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26 │
Volumen. 5, Nº 9, diciembre 2021 - mayo 2022, pp. 22-28
Vargas et al. Validación de un método analíco que determina HAP’s en agua.
El intervalo de trabajo fue de 0,002 mg/l a
0,08 mg/l, excepto para el Naftaleno que fue
de 0,008 mg/l a 0,08 mg/l. Se obtuvieron
los valores de incertidumbre para los 15
HAP’s correspondiente al 95% de confianza
presentando valores menores al 35% para
el Fluoreno 34,21%, Fenantreno 26,92%,
Fluoranteno 34,75%, Benzo (a) Antraceno
34,21%, Benzo (b) fluoranteno 32,35%,
Dibenzo (a,h) antraceno 32,05%, Benzo
(g,h,i) perileno 26,92%; y valores entre 35%-
46,01% para el Naftaleno 35,62%, Criseno,
Pireno y Benzo (a) pireno 37,73%, y para el
Acenafteno, Antraceno e Indeno (1,2,3-cd)
Pireno 46,01%.
Los valores obtenidos del porcentaje de
recuperación fueron de 98,41 para el
Fenantreno y Benzo (g,h,i) Perileno, de
101,42 - 101,95 para el Naftaleno, Pireno,
Criseno, Benzo (a) Pireno, Fluoreno y Benzo
(a) Antreceno, de 102,17 - 102,80 para
Fluoranteno, Benzo (b) fluoranteno y Dibenzo
(a,h) Antraceno, y de 104,98 para Acenafteno,
Antraceno, Benzo (k) Fluoranteno e Indeno
(1,2,3-cd) Pireno; demostrando que el
porcentaje de recuperación de cada analito
Analitos
Concentración
mg/l
Repebilidad
% CVr
Precisión
intermedia
% CVR
Incerdumbre
%U
Veracidad
% Recuperación
Naaleno 0,008 a 0,080 5,25 5,59 35,62 101,66
Acenaeno 0,002 a 0,080 5,59 6,58 46,01 104,98
Fluoreno 0,002 a 0,080 4,41 5,19 34,21 101,95
Fenantreno 0,002 a 0,080 3,04 4,08 26,92 98,41
Antraceno 0,002 a 0,080 5,59 6,58 46,01 104,98
Fluoranteno 0,002 a 0,080 2,80 3,96 34,75 102,17
Pireno 0,002 a 0,080 4,44 5,34 37,73 101,42
Benzo (a) Antreceno 0,002 a 0,080 4,41 5,19 34,21 101,95
Criseno 0,002 a 0,080 4,44 5,34 37,73 101,42
Benzo (b) Fluoranteno 0,002 a 0,080 3,61 4,81 32,35 102,80
Benzo (k) Fluoranteno 0,002 a 0,080 5,59 6,58 46,01 104,98
Benzo (a) Pireno 0,002 a 0,080 4,44 5,34 37,73 101,42
Dibenzo (a,h) Antraceno 0,002 a 0,080 5,34 6,48 32,05 102,29
Benzo (g,h,i) Perileno 0,002 a 0,080 3,04 4,08 26,92 98,41
Indeno (1,2,3-cd) Pireno 0,002 a 0,080 5,59 6,58 46,01 104,98
Tabla 2. Coeficientes de variación de Repetitividad y Precisión intermedia
cumple con el objetivo de validación
propuesto ya que todos los valores se
encuentran dentro del rango de 70 - 120%.
CONCLUSIONES
Se realizó un estudio de validación para
la determinación cuantitativa de los
hidrocarguros aromáticos policlínicos en
agua mediante cromatografía líquida de alto
rendimiento con la técnica de extracción
en fase sólida (SPE) en modalidad de
cartuchos Oasis ®HLB. Se desarrollaron
los procedimientos estadísticos de los
parámetros de validación: repetibilidad,
precisión intermedia, incertidumbre,
veracidad, límite de detección y
cuantificación; evaluando cada uno de estos
con los respectivos criterios de aceptación en
función del objetivo planteado.
El desarrollo de un método analítico
instrumental en el equipo HPLC permitió
identificar 15 HAP’s con buena resolución y
simetría. Para la determinación de la exactitud
se calculó el porcentaje de recuperación de
cada uno de los hidrocarburoa aromáticos
policíclicos, encontrando que el porcentaje