The global concern about food safety and environment quality has produced the development of a legal framework to control residues of organic compounds (e.g. pesticides and veterinary and human drugs). In this context, the establishment of analytical methods achieving satisfactory performances in terms of sensitivity, selectivity, resolution, identification, sample throughput, and applicability, is mandatory. Multiresidue methods mainly based on chromatographic techniques [i.e., gas chromatography (GC) and liquid chromatography (LC)] coupled to mass spectrometry (MS) are currently applied in routine laboratories. Furthermore, capillary electrophoresis (CE) has emerged as an alternative to LC and GC, owing to the development of on‐line preconcentration strategies for sensitivity enhancement. The recent integration of ion mobility spectrometry (IMS) in LC‐MS workflows also involves new possibilities for the separation of isomeric and isobaric residues, as well as for the separation of analytes of interest from background noise. New trends in multiresidue analysis point towards ambient ionization mass spectrometry (AIMS) strategies, which avoid chromatographic separations and substantially reduce analysis time. On the other hand, sample preparation has evolved through the development of miniaturized and environmentally friendly procedures according to the Green Chemistry principles. In addition, generic extraction procedures for multiclass analysis have been optimized, increasing sample throughput. This article aims to show an overview of the current trends in the analysis of pesticide and drugs in food and environmental samples, discussing the relevant advances in sample treatments and the technological evolution of the instrumental techniques. We hope to offer with this article a critical review of the analytical possibilities for routine analysis laboratories focused on monitoring of residues.
