For the first time, a germania-based sol-gel coating was used in capillary microextraction (CME) in combination with high-performance liquid chromatography (HPLC). A hydroxy-terminated triblock copolymer, poly(ethylene oxide)-block-poly(propylene oxide)-block-poly(ethylene oxide), was covalently bonded into a sol-gel germania matrix in the course of its creation from an alkoxide precursor via hydrolytic polycondensation reactions. A thin layer of this in situ-created sol-gel hybrid material was covalently anchored to the inner walls of a 0.25 mm i.d. fused silica capillary to produce a sol-gel germania triblock polymeric sorbent in the form of a highly stable surface coating. Such a coating served as an effective extracting phase for the preconcentration of a wide range of polar and nonpolar analytes (e.g., alcohols, amines, ketones, phenols, and polycyclic aromatic hydrocarbons) with nanomolar and picomolar detection limits. Most significantly, the sol-gel germania triblock polymer coating demonstrated impressive resistance to extreme pH conditions, surviving 5 days of continuous exposure to 1.0 M HCl (pH approximately 0.0) or 1.0 M NaOH (pH approximately 14.0), practically without any changes in performance. This shows the suitability of sol-gel germania hybrid organic-inorganic hybrid materials for use as sorbents or stationary phases under extreme pH conditions, often needed in a variety of separation and sample preparation techniques and applications, including ion chromatography, hydrophobic interaction chromatography, proteomics, HPLC with electrochemical detection, isoelectric focusing, and extraction of acidic and basic analytes.

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Sol-gel technology provides a simple and reliable method for solid-phase microextraction (SPME) fiber preparation through in situ creation of surface-bonded organic-inorganic hybrid coatings characterized by enhanced thermal stability and solvent-resistance properties that are important for the coupling of SPME with GC and HPLC, respectively. The sol-gel coating technology has led to the development of an extensive array of sol-gel sorbent coatings for SPME. In this article, sol-gel microextraction coatings are reviewed, with particular attention on their synthesis, characterization, and applications in conjunction with GC and HPLC analyses. In addition, the development of sol-gel-coated stir bars, their inherent advantages, and applications are discussed. Next, the development and applications of sol-gel capillary microextraction (CME) in hyphenation with GC and HPLC is extensively reviewed. The newly emerging germania- and titania-based sol-gel microextraction phases look promising, especially in terms of pH and hot solvent stability. Finally, sol-gel monolithic beds for CME are reviewed. Such monolithic beds are in a position to greatly improve the extracting capabilities and enhanced sensitivity in CME.

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