In agriculture, a wide range of OPPs has been employed to boost crop yield, quality, and storage life. However, due to the ever-increasing population and rapid urbanization, pesticide use has surged in recent years. These compounds are exceedingly poisonous to humans, and despite the fact that specific legislation prohibits their use, the frequency of toxic and/or fatal incidents, as well as current statistics, suggest that they are currently accessible. As a result, determining the exposure to these substances as well as their detection (and that of their metabolites) in different types of exposed samples has become a hot issue in terms of quality and safety concerns. However, developing tools for the evaluation of these substances is a critical challenge for laboratories. Various chromatographic-based methods reported in the period of 2015-2020 have been developed, which are summarized and critically reviewed in this article, including the extraction of the target OPPs from different kinds of matrices. A comparison among the extraction and analysis techniques has been made in the current review article.