Sample preparation is the rate-limiting step in the success of an analytical
methodology. It is needed not only to clean–up and concentrate the sample but to avoid
the matrix effect and to protect high–cost equipment from deterioration. Therefore, an
appropriate sample pretreatment procedure will improve method sensitivity and
selectivity and increase analyte recovery to achieve a method of high precision and
accuracy that will result in an overall improvement of the performance of the analytical
system. The sample preparation method should be as simple as possible, with minute
sample requirements, easily automatized, and versatile enough to be coupled to
different types of equipment. The new trend in this topic also considers miniaturization
without sacrificing performance and embraces the principles of green and sustainable
chemistry to reduce the costs and consumption of solvents and reagents, devices
corrosion, and excessive disposal. This chapter will review the most recent and
innovative developments in sample preparation applied to pharmaceutical,
environmental, and biological analysis, bearing in mind the above–mentioned
characteristics to achieve an appropriate analytical performance.
Keywords: Carbon Sorbents, Imprinting, Magnetic Nanoparticles, Metal-Organic Frameworks Microextraction, Monoliths, Nanomaterials, Supramolecular Solvents.