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Summary: Bioanalysis of endogenous substances, metabolites, and contaminants poisons is important in analyses of biological functions, metabolomics, forensic toxicology, patient diagnosis and biomonitoring of human exposure to hazardous chemicals. In these analyses, methods of sample preparation are essential for the isolation and concentration of target analytes from complex biological matrices. These processes, however, are time-consuming, labor-intensive and error-prone, and markedly influence the reliability and accuracy of determining target analytes. Thus, efficient sample preparation techniques and their integration with analytical methods have become significant. Solid-phase microextraction (SPME) is a simple and convenient sample preparation technique that has enabled automation, miniaturization, high-throughput performance, and online coupling with analytical instruments. Moreover, SPME has reduced analysis times, as well as solvent and disposal costs.This reprint consists of 14 original, peer-reviewed papers for the Special Issue in the MDPI journal Molecules. The topics covered include headspace fiber SPME (HS-SPME) gas chromatography-mass spectrometry (GC-MS), HS-in-needle microextraction GC-MS, thin film SPME liquid chromatography-tandem mass spectrometry (LC-MS/MS), magnetic solid phase extraction LC-MS/MS, in-tube SPME LC-MS/MS and in-tube SPME LC-UV. Samples analyzed include plant-derived volatile organic compounds; body odor; metabolites in urine, plasma and saliva sample; and biomarkers of tobacco smoke exposure in hair and environmental estrogens.

Summary: In recent years, inorganic oxidic nanomaterials have been extensively investigated for their outstanding properties that allow their use within a large variety of raising fields of interest, ranging from (photo)catalysis to the development of functional nanocomposites. Nanoscopic metal (eventually mixed) oxides are often fabricated following soft-chemistry approaches, characterized by the possibility of favouring specific morphologies, particles dimensions, and surface porosities through different synthetic methods and templating processes. In this context, surface functionalities and reactivity play a major role in the determination of nanomaterials final properties. For this reason, further surface functionalization with specific chemical moieties is often recommended to extend their field of application. This Special Issue, now edited as a book, aimed at extending the comprehension of the mechanisms involved in the synthesis and templating of inorganic oxidic nanomaterials, as well as in their surface functionalization and reactivity. Additionally, this Special Issue aimed at increasing the knowledge on the latest advances of these systems in (photo)catalysis, environmental clean-up processes, energy storage, controlled transport and/or release, biomedicine, sensing, development of smart-materials, stimuli-responsive materials, and nanocomposites. Nanomaterials of interest included: silica, alumina, titania, zirconia, zinc oxide, aluminosilicates, iron oxides, perovskites and titanates, rare earth oxides, and composites. Furthermore, particular attention was dedicated toward studies describing alternative ecofriendly preparation methods.