For analytic determination, it is necessary to have an appropriate methodology for desorption and quantification of the VOCs present in the monitor. In this sense, an analytic methodology was conducted and optimized which allowed an adequate separation and resolution of a mixture of 23 Volatile Organic Compounds, of which only the ethyl-benzene - m-xylene pair could not be solved in an short time run (36 final minutes) and a simple technique of extraction of the monitor’s matrix by using the dichloromethane: methanol (50:50) mixture recoveries higher than 66% are obtained except for styrene (25.4%), with standard deviations lower than 5%.