TRANSFER OF ANALYTICAL METHODS FOR THE CHARACTERISATION OF NATURAL PRODUCTS TO R&D PROCESSES OF IDOKI

IDOKI SCF Technologies S.L. is a technology-based company, set up on September 2006 in Derio (Biscay) with the main scope of developing extraction and purification processes based on the use of supercritical fluid extraction technology (SFE) in food processing, extraction of natural products and the production of personal care products. IDOKI¿s researchers have been working on many different R&D projects so far, most of them using this technology. However, the optimization of a SFE method for the different matrices cannot be performed unless we have an analytical method for the characterisation of the extracts obtained in each experiment. The analytical methods are also essential for the quality control of the raw materials that are going to be used and also for the final product. This PhD thesis was born to tackle this problem and therefore, it is based on the development of different analytical methods for the characterisation of the extracts and products. The projects that we could include in this thesis were the following: the extraction propolis, the recovery of agroindustrial residues (soy and wine) and the dealcoholisation of wine.On the one hand, for the extraction of propolis, several UV-Vis spectroscopic methods were used in order to measure the antioxidant capacity and the total polyphenol and flavonoid content of the extracts. A SFC method was also developed in order to measure more specific phenolic compounds. On the other hand, for the recovery of agroindustrial residues UV-Vis spectroscopy was used to determine the total polyphenol content and two SFC methods were developed to analyse different phenolic compounds. Extraction methods such as MAE, FUSE and rotary agitation were also evaluated for the characterisation of the raw materials.Finally, for the dealcoholisation of wine, the development of a SBSE-TD-GC-MS and DHS-TD-GC-MS methods for the analysis of aromas and a NIR spectroscopic method for the determination of ethanol content with the help of chemometrics was necessary. Most of these methods are typically used in IDOKI¿s lab as routine analyses apart from others not included in this PhD thesis.

LC-MS based methods for phytosterols determination in oenological matrices. Targeted metabolomic study of Rioja grape varieties

221 p.+ anexos

Determination of drugs used in combined cardiovascular therapy

Cardiovascular diseases are nowadays the first cause of mortality worldwide, causing around the 30% of global deaths each year. The risk of suffering from cardiovascular illnesses is strongly related to some factors such as hypertension, high cholesterol levels, diabetes, obesity The combination of these different risk factors is known as metabolic syndrome and it is considered a pandemic due to the high prevalence worldwide. The pathology of the disorders implies a combined cardiovascular therapy with drugs which have different targets and mechanisms of action, to regulate each factor separately. The simultaneous analysis of these drugs turns interesting but it is a complex task since the determination of multiple substances with different physicochemical properties and physiological behavior is always a challenge for the analytical chemist. The complexity of the biological matrices and the difference in the expected concentrations of some analytes require the development of extremely sensitive and selective determination methods. The aim of this work is to fill the gap existing in this field of the drug analysis, developing analytical methods capable of quantifying the different drugs prescribed in combined cardiovascular therapy simultaneously. Liquid chromatography andem mass spectrometry (LCMS/MS) has been the technique of choice throughout the main part of this work, due to the high sensitivity and selectivity requirements.

Metalak eta metaloideak itsasadarretan: kutsadura jarraitzeko erreminta analitikoen

265 p.

El soleamiento en las fachadas, técnicas para su reducción y pre dimensionamiento.

[EU]Lan honen helburu nagusia eraikuntzan gehituko diren argi-babeski sistema mota desberdinak aurkeztea da, bertan ematen den energia kontsumoa murrizteko asmoz. Izan ere, argi naturalaren erabilpen egoki batek eraikinaren efizientzia hobetzera eramango gaitu. Horretarako, ezinbestekoa izango da baliabide hau behar bezala ezagutzea, argitasuna eta beharrezko babesa eskaintzeko, eta ondorioz, energia aurreztea lortzeko. Babes sistema egokiena aukeratu baino lehen, aldez aurretik sortu izan diren argi-babeski mota desberdinak aztertu izan dira. Horrez gain, eguzki erradiazioa neurtzeko metodo grafiko eta analitikoak ere aztertu dira. Ondoren, Ecotect programak eskaintzen dituen simulazioei esker, eguzki erradiazioaren datu zehatzagoak lortzeko asmoz, ikasketa horretan erabiliko den eraikinaren kokapena, orientazioa eta ezaugarriak erabaki dira. Behin prototipoa definituta, programa bidez lau babes sistema mota desberdinak aztertu dira, horrela babesik gabeko eraikinean lortutako datuak alderatzeko. Azterketa Bilbo eta Sevillan egitea erabaki izan da. Izan ere, bi hiriburu hauek klimatologian duten desberdintasuna argi-babeskien aukeraketan duen eragina aztertzeko aukeratu dira, gainera, orientazioak eta argi babeskien dimentsioek ere izan dute zer esana aukeraketa garaian. Horrez gain, argi-babeskiek sortutako itzala ere aztertu izan da. Horrela, sistema hauen jarrera orokorra ikusi daiteke, eta beraz, uda garaian babesteko eta negu garaian eguzki izpiak sartzen uzteko duten ahalmena ikusi da. Bukatzeko, aurretik lortutako datu guztiei esker, eta bai kokapena zein orientazioa kontutan hartuz, babes sistema egokiena aukeratu da, jakinik ezinbestekoa dela argitasuna, babesa eta aurrezte energetikoaren arteko oreka egoki bat lortzea.