Desarrollo de un Método para la Especiación de Selenio en Muestras de Cerveza

Development of a Method for the Speciation of Selenio in Beer Samples

  • Jenifer Smith
  • Marinela Colina
  • Gilberto Colina
  • Brinolfo Montilla

Resumen

Se desarrolló un método por cromatografía iónica (CI) para la especiación de selenio en muestras líquidas de cerveza, empleando H2O2 y luz UV como sistema oxidante. Las especies aniónicas de selenio fueron separadas utilizando una columna aniónica AS4A y un guarda columna AG4 Dionex, la fase móvil empleada fue de 1,7 mM NaHCO3/1,8 mMNa2CO3, para la cuantificación se empleó un detector de conductividad iónica. El tiempo de retención del ión Se(IV) fue de 7,8 min y para Se(VI) de 15,7 min. Los límites de detección obtenidos para Se(IV) y Se(VI) fueron de 0,15 y 0,28 mgL-1, respectivamente. Se establecieron las condiciones óptimas de análisis del proceso de oxidación de los compuestos puros de selenio: selenito y selenio-DL- metionina, mediante el estudio de diferentes parámetros como cantidad de peróxido adicionado, tiempo de digestión y pH. La separación de los iones Se(IV) y Se(VI) en muestras de cerveza se realizó empleando una fase móvil de 2,0 mM de carbonato de sodio y 1,0 mM de hidróxido de sodio, ésta mezcla separa los iones de selenio sin tener problemas de interferencias de nitrato, fosfato y sulfato. Los límites de detección determinados para Se(IV) y Se(VI) fueron 0,08 y 0,07 mgL-1, respectivamente. El método desarrollado se comparó con un método referencial ICP AES, obteniéndose excelentes resultados.


Palabras clave: Especiación, selenio, cerveza, cromatografía iónica. 


 


ABSTRACT


In this work, analytical methodologies were developed for the determination of mercury levels in blood and plasma samples of patients with leukemia registered at the Haematological Institute of the West, Maracaibo, evaluating the total concentration of Hg and its chemical species in blood samples from the patients studied (n = 34) and of control subjects (n = 5), by the HPLC-ICP-MS. The calculated limit of detection found for the determination of Hg in blood and plasma was 1.39 μg Hg/L and the limit of quantification was 1.39 μg Hg.L-1. The total mercury concentrations in blood and plasma of 16.89±8.76 μg Hg.L-1 [8.22-45 μg Hg.L-1] and 25.77±5.12 μg Hg.L-1 [10.6-40.87μg Hg.L-1] respectively and for the control population were 25.3637±11.4 [10.6-40.87 μg Hg.L-1] and 74.46±16.09 [64.38-102.82 μg Hg.L-1]. The mean of Hg-S of the group of males evaluated was 16.08±7.85 µg Hg.L-1, and in females were 18.68±10.05 μg.L-1, the mean of Hg-S in the females was significantly higher (P <0.05) than the mean Hg-S observed. The detection limits for the Hg chemical species studied in blood are: Hg+ (0,7 µg Hg.L-1), Hg+2 (0,53 µg Hg.L-1). The concentrations found for Hg+2 and CH3Hg+ in leukemia patients in blood and plasma were 8.16±1.67 [6.96-10.97], 9.85±6.22 μg Hg+2.L-1 [6.04-20.74], and 11.47±4.33 μg Hg+2.L-1 [7.28-18.63], 11.28±5.40 [6.24-18.63] respectively, while for the control population were 10.04±3.84 μg Hg+2.L-1 [5.41-15.86], 12.24±5.76 [6.00-21.37] and 33,48±8.62 μg Hg+2.L-1 [27.59-48.36], 28.44±13.13 [18.25-50.23]. 


Key words: leukemia, mercury, blood, plasma.

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Publicado
2018-04-30
Sección
Ciencias Químicas