Desarrollo de métodos analíticos para cuantificar perfluorooctano sulfonato y compuestos relacionados en el medio ambiente

Valeria de Lourdes Ochoa-Herrera, Jim A. Field, Reyes Sierra-Alvarez

Resumen

Métodos analíticos basados en 19F NMR y HPLC con detector de conductividad suprimida fueron desarrollados para detectar y cuantificar sulfonato de perfluorooctano (PFOS), ácido perfluorooctanoico (PFOA) y sulfonato de perfluorobutano (PFBS) en muestras ambientales. La separación de los surfactantes perfluorinados (PFAS) se realizó con una columna C18 de fase reversa y una fase móvil compuesta de ácido bórico y acetonitrilo. El límite de detección para PFOS con 19F NMR fue 3.6 mg L-1, mientras que para PFAS con HPLC con detector de conductividad suprimida fue 1 mg L-1. Los límites de detección mejoraron considerablemente si las muestras fueron pre-concentradas a través de una extracción en fase sólida (SPE) registrando valores para PFOS con 19F NMR y HPLC con detector de conductividad suprimida de 3.6 mg L-1 y 10 ug L-1, respectivamente. Esta última demostró ser la mejor técnica para análisis rutinario de cuantificación de contaminantes fluorinados debido a su simplicidad, rapidez y precisión. 19F NMR fue muy efectiva para detectar y caracterizar cambios en la estructura química de los compuestos fluorinados ya que es una técnica analítica altamente específica en la que la matriz ambiental no interfiere con el análisis. El análisis de carbono orgánico total (TOC) y la determinación de la demanda química de oxígeno (COD) para la cuantificación de PFOS en muestras acuosas también fueron estudiados. A pesar de que los análisis de TOC permitieron cuantificar exitosamente PFAS, la falta de especificidad de este método es una limitación considerable. Finalmente, el análisis de PFOS a través de la determinación de COD no fue posible debido a una oxidación incompleta de los altamente estables compuestos fluorinados bajo las condiciones de operación evaluadas.


DOI: http://dx.doi.org/10.18272/aci.v3i2.63

Palabras clave

PFAS; PFOS; PFOA; PFBS; 19F NMR; HPLC; detector de conductividad suprimida; TOC and COD

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