANTIAGO DE COMPOSTELA [www.usc.es].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: FACULTAD DE QUÍMICA.

Summary: This thesis describes the development and improvement of analytic methodology for the determination of priority pollutants and emerging nature of organic and organometálica (organotin, anti-inflammatory drugs and estrogen) in our environment (water and sedimientos) by gas chromatography coupled to atomic spectroscopy with helium plasma induced by microwave (MIP-AES) and mass spectrometry in tandem MS and simple MS-MS.La preparation of the samples has focused on the use of microextración in solid phase SPME as a method of concentration. The selection of the three groups of analytes believe in the memory has been done because of their environmental interest, based on parameters such as toxicity, distribution, law, persistence, and activity disruptora on the metabolism of living organisms. One of the basic objectives pursued in this memory has been the development and optimization methods derivatization to enable determination of polar analytes using gas chromatography and are compativles with the use of SPME as technical preparation muestra.Para It felt both derevatización delos within the same sample, prior to its merger, and subsequently its inclusion on the fiber microextración derivation amid dry. Specifically, the latter method has helped address the study by SPME and gas chromatography compounds nature acid and polar difilmente derivatizables in the sample itself, which, until this moment, had not been determined maner satisfactory mestras real using the tools previously descritas.Además also studied posibilada minimize the duration and cost of genetic procedures developed by reducing the length of some of these steps considradas in them, incremntando the number of species analyzed together, simplifying processes calibration and / or using tools quimiométricas such as the composition strategic muestras.Esta latest information allows semi-cuantitativa on the levels of analytes in samples problem, through the analysis of a small number of specimens compounds prepared automatically by mixture of the above. The possibilities and limitations of the methods developed are discussed critically and objectively, by comparing their physical and chemical properties with corespondientes others in the bibliografía.Otro key aspect of the work done has been systematic validation of the proposed methods by analyzing certified reference materials, participation in ejercicioes intercomparison yla systematic comparison with the results obtained using other methods of sample preparation more classic and normally more laborioasa, for the same analytical problems.

Author: UNCETA ZABALLA NORA.
Year: 2004.
University: PAÍS VASCO [www.ehu.es].
Place of defense: FACULTAD DE FARMACIA.
Place of preparation: FACULTAD DE FARMACIA.

Summary: Doctoral Thesis This reflects the analytical methodologies optimized in various research projects of a multidisciplinary nature made in the Departments of Analytical Chemistry and Pharmacology, College of Pharmacy, University of the Basque Country. On the one hand, in order to study the development of hypertension in patients with syndrome of Obstructive Sleep Apnea, have been optimized two methods for the determination of catecholamines and their metabolites as well as for the determination of mono and dimetilargininas in human plasma. On the other hand, and plows ratify the therapeutic benefit that features the use of a single enantiomer of the antidepressant fluoxetine (Prozac), has been optimized methods that permit the identification of fluoxetine and its metabolite norfluoxetina as well as their enantiomers RyS plasma and bark cerebral.

Author: Dopico García Ma. Sonia.
Year: 2004.
University: A CORUÑA [www.udc.es].
Place of defense: Vicerrectorado del Campus de Ferrol.
Place of preparation: Facultad de Ciencias.

Summary: This work focuses on the study of behavior evnases of polyolefins for food use in migration testing. The study focuses on the following points: - The proposed analytical method alternative to formal method for determining overall migration in olive oil which allows the quantification of oil absorbed by the plastic by extraction with ultrasonic energy and determination by chromatography fluid high efficiency (HPLC) with detector evaporativo light scattering (ELSD). - Is about to put two chromatographic methods that allow simultaneous separation and quantification of primary and secondary antioxidants in food simulants (aqueous and olive oil) by reverse phase HPLC and ultraviolet (UV) detection with network diodes for you get good quality parameters. - Develop methods of pretreatment of the sample to enhance the sensitivity of an `alisis specific migration of antioxidants in food simulants, using extraction techniques liquid liquid (LL) and solid phase extraction (SPE). - It puts out a extraction step energy mmicrondas of antioxidants from samples of polyolefins, prior to quantification by HPLC-UV, in order to determine the concentration levels of antioxidants present in the polyolefin. - We have studied the stability of anitioxidantes in food simulants in the conditions of migration testing. - Packs are studied commercial food use of polyolefins identifying antioxidant most often used, its concentration in the matrix and their levels of specific migration. - Is studying a material low density polyethylene (PEBD) extruded to characterize the potential relationship between migration levels and characteristics of the matrix.

Author: ESPEJO MAQUEDA JESÚS.
Year: 2004.
University: SEVILLA [www.us.es].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: FACULTAD DE QUÍMICA.

Author: LOSA RIERA RAQUEL.
Year: 2004.
University: OVIEDO [www.uniovi.es].
Place of defense: FACULTAD DE QUMICA.
Place of preparation: FACULTAD DE QUIMICA.

Author: GARCÍA LOMILLO INMACULADA.
Year: 2004.
University: BURGOS [www.ubu.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: The analytical procedure, operational sequence of actions described accurately, chemistry is especially dedicated to information on the composition of matter. Its result, the analytical result, is a key to ensuring the quality of our life even before birth. The analytical result is information about the presence of toxic substances and / or potentially hazardous to human health and is to be submitted in accordance with the legal regulations. In addition, analytical procedures must meet the requirements needed to ensure reliability in its results. The theory based on the order of the signal is particulamente important because it allows insesgadas analytical determinations in the presence of interfering. The optimum use of the information contained in data n-vías provided by the modern instrumentation along with a careful evaluation of the uncertainties have been the methodological approaches for which has discurrido research work described in this report. Directive 96/23/EC declared annulled by the directives that were established methods for the investigation of waste and heavy metals arsenic, for the detection of substances having a hormonal or thyrostatic action and for the detection of residues. This allows the use of multi-calibrated signals for analysis in laboratories official responsible for the health monitoring. The legal provision states that the analytical methods must be documented in the instructions for testing and have to meet certain performance criteria to be validated: specificity, accuracy, robustness, stability, recovery, repeatability, reproducibility intralaboratorio, reproducibility, curves calibrators, decision-making capacity and capability of detection. Both definitions as the way to get the parameters, the legal text falls systematically in the context of ISO. The generalization of the detection capability of calibrated data of any kind, particularly calibrated by PARAFAC with signs of order two, ensures that the decision can be applied to the data from instrumentation coupled, on the other hand, the decision itself calls in the identification process. This approach does not require the specific nature of the analytical signal as a prerequisite to the procedures and safeguards against potentially interfering completely unresolved in the chromatographic phase. In practice, this facilitates the analysis of samples remarkably complex. Accordingly, the thesis explores with various analytical techniques (fluorescence excitación-emisión, GC / MS and HPLC / SDA) implementation of the calibrated PARAFAC, PARAFAC2, PLS bilinear and trilinear PLS for various prohibited substances or ceiling allowed. Moreover, the need to manage complex biological samples need to optimize stages of pretreatment and extraction stages, in which it has been very efficient use of various types of designs of experiments. On the other hand, handling signals of a second order requires new approaches to the problems of standardization, correction of the baseline and displacement in the chromatographic phase treatment of analytical signal prior to the construction of mathematical models. In summary, the research work carried out in this thesis seeks to add academic knowledge in advanced chemical analysis to improve the quality of analytical determinations in complex samples without requiring specificity.

Author: RAMOS BORDAJANDI LUISA FERNANDA.
Year: 2004.
University: AUTÓNOMA DE MADRID [www.uam.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: IQOG, CSIC..

Summary: With the development of agriculture and industrial chemical sectors have aparecidó large number of new chemicals and in turn resulting in the synthesis products or burning them, just deposited in environmental compartments and that are extraneous to the membership. In this type of compounds are called environmental chemical pollutants. These include persistent organic pollutants, such as polychlorinated biphenyls (PCBs), Polychlorotrifluoroethylene dibenzo-para-dioxinas (PCODs), Polychlorotrifluoroethylene dibenzofurans (PCDFs), DDT, toxafenos and polycyclic aromatic hydrocarbons (PAHs). Because of its ubiquity, toxicity and persistence in the environment are on the list of substances subject to the Stockholm Convention, which recently have signed numerous countries and among them Spain, which sets out a series of measures to reduce ylo eliminate their production, use and marketing. Other pollutants are relevant heavy metals (lead, cadmium, copper and zinc) and arsenic. The primary route of entry for these contaminants in the human body is food consumption. Following episodes of contamination of food in recent years that have been implicated some of them, there is a growing concern among consumers about food safety. This has led to different institutions to take measures, which include the monitoring of levels in foods, to know the background levels, establish a legislation and ensure their compliance, and certifying the safety of its consumption . Also, efforts are focused on the development of methodologies fast, reliable, simple and low cost, to conduct these tests routinely, especially in the case of PCBs and PCDD / Fs to rapidly detect potential sources of pollution, thus avoiding the pollutants that enter the food chain. For these two basic objectives of this thesis were: 1. The evaluation and development of methods based on gas chromatography (GC) multidimensional as heart-cut MDGC and comprehensive two-dimensional GC (GC GC), for the determination of PCBs, PCOD / Fs and PCBs and toxafenos chiral in food, and 2. The determination of levels of contaminants in foods of particular interest as food purchased in Huelva, fish caught in the river Turia and milk, and chiral enrichment enantiomérico of PCBs in breast milk, milk and milk products from cows, goats and sheep and toxafenos chiral in fish oil. As most relevant conclusions should be noted that: - There have been optimized parameters and conditions of a chromatography system GC x GC-microECD for the determination of PCDD / Fs and PCBs. It has achieved the separation of toxic congeners with TEF with different combinations ZB-5 x HT-8 and HT-8 x BPX-50. Ambas You can obtain chromatograms structured, which facilitates the identification of the analytes. Combinations ZB-5 x Supelcowax-1 Oy DB-17 x Supelcowax-10 allowed the identification of 12 PCB coplanar with the advantage of being able to simultaneously determine the 7 PCB indicators except PCBs 28. - Has been optimized parameters and conditions befitting a chromatography system heart-cut MDGC and GC x GC-microECD for the determination of PCBs and toxafenos chiral in real samples, using 3 columns nantioselectivas settled a total of 15 PCB and the chiral 5 toxafenos under study. In the case of determining the PCB chiral through GO x GC-microECD, combinations that provide the best results are those that employ as 20 column Supelcowax-10. In the case of toxafenos, the best results are obtained with the combination BGB-172 x BPX-50. - The levels of contaminants in food consumed by people in Huelva and the fish found in the river Turia show generally concentrac 8 ions po 504 r below the maximum established by the legislation. The intake of pollutants by the population of Huelva is within the range recommended by the WHO. The levels of PCBs and PCDD / Fs in breast milk show a marked decline respect to those described in previous years in Spain and other countries. - The determination of the enrichment enantiomérico in milk and milk and milk products from cows, goats and sheep ha.demostrado the existence of transformations enantioselectivas, especially in the case of PCB 171 and 183. There have been differences between the enantiomeric composition of the milk cow, goat and sheep, as well as between the different dairy products. In the case of toxafenos in fish oil, there has been an enrichment enantiomérico the first enantiomer respect to the second to Parlar 40.

Author: RODIL RODRÍGUEZ MARÍA DEL ROSARIO.
Year: 2004.
University: SANTIAGO DE COMPOSTELA [www.usc.es].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: FACULTAD DE QUÍMICA.

Summary: The work carried out in this thesis focuses on the development of new strategies for sample preparation for the control of pollutants to trace levels in the aquatic environment. For this study were selected three main groups of environmental pollutants, mercury compounds and derivatives, halogenated compounds as organochlorine pesticides (OCP), polychlorinated biphenyls (PCBs), bigenilos polybrominated (PBB) and polybrominated defined ethers (PBDE) and organophosphorus compounds, as tri alqui-/aril phosphates and bisfosfatos. For the development of new strategies for sample preparation of various methodologies have been used for the extraction of compounds arrays of arrays both aqueous and solid, trying to minimize the time of analysis time analysis, the amount of sample and organic solvent. Among the methodologies used are the supercritical fluid extraction (SFE), microwave assisted extraction (MAE) and dispersion of the matrix in solid phase (MSPD) in solid samples (PES) and microextracción solid phase (SPME) samples liquid. The final determination of the compounds was carried out by chromatography techniques coupled with different detection systems. The development of these analytical methodologies to determine levels of the compounds studied in the environment, mainly in the aquatic environment. Thus, it is intended that can be expanded knowledge of the behavior of these compounds in the aquatic environment.

Author: VELEDO MARIA TERESA.
Year: 2004.
University: AUTÓNOMA DE MADRID [www.uam.es].
Place of defense: FACULTAD DE CIENCIAS.
Place of preparation: FACULTAD DE CIENCIAS.

Summary: This thesis describes the work done to develop a system of capillary electrophoresis (CE) detection en-columna by laser induced fluorescence (LlF), which enables the detection of analytes in samples of small volume and / or they are in very low concentrations (10-6 M). The analytes, amino acids and proteins, are derivatizaron covalentemente en-columna with reactívo 3-(2-furoil) quinolin-2-carbaldehído (CF) to generate products with a fluorescent excitable argon laser ionized (exc = 488 nm). The system CE-LlF and developed methods were applied to the analysis of amino acids in drugs and human plasma samples, and three types of studies related to the analysis of proteins, specifically, the identification of allergen beta-Iactoglobulina bovine baby foods, study of the effect of covalent derivatization on the separation of glicoformas of ribonuclease BJRib B) And the characterization of microorganisms using protein profiles. In the last chapter of the thesis, have been collected the results of the study at the level of cells indíviduales two proteins involved in cell cycle of the yeast Saccharomyces cerevisiae, Gal1 and Gal4.

Author: BROSSA PIÑERO LÍDIA.
Year: 2004.
University: ROVIRA I VIRGILI [www.urv.cat].
Place of defense: FACULTAD DE QUÍMICA.
Place of preparation: FACULTAD DE QUÍMICA.

Summary: The aim of the thesis was the development of analytical methods bread! The determinaCión and control of a group of EDs in environmental samples. The methods developed are based on the one hand in the use of gas chromatography with spectrometry mases (GC-MS) with different techniques of extraction, solid phase extraction (SPE) and a technique appeared recently, the extraction bars magnetic shaker (SBSE). These methods use injection techniques of large volumes (LVI) recently developed to introduce the extract in the chromatographic system. The PES has been coupled on-line to the GC using the interface on-column and vaporizer temperature programmed, getting methods with a high degree of automation and better sensitivity. The SBSE has been used with liquid desorption rather than thermal desorption widely used in combination with GC, to study the applicability of techniques LVI in the absence of a desorbedor heat. On the other hand, with the aim of expanding the number of compounds studied, methods have been developed based on liquid chromatography (HPLC) high resolution and using the SPE as preconcentration technique. We have used the detector UV-Visible, getting a quick and easy implementation in the laboratory as a control method for the group of compounds studied in aqueous environmental samples, and mass spectrometry using the interface electroespray. With some of the methods developed have been carried out monitoring studies of different groups of environmental endocrine disrupters in water from the river and sea waters and entry and exit stations plants. These samples have been collected in the area of Tarragona, where so far there were no studies to control these pollutants.

Author: PUNÍN CRESPO MARÍA OLIVA.
Year: 2004.
University: SANTIAGO DE COMPOSTELA [www.usc.es].
Place of defense: FACULTAD DE FARMACIA.
Place of preparation: FACULTAD DE FARMACIA.