Palabras clave: contaminantes, proceso de extracción, análisis químico, cromatografía de gases RESUMEN La metodología QuEChERS fue implementada para la extracción de catorce plaguicidas, diez organoclorados y cuatro organofosforados en muestras de suelo. El análisis se llevó a cabo por cromatografía de gases acoplado a una trampa de iones cuadrupolar en tándem (MS 2 ). La extracción de los plaguicidas por la metodología seleccionada se ve afectada por diferentes factores, por tanto, la optimización del proceso de extracción incluyó el uso de dos diseños experimentales: un diseño ortogonal Taguchi inicial para determinar los factores de mayor influencia y posteriormente, un diseño factorial fraccionado 2 5-1 para determinar las condiciones óptimas preparativas. Los resultados mostraron que, el pH, el ultrasonido y el uso de adsorbentes de limpieza son factores poco relevantes en el proceso de preparación. Por el contrario, la cantidad de agua en la matriz, la relación muestra:solvente y las cantidades de MgSO4 y NaCl como sales de partición, juegan un rol importante dentro del proceso. El método final consistió en la hidratación del suelo con 5 mL de agua tipo I, utilizando 10 g de muestra, agitación por 1 min, adición de 10 mL de acetonitrilo como solvente extractor, desplazamiento salino con 2 g de MgSO4, 2 g de NaCl y limpieza final del extracto con 100 mg de octadecilsilano (C18), 10 mg de carbón grafitado y 600 mg de MgSO4 (por mL de extracto). Con el método obtenido, los plaguicidas estudiados pueden ser extraídos cuantitativamente de la matriz, con recuperaciones entre 70 y 120 %, coeficientes de variación menores al 10 % y límites de detección entre 4.9 y 21.7 μg/kg. Key words: contaminants, extractive process, chemical analysis, gas chromatography ABSTRACT The QuEChERS methodology was implemented for the extraction of fourteen pesticides, ten organochlorines and four organophosphates in soil samples. The analysis was carried out by gas chromatography coupled to a quadrupole ion trap in tandem mode (MS 2 ). The extraction of the pesticides by the selected methodology is affected by different factors. Therefore, the extraction process optimization included the use of two experimental designs: a Taguchi orthogonal design to determine most influential factors and, subsequently, a fractional factorial design 2 5-1 to determine the optimal
Four types of soils were prepared with humified matter, bentonite, kaolin and inert matter, in order to control the organic matter (OM) content in the evaluation of retention of lead (II) by adsorption in disturbed soils with the possibility of being contaminated. The results indicated that retention capacity of Pb+2 increases as organic matter increases, however, this retention is not proportional to the organic matter increment. An increase of 10 units in the concentration of the background solution results in a decrease in the retention capacity of 50%. The outcomes also indicated that lead (II) adsorption is successfully explained by the Langmuir model and the adsorption kinetics fitted well to the Ho pseudo second order model. The thermodynamic values of the Gibbs free energy indicated that it was a spontaneous process and the energy of the process suggests a retention mechanism by ion exchange. A soil with high content of organic matter does not guarantee high retention of lead, even more so when the adsorption mechanism is given by ion exchange.
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