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Empleo De Nuevos (Nano)Materiales Para El Desarrollo De Metodologías Analíticas En Los Campos Alimentarios, Farmacéuticos Y Bioanalíticos

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Empleo De Nuevos (Nano)Materiales Para El Desarrollo De Metodologías Analíticas En Los Campos Alimentarios, Farmacéuticos Y Bioanalíticos EMPLEO DE NUEVOS (NANO)MATERIALES PARA EL DESARROLLO DE METODOLOGÍAS ANALÍTICAS EN LOS CAMPOS ALIMENTARIOS, FARMACÉUTICOS Y BIOANALÍTICOS USE OF NEW (NANO)MATERIALS FOR THE DEVELOPMENT OF ANALYTICAL METHODOLOGIES IN FOOD, PHARMACEUTICAL AND BIOANALYTICAL FIELDS Khaled Ali Murtada Departament of Analytical Chemistry and Food Technology Faculty of Sciences and Chemistry Technology University of Castilla-La Mancha Ciudad Real, 2019 EMPLEO DE NUEVOS (NANO)MATERIALES PARA EL DESARROLLO DE METODOLOGÍAS ANALÍTICAS EN LOS CAMPOS ALIMENTARIOS, FARMACÉUTICOS Y BIOANALÍTICOS USE OF NEW (NANO)MATERIALS FOR THE DEVELOPMENT OF ANALYTICAL METHODOLOGIES IN FOOD, PHARMACEUTICAL AND BIOANALYTICAL FIELDS Supervised by Signed. Dr. Ángel Ríos Castro Signed. Dr. Mohammed Zougagh Zariouh Full professor Associate professor Department of Analytical Chemistry and Department of Analytical Chemistry and Food Technology, Faculty of Chemical Food Technology, Faculty of Pharmacy Science and Technology University of Castilla-La Mancha, Spain University of Castilla-La Mancha, Spain Thesis submitted to obtain the degree of International Doctorate in Chemistry Signed. Khaled Ali Murtada Master´s Degree in Chemistry Department of Analytical Chemistry and Food Technology Dr. Gregorio Castañeda Peñalvo, Associate Professor and Secretary of the Department of Analytical Chemistry and Food Technology, University of Castilla-La Mancha. CERTIFY THAT: This research work entitled “USE OF NEW (NANO)MATERIALS FOR THE DEVELOPMENT OF ANALYTICAL METHODOLOGIES IN FOOD, PHARMACEUTICAL AND BIOANALYTICAL FIELDS” constitutes the Doctoral Thesis presented by Mr. Khaled Ali Murtada to obtain the degree of International Doctorate in Chemistry. The Thesis has been developed at the Department of Analytical Chemistry and Food Technology, fulfilling all the academic requirements, under the supervision of Prof. Ángel Ríos Castro and Dr. Mohammed Zougagh Zariouh. And for the record, I hereby issue, and sign this present certificate in Ciudad Real on 26 March, 2019. Signed and approved by: Rosa C. Rodríguez Martín-Doimeadiós Gregorio Castañeda Peñalvo Head of the Department Secretary of the Department Mención Doctorado Internacional Programa de Doctorado en Química por la UCLM, verificado por R.D. 99/2011. Mediante la defensa de esta Memoria de Tesis Doctoral se pretende optar a la obtención de la Mención de “Doctorado Internacional”, habida cuenta de que se reúnen los requisitos que establece el R.D. 99/2011, de 28 de Enero de 2011: 1. Cuenta con los informes favorables de dos doctores pertenecientes a instituciones de Enseñanza Superior de países distintos a España. 2. Uno de los miembros del tribunal que ha de evaluar la Tesis pertenece a un centro de Enseñanza Superior de otro país distinto a España. 3. Parte de la Tesis Doctoral se ha redactado y presentado en una lengua habitual para la comunicación científica de su campo de conocimiento, distinta a cualquiera de las lenguas oficiales de España. 4. El doctorando ha realizado una estancia de tres meses en la Escuela Nacional de Ciencias Aplicadas de la Universidad IBN ZOHR de Agadir (Marruecos), que ha contribuido a su formación y ha permitido desarrollar parte del trabajo experimental de esta Memoria. Index / Índice Index / Índice Index / Índice ................................................................................................................................ IX Dedication / Dedicación ................................................................................................................. I Acknowledgements / Agradecimientos ........................................................................................ II Abstract / Resumen ...................................................................................................................... III Abbreviations / Acrónimos............................................................................................................ V Aim / Objetivo ............................................................................................................................... 1 1. INTRODUCTION ..................................................................................................................... 3 1.1. Analytical Chemistry and Analytical Science ................................................................. 4 1.2. New (nano)materials as analytical tools in non-chromatographic separation techniques: treatment/separation of analytes in food, pharmaceutical and bioanalytical samples ................................................................................................................................... 10 1.2.1. Types of new (nano)materials used in separation by extraction ........................ 11 1.2.2. Types of extraction techniques involving (nano)materials ................................. 21 1.3. New nanomaterials as tools for analytical detection of residues in food, pharmaceutical and bioanalytical samples ............................................................................. 26 References ................................................................................................................................... 32 2. MATERIALS, EQUIPMENT AND METHODS .......................................................................... 41 2.1. Standards, reagents and samples ............................................................................... 42 2.2. Equipment ................................................................................................................... 47 2.3. Methods ...................................................................................................................... 56 2.3.1. Synthesis, decoration and functionalization of nanoparticles .................................. 56 2.3.2. General Procedures used in the extraction/separation of analytes. ........................ 61 References ................................................................................................................................... 66 3. RESULTS AND DISCUSSION .................................................................................................. 67 3.1. Use of nanosized and non-nanosized co-polymer for bio-analytical sample preparation ............................................................................................................................. 68 3.1.1. Strategies for Antidepressants Extraction from Biological Species Using Nanotechnology: A Review ................................................................................................. 70 3.1.2. Determination of antidepressants in human urine extracted by magnetic multiwalled carbon nanotube poly(styrene-co-divinylbenzene) composites and separation by capillary electrophoresis .............................................................................................. 117 3.1.3. Magnetic multiwalled carbon nanotube poly(styrene-co-divinylbenzene) composites for the extraction and LC-MS determination of catecholamines and related compounds in red deer urine and hair ............................................................................. 142 Index / Índice 3.1.4. A simple poly(styrene-co-divinylbenzene)-coated glass blood spot method for monitoring of seven antidepressants using capillary liquid chromatography-mass spectrometry ..................................................................................................................... 166 3.2. Nanoparticles in electrochemical sensors for food and pharmaceutical samples monitoring ............................................................................................................................. 188 3.2.1. Development of an Aluminium Doped TiO2 Nanoparticles-modified Screen Printed Carbon Electrode for Electrochemical Sensing of Vanillin in Food Samples ..................... 191 3.2.2. A Sensitive Electrochemical Sensor Based on Aluminium Doped Copper Selenide Nanoparticles-modified Screen Printed Carbon Electrode for Determination of L-tyrosine in Pharmaceutical Samples ............................................................................................... 209 3.2.3. Decoration of Graphene oxide with Copper Selenide in Supercritical Carbon Dioxide Medium as a Novel Approach for Electrochemical Sensing of Eugenol in Various Samples ........................................................................................................................................... 230 4. Conclusions / Conclusiones ............................................................................................... 253 5. Scientific Self-assessment / Autoevaluación científica ..................................................... 257 Annexes / Anexos ...................................................................................................................... 261 Annexe I. Figure captions / Índice de figuras .................................................................... 262 Annexe II. Table captions / Índice de tablas ...................................................................... 269 Annexe III. Publications / Publicaciones ............................................................................ 272 Annexe IV. Participation of conference papers (oral communications and posters) / Participación en ponencias (comunicaciones orales y pósters). ....................................... 274 Annexe V. Curriculum Vitae .............................................................................................. 276 Dedication
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