This article describes the fabrication of porous nicotinic acid-functionalized chito-oligosaccharide-bonded titania/silica hybrid monoliths (TiO2/SiO2@ChO-N) through a co-gelation sol-gel process. A capillary monolith with a well-defined and homogeneous structure was obtained by controlling the hydrolysis speed of titanium alkoxides in a sol mixture by using glycerol and acetylacetone. As a result of the functionalization with chito-oligosaccharides (ChO)-modified nicotinic acid, the obtained stationary phase provides superior physiochemical properties, such as a cationic hydrophilic surface, porosity, and mechanical strength. Scanning electron microscope and attenuated total reflectance-infrared spectroscopy were used to characterize the functionalized monolithic columns. The produced capillary columns showed high chromatographic performance with acceptable selectivity for charged analytes as well as organic polar compounds such as nucleic bases, nucleosides, carbamate pesticides, and strobilurin fungicides. The obtained results also indicated that the functionalized ChO's amino, amide, hydroxyl, and pyridinium ring moieties served as hydrophilic electrostatic traps for charged substances, in addition to stroing π-π interaction with the carbamate pesticides and strobilurin fungicides analytes via hydrogen bonding.
Analytical processes involving sample preparation, separation, and quantifying analytes in complex mixtures are indispensable in modern-day analysis. Each step is crucial to enriching correct and informative results. Therefore, sample preparation is the critical factor that determines both the accuracy and the time consumption of a sample analysis process. Recently, several promising sample preparation approaches have been made available with environmentally friendly technologies with high performance. As a result of its many advantages, solid-phase extraction (SPE) is practiced in many different fields in addition to the traditional methods. The SPE is an alternative method to liquid-liquid extraction (LLE), which eliminates several disadvantages, including many organic solvents, a lengthy operation time and numerous steps, potential sources of error, and high costs. SPE advanced sorbent technology reorients with various functions depending on the structure of extraction sorbents, including reversed-phase, normal-phase, cation exchange, anion exchange, and mixed-mode. In addition, the commercial SPE systems are disposable. Still, with the continual developments, the restricted access materials (RAM) and molecular imprinted polymers (MIP) are fabricated to be active reusable extraction cartridges. This review will discuss all the theoretical and practical principles of the SPE techniques, focusing on packing materials, different forms, and performing factors in recent and future advances. The information about novel methodological and instrumental solutions in relation to different variants of SPE techniques, solid-phase microextraction (SPME), in-tube solid-phase microextraction (IT-SPME), and magnetic solid-phase extraction (MSPE) is presented. The integration of SPE with analytical chromatographic techniques such as LC and GC is also indicated. Furthermore, the applications of these techniques are discussed in detail along with their advantages in analyzing pharmaceuticals, biological samples, natural compounds, pesticides, and environmental pollutants, as well as foods and beverages.