Implementación de la técnica de extracción por adsorción con disco rotatorio usando un eco-sorbente con arcillas modificadas para el análisis de estrógenos en efluentes hospitalarios por medio de cromatografía de líquidos

dc.contributorRosero-Moreano, Milton
dc.contributorGrupo de Investigación en Cromatografía y Técnicas Afines (Categoría A1)
dc.creatorLÓPEZ, CARLOS ANDRÉS
dc.date2022-02-22T22:37:05Z
dc.date2022-05-30
dc.date2022-02-22T22:37:05Z
dc.date2022-02-22
dc.date.accessioned2023-09-06T18:33:31Z
dc.date.available2023-09-06T18:33:31Z
dc.identifierhttps://repositorio.ucaldas.edu.co/handle/ucaldas/17444
dc.identifierUniversidad de Caldas
dc.identifierRepositorio institucional Universidad de Caldas
dc.identifierhttps://repositorio.ucaldas.edu.co/
dc.identifier.urihttps://repositorioslatinoamericanos.uchile.cl/handle/2250/8699202
dc.descriptionIlustraciones, gráficas
dc.descriptionspa:En la determinación de analitos, es fundamental preparar la muestra antes de hacer la introducción en el sistema de análisis, por lo tanto, es necesario aplicar diversas técnicas entre ellas la extracción y microextracción. Actualmente se buscan métodos de extracción que sean más amigables con el medio ambiente, que faciliten el mejoramiento de las técnicas analíticas con ayuda de los principios de la química verde; por ejemplo, realizar análisis con el menor uso de sustancias contaminantes, al igual que disminuir el tiempo de análisis y de trabajo experimental. Estos procesos, son trascendentales en el análisis de compuestos como estrógenos E3, E2 y EE2, encontrados en cantidades traza y con actividad biológica potencialmente peligrosa en animales. Entre estos compuestos, se encuentran las hormonas y tanto las naturales, como las sintéticas, pueden llegar al medio acuoso a través de diferentes vías, siendo la fuente principal la descarga al medio de las plantas de tratamiento de aguas residuales (PTAR´s) y debido a su eliminación incompleta, estos compuestos siguen presentes en el medio acuático con concentraciones que suelen ser del orden de pg a ng L-1 y son las aguas residuales hospitalarias consideradas como uno de los principales focos de contaminación emergente, debido a las distintas actividades que allí se realizan, donde se incluyen trabajos de investigación, laboratorio clínico y la excreción de pacientes que están recibiendo tratamiento con un variado número de sustancias para un amplio rango de enfermedades; el contexto actual plantea una serie de interrogantes frente a la baja tasa de remoción de compuestos que son altamente recalcitrantes, con baja biodegradabilidad y remoción por medio de tratamientos convencionales, por lo que pueden llegar a los sistemas de alcantarillado urbano o fuentes de agua potable lo que constituye un potencial riesgo para la salud humana y en este sentido se necesitan metodologías analíticas, rápidas, sensibles y selectivas para su determinación. Este trabajo, se basa en la implementación de un método analítico de extracción por adsorción con disco rotatorio (RDSE) empacado con arcillas modificadas con líquidos iónicos, para el análisis de estrógenos E3, E2 y EE2 provenientes de muestras acuosas de plantas de tratamiento de aguas residuales de hospital; los analitos de interés son 17β-estradiol (E2), estriol (E3) y 17α-etinilestradiol (EE2). Los compuestos en las muestras se extrajeron por extracción con RDSE a partir de muestras dopadas y fueron leídas por cromatografía líquida de alta eficiencia con detector de arreglo de diodos y fluorescencia en serie (HPLC-PDA-FL), usando como patrones las hormonas (E2), (E3) y (EE2) se realizaron extracciones con adsorbente comercial (C18) y arcillas modificadas con líquidos iónicos tipo [C16MIM+] [anión-], con distintos aniones [Br-], [BF4-] y [OH-], obteniéndose porcentajes de recuperación con rangos de 24 a 26%, 42 a 48% y 57 y 67% para E3, E2 y EE2 respectivamente los cuales mostraron competitividad con la fase adsorbente comercial C18. Las condiciones óptimas de extracción fueron las siguientes: volúmenes de muestra de 10 mL, tiempo de extracción de 60 minutos, temperatura de extracción de 30 °C y 1500 rpm, bajo estas condiciones, las recuperaciones han sido de adecuadas para este tipo de técnicas de extracción, reproducibles y con bajos límites de detección. Los límites de detección alcanzados con la técnica de RDSE fueron de 0,18; 0,15 y 0,07, ng mL -1 y con linealidades de 0,9963, 0,9995 y 0,9915 para E3, EE2 y E2 respectivamente. Con ayuda de la técnica de RDSE se alcanzaron factores de concentración de 13, 23 y 32 para E3, EE2 y E2 respectivamente, mientras que en lectura de muestra reales la RSDE intradisco alcanzó valores máximos de 12 % siendo la E3 la de mayor % RSD y la E2 la de menor variabilidad con 7 %. La lectura de muestras reales arrojó valores promedio de las 3 hormonas en concentraciones de 4,30; 3,85 y 7,23 ng mL-1 en afluente y 3,81; 1,33 y 4,00 ng mL-1 en efluente para E3, E2 y EE2 respectivamente
dc.descriptioneng:Human steroid hormones pose a danger to human health. These hormones are classified as emerging pollutants and endocrine disrupting compounds. 17α- ethinylestradiol (EE2) and 17β-estradiol (E2) and estriol (E3) are present in wastewater samples in amounts expressed in ng L-1. Using the spinning disk sorption extraction (RDSE) method with different sorbent phases, such as ionic liquid modified clays, we analyzed human steroid hormones in wastewater samples. We modified the natural clay, by introducing ionic liquid ([C16MIM+] [anion], anion = Br-, OH- or BF4- between its intermediate layers. After extraction, the analytes were read with the help of chromatography (HPLC- PDA-FL). The technique achieved recoveries of 63% for EE2, 45% for E2 and 25% for E3. Finally, the method achieved detection and quantification limits between 0.18 and 0.42, 0.15 and 0.37, 0.07 and 0.16 ng mL- 1 for E3, E2 and EE2, respectively, with the modified clays. In a wastewater plant, the method yielded mean concentration values of 4.30, 3.85 and 7.23 ng mL-1 in the effluent, and 3.81, 1.33 and 4.00 ng mL-1 in the effluent for E3, E2 and EE2, respectively An efficient and replicable method has been applied for the extraction of estrogens in wastewater with relevant adequate results.
dc.description1. Introducción / 2. Objetivos/ 2.1 Objetivo General / 2.2 Objetivos Específicos/ 3. Planteamiento del Problema / 4. Justificación / 5. Marco Teórico/ 5.1 Contaminantes Emergentes/ 5.1.1 Contaminantes emergentes en el agua / 5.1.2 Contaminantes emergentes caso especial de estrógenos / 5.2 La Disrupción Endocrina Y Su Relación Con Los Contaminantes Emergentes/ 5.3 Tratamiento De Contaminantes Emergentes En Aguas/ 5.3.1 Estado de los contaminantes emergentes en el ambiente y su relación con las plantas de tratamiento/ 5.4 Plantas De Tratamiento De Aguas/ 5.4.1 Origen y evolución de los tratamientos en aguas/ 5.5 Preparación De Muestras Miniaturizada (Técnicas De Extracción Y Microextracción)/ 5.5.1 Análisis bibliométrico de técnicas analíticas de extracción y microextracción/ 5.5.2 Importancia de las técnicas de extracción y microextracción/ 5.5.3 Ventajas de las técnicas de microextracción/ 5.5.4 Las nuevas técnicas de microextracción / 5.6 Extracción Por Adsorción Con Disco Rotatorio RDSE/ 5.6.1 Modos de trabajo en la extracción por adsorción con discos rotatorios RDSE/ 5.7 Fases Eco-Sorbentes Con Utilidad En Procesos De Extracción / 5.7.1 Arcillas naturales Montmorillonitas / 5.7.2 Características y propiedades de las montmorillonitas/ 5.7.3. Desarrollo y aplicación de nuevos materiales utilizando montmorillonitas y líquidos iónicos/ 5.7.4 Uso de bentonitas y líquidos iónicos como eco-sorbentes/ 5.7.5 Mecanismos de interacción entre líquidos iónicos y minerales tipo arcilla/ 5.1 Métodos De Extracción De Hormonas En Agua Residual / 5.2 Sistema De Análisis HPLC Para Hormonas En Aguas/ 5.3 Moléculas De Estudio / 6 6. Materiales y Métodos/ 6.1 Reactivos/ 6.2 Instrumentación/ 6.3 Condiciones Cromatográficas/ 6.4 Síntesis De Líquidos Iónicos/ 6.5 Purificación Y Funcionalización De Las Arcillas/ 6.6 Extracción Y Desorción De Los Analitos Usando Adsorbentes Comerciales Y Arcillas Modificadas Con La Técnica De RDSE / 6.7 Validación Del Método / 6.8 Optimización De Los Parámetros De Extracción / 6.9 Análisis De Muestras Reales/ 7. Resultados y Análisis/ 7.1 Arcillas Modificadas/ 7.1.1 Espectroscopia FT-IR para MMT pura y MMT modificada / 7.1.2 Difracción por rayos X (XRD) de arcilla MMT modificada / 7.1.3 Análisis por microscopía electrónica de barrido SEM / 7.2 Validación Del Método Analítico / 7.2.1 Límites de detección y cuantificación/ 7.2.2 Modelo de regresión lineal y figuras de mérito / 7.3 Optimización Del Método De Extracción/ 7.3.1 Control de variables de extracción dependientes del tiempo y la velocidad de agitación RDSE/ 7.3.2 Efecto de la cantidad de adsorbente en la RDSE usando arcilla modificada con líquidos iónicos/ 7.3.3 Efecto de la cantidad de muestra en la extracción RDSE para hormonas / 7.3.4 Efecto de la temperatura en la extracción RDSE para hormonas/ 7.3.5 Variables óptimas de extracción RDSE/ 7.4 Características Analíticas Del Método Usando RDSE/ 7.5 Tiempo De Desorción Y Volumen Del Eluyente Para El Uso De La RDSE / 7.6 Selección Del Tipo De Adsorbente Para La Extracción Con RDSE / 7.7 Selección De La Arcilla Modificada/ 7.8 Análisis De Muestras Reales En La Planta De Tratamiento Del Hospital Santa Sofía De Caldas/ 7.8.1 Mediante el uso de arcilla en el proceso de extracción/ 7.8.2 Análisis de los sitios de muestreo usando arcilla como adsorbente/ 7.8.3 Análisis del tiempo de muestreo usando arcillas en la extracción/ 7.8.4 Comparativo mediante el uso de C18 y arcilla modificada en el proceso de extracción/ 7.8.5 Análisis de los sitios de muestreo usando C18 como adsorbente/ 8. Conclusiones/ 9. Recomendaciones / 10. Bibliografía / 11. Anexos/ 11.1 Tratamiento En Aguas Caso Especial Estrógenos / 11.2 Caso Específico De Colombia En Tratamientos De Agua Residual.
dc.descriptionMaestría
dc.descriptionNo se autoriza publicacion de tesis, hasta tanto no se publique en articulo cientifico de la revista Water Science and Technolgy
dc.descriptionMagister en Química
dc.descriptionTécnicas de preparación de muestras y análisis de contaminantes emergentes
dc.formatapplication/pdf
dc.formatapplication/pdf
dc.formatapplication/pdf
dc.formatapplication/pdf
dc.languageeng
dc.languagespa
dc.publisherFacultad de Ciencias Exactas y Naturales
dc.publisherManizales
dc.publisherMaestría en Química
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dc.rightsinfo:eu-repo/semantics/closedAccess
dc.rightsinfo:eu-repo/semantics/closedAccess
dc.rightsinfo:eu-repo/semantics/closedAccess
dc.rightsinfo:eu-repo/semantics/closedAccess
dc.rightshttp://purl.org/coar/access_right/c_14cb
dc.subjectAguas residuales
dc.subjectAnálisis químico
dc.subjectContaminación
dc.subjectLíquido iónico
dc.subjectContaminante emergente
dc.subjectHormonas estrogénicas
dc.subjectMontmorillonita
dc.subjectArcilla natural
dc.subjectExtracción por adsorción con disco rotatorio
dc.titleImplementación de la técnica de extracción por adsorción con disco rotatorio usando un eco-sorbente con arcillas modificadas para el análisis de estrógenos en efluentes hospitalarios por medio de cromatografía de líquidos
dc.typeTrabajo de grado - Maestría
dc.typehttp://purl.org/coar/resource_type/c_bdcc
dc.typeText
dc.typeinfo:eu-repo/semantics/masterThesis
dc.typehttps://purl.org/redcol/resource_type/TM
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