[en] The residues of pharmaceuticals, drugs of abuse and personal care products are detected in the environment due to the high consumption, uncontrolled discharges and lack of techniques for the total removal of these substances. These compounds are part of a group of pollutants named emerging pollutants, since they are not normally monitored or their presence in the environment is not regulated and could be a cause for any ecological damage or even for the human health. During the last years, the number of studies to develop analytical, reliable and sensitive methods has increased, as well as those to monitor these kind of compounds in the aquatic ecosystems. The existing analytical methods have been developed for a reduced number of compounds mainly in water, being other environmental matrices, like soils and biota, more difficult to analyse. This thesis is focused on the development of a method to analyse pharmaceuticals, drugs of abuse, personal care product and other kind of emerging contaminants from different nature, in surface, waste and drinking water, soils, sediments and fish, which can be used in different chromatographic method. This method is applied to study the ecosystem of the Turia River, a Mediterranean river of reference, heavily affected by the climate change, in order to establish the presence, transport and degradation of these compounds, and shed light on their dynamics in fragile ecosystems. Therefore, it was developed an analytical method for the determination and identification, selective, sensible and reliable for pharmaceuticals, drugs of abuse, personal care products and other emerging pollutants based in high-resolution liquid chromatography in tandem with mass spectrometer. Furthermore, it was developed an extraction method for solid matrices that is fast, efficient which improves the pharmaceuticals, drugs of abuse and other compounds recoveries comparing with the traditional methods and will be not required an expensive and sophisticated equipment. The analytical method developed was applied to study the presence and concentration of pharmaceuticals, drugs of abuse and other emerging pollutants, in water, soils, sediments and biota samples of the Turia River and, especially, to L'Albufera Natural Park as an example of Mediterranean River strongly affected by human activity and climate change. The developed analytical method was also used to obtain a better knowledge of the water cycle that affects this vulnerable area, including the study of wastewater and drinking water, and the level that is affected for these compounds. As well as to know the efficiency of the studied treatment plants. As a result, among the different mobile phase additives tested to improve the signal of the compounds in the mass spectrometer in negative ionization mode, ammonium fluoride (and adding acid to the positive ionization mode) proved reliable, sensitive and effective, increasing the signal of the compounds between 2 and 15 times in comparison to the traditional. The developed method to extract the compounds in solid matrices, showed that provides better recoveries and is more sensitive and accurate than the traditional method to extract the same compounds. With this method were analysed up to 47 emerging pollutants with the Liquid Chromatograph coupled to the triple quadrupole mass spectrometer and up to 319 were identified with the time of flight mass spectrometer.

[es] Los residuos de fármacos, drogas de abuso y productos cosméticos se detectan en la naturaleza debido a su elevado consumo, vertidos no controlados y falta de técnicas para la eliminación total de estas sustancias. Estos compuestos forman parte de un grupo de contaminantes llamados contaminantes emergentes, dado que no se monitorizan normalmente o su presencia en el medioambiente no está regulada y pueden llegar a causar un daño ecológico o incluso para la salud humana. Durante los pasados años, el número de estudios para tratar de desarrollar métodos analíticos robustos y sensibles, así como tratar de monitorizar estos compuestos en los ecosistemas acuáticos, ha ido en aumento. Los métodos analíticos existentes se han desarrollado para un número reducido de compuestos principalmente en aguas, siendo otros compartimientos medioambientales como suelos y biota más difíciles de analizar. La presente Tesis Doctoral se focaliza en el desarrollo de métodos de análisis que abarque fármacos, drogas de abuso, productos cosméticos y otros contaminantes emergentes de diferente naturaleza, en aguas superficiales, residuales y de consumo, suelos, sedimentos y peces que pueda ser usado con diferentes métodos cromatográficos. Estos métodos se aplican al estudio del ecosistema del rio Turia, fuertemente afectado por el cambio global que se está produciendo, con objeto de establecer la presencia, transporte y degradación de estos compuestos, y arrojar luz sobre su dinámica en los ecosistemas frágiles. Es por ello que se puso a punto un método de identificación y determinación, selectivo, sensible y robusto para fármacos, drogas de abuso, productos cosméticos y otros contaminantes emergentes basado en la cromatografía líquida de alta resolución acoplada a espectrometría de masas, además se desarrolló un método de extracción para matrices sólidas rápido, eficiente y que mejora las recuperaciones de los métodos tradicionales y no requiere la utilización de equipamiento costosos y sofisticados. Estos métodos se aplicaron a muestras de agua, suelo y sedimentos y biota del río Turia y especialmente, del área del Parque Natural de L'Albufera como ejemplo de río Mediterráneo severamente afectado por las actividades desarrolladas por el ser humano y el cambio climático. El método desarrollado se utilizó para obtener un mejor conocimiento del ciclo del agua que afecta a esta zona vulnerable, incluyendo el estudio de aguas residuales y de consumo humano, y el grado en el que se encuentran afectadas por estos compuestos, así como conocer la eficiencia de las depuradoras estudiadas.