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HUMAN EXPOSURE PATHWAYS to FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014

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HUMAN EXPOSURE PATHWAYS to FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 ADVERTIMENT. L'accés als continguts d'aquesta tesi doctoral i la seva utilització ha de respectar els drets de la persona autora. Pot ser utilitzada per a consulta o estudi personal, així com en activitats o materials d'investigació i docència en els termes establerts a l'art. 32 del Text Refós de la Llei de Propietat Intel·lectual (RDL 1/1996). Per altres utilitzacions es requereix l'autorització prèvia i expressa de la persona autora. En qualsevol cas, en la utilització dels seus continguts caldrà indicar de forma clara el nom i cognoms de la persona autora i el títol de la tesi doctoral. No s'autoritza la seva reproducció o altres formes d'explotació efectuades amb finalitats de lucre ni la seva comunicació pública des d'un lloc aliè al servei TDX. Tampoc s'autoritza la presentació del seu contingut en una finestra o marc aliè a TDX (framing). Aquesta reserva de drets afecta tant als continguts de la tesi com als seus resums i índexs. ADVERTENCIA. El acceso a los contenidos de esta tesis doctoral y su utilización debe respetar los derechos de la persona autora. Puede ser utilizada para consulta o estudio personal, así como en actividades o materiales de investigación y docencia en los términos establecidos en el art. 32 del Texto Refundido de la Ley de Propiedad Intelectual (RDL 1/1996). Para otros usos se requiere la autorización previa y expresa de la persona autora. En cualquier caso, en la utilización de sus contenidos se deberá indicar de forma clara el nombre y apellidos de la persona autora y el título de la tesis doctoral. No se autoriza su reproducción u otras formas de explotación efectuadas con fines lucrativos ni su comunicación pública desde un sitio ajeno al servicio TDR. Tampoco se autoriza la presentación de su contenido en una ventana o marco ajeno a TDR (framing). Esta reserva de derechos afecta tanto al contenido de la tesis como a sus resúmenes e índices. WARNING. Access to the contents of this doctoral thesis and its use must respect the rights of the author. It can be used for reference or private study, as well as research and learning activities or materials in the terms established by the 32nd article of the Spanish Consolidated Copyright Act (RDL 1/1996). Express and previous authorization of the author is required for any other uses. In any case, when using its content, full name of the author and title of the thesis must be clearly indicated. Reproduction or other forms of for profit use or public communication from outside TDX service is not allowed. Presentation of its content in a window or frame external to TDX (framing) is not authorized either. These rights affect both the content of the thesis and its abstracts and indexes. UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 IDENTIFYING HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Doctoral Thesis Supervised by Dr. Rosa Maria Marcé Department of Analytical Chemistry and Organic Chemistry and Dr. Georg Becher and Dr. Cathrine Thomsen Norwegian Institute of Public Health Tarragona 2014 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T U1518-2014NIVERSITAT ROVIRA I VIRGILI DEPARTAMENT DE QUÍMICA ANALÍTICA I QUÍMICA ORGÀNICA Campus Sescelades C/ Marcel.lí Domingo s/n 43007 Tarragona Tel. 34 977 55 97 69 Fax 34 977 55 84 46 e-mail: [email protected] FEM CONSTAR que el treball “Identifying human exposure pathways to flame retardants”, que presenta l’Enrique Cequier Manciñeiras per a l’obtenció del títol de Doctor, ha estat realitzat sota la direcció conjunta de la Dra. Rosa Maria Marcé i Recasens del Departament de Química Analítica i Química Orgànica d’aquesta Universitat i del Dr. Georg Becher i la Dra. Cathrine Thomsen de l’Institut de Salut Pública Noruec, i que acompleix els requeriments per poder optar a Menció Europea. I, per a que consti, expedim aquest certificat a Tarragona / Oslo, 18 de Juny de 2014 Dra. Rosa Maria Marcè Dr. Georg Becher Dra. Cathrine Thomsen UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 I acknowledge the Coordinator and all Researchers involved in the splendid project funded by the European Commission and entitled “Indoor Contamination with Flame Retardant Chemicals: Causes and Impacts” (INFLAME) because thanks to all of them I had the opportunity to meet beautiful people, to further develop my career in the environmental research field, to travel around the World, and to experience the Norwegian life style (Jeg likte å vare her og jobbe sammen med dere! Tusen takk!). This work has also been carried out thanks to the support of my supervisors, co-workers and colleagues. Definitely, this Thesis has been much easier to write with their help. Thank you all! In the following lines, I would like to express my gratitude to the closest persons who have had an enormous impact on this work, but their names do not appear along the pages of this Thesis: A mis Abuelos, tanto para los que están como para los que ya nos dejaron, debo agradecerles todo su cariño y apoyo durante todas las etapas de mi vida. Me han enseñado, entre muchas otras cosas, que envejecer merece la pena. Papá, Mamá, es difícil expresar con palabras certeras el profundo agradecimiento y amor que os profeso porque sois las únicas personas del mundo que siempre habéis estado, estáis y estaréis a mi lado. Gracias por todo. A mi hermano, gracias por tener esa constancia para, a pesar de la distancia, hacerme sentir como uno más de la familia tan maravillosa que has formado. Para Elisa, la mujer que ha compartido mis buenos y malos momentos durante esta travesía, me ha mejorado como investigador, me complementa diariamente y me ha hecho pensar en un futuro diferente, gracias por estar ahí. UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 Table of Contents 1. Introduction………………………………………………………………………… 1 1.1. Flame retardants………………………………………………………………... 5 1.1.1. Persistent flame retardants……………………………………………… 9 1.1.2. Organophosphate flame retardants……………………………………… 13 1.2. Occurrence of flame retardants and human exposure pathways……………….. 15 1.3. Human biomonitoring of flame retardants……………………………………... 21 1.4. Analytical methods for determination of flame retardants…………………….. 25 1.4.1. Sample collection and treatment………………………………………… 27 1.4.1.1. Indoor air samples……………………………………………….. 28 1.4.1.2. Dust samples……………………………………………………... 28 1.4.1.3. Blood samples…………………………………………………… 30 1.4.1.4. Urine samples……………………………………………………. 32 1.4.2. Determination techniques………………………………………………... 34 1.4.2.1. Gas chromatography coupled to mass spectrometry………….…. 34 1.4.2.2. Liquid chromatography coupled to mass spectrometry….……… 41 1.5. References……………………………………………………………………… 45 2. Scope of the Thesis…………………………………………………………………. 55 3. Experimental, results and discussion………………………...…………………… 59 3.1. Recruitment of the cohort and sampling campaign……………………………. 63 3.2. Occurrence of flame retardants in indoor air and dust…………………………. 69 3.2.1. Occurrence of a broad range of legacy and emerging flame retardants in indoor environments in Norway………………………………….…... 73 3.2.2. Discussion of the results…………………………………………………. 115 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier Manciñeiras Dipòsit Legal: T 1518-2014 3.3. Human exposure to persistent flame retardants………………………………... 119 3.3.1. The lipid content in serum affects the extraction efficiencies of highly lipophilic flame retardants………………………………………...…….. 123 3.3.2. Determination of emerging halogenated flame retardants and polybrominated diphenyl ethers in serum by gas chromatography mass spectrometry……………………………………………………………... 143 3.3.3. Comparing human exposure to emerging and legacy flame retardants from the indoor environment and diet with concentrations measured in serum………………………………………………………….…...….. 157 3.3.4. Discussion of the results…………………………………………………. 173 3.4. Human exposure to organophosphate flame retardants……...………………… 179 3.4.1. A high-throughput method for determination of metabolites of organophosphate flame retardants in urine by ultra performance liquid chromatography-high resolution mass spectrometry………….………… 183 3.4.2. Human exposure pathways to organophosphate triesters – A biomonitoring study of mother-child pairs…………….……….……... 207 3.4.3. Discussion of the results…………………………………………………. 229 4. Conclusions…………………………………………………………………………. 233 Annex I – List of abbreviations…………………………………………………………. 237 Annex II – List of publications………………………………………………………….. 241 UNIVERSITAT ROVIRA I VIRGILI HUMAN EXPOSURE PATHWAYS TO FLAME RETARDANTS Enrique Cequier
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