Development of the Space-Resolved Solid-Phase Microextraction Technique and Its Application to Biological Matrices

Abstract

To facilitate rapid in situ analyte monitoring within heterogeneous samples, a space-resolved solid phase microextraction (SR-SPME) technique was developed that utilized miniaturized segmented fibers. Initially, a multilayered agarose gel was used to determine the effects of diffusion-based mass transfer and fiber dimension on the space-resolving capability of SPME. For diazepam within agarose gel, the SR-SPME limit of detection was 2.5 ng/mL, with a linear dynamic range up to 500 ng/mL. The efficacy of the SR-SPME technique was further evaluated within diverse biological matrices (onion bulb, fish muscle, and adipose tissues) containing stratified pharmaceutical analytes. Empirically, the results agreed well with established techniques such as microdialysis and liquid extraction, but SR-SPME was simpler to implement, displayed higher spatial resolution, and was more cost-effective than traditional approaches. Additionally, the segmented design of the SPME fibers and stepwise desorption protocols offer potential advantages within high throughput applications.

In vivo solid-phase microextraction for single rodent pharmacokinetics studies of carbamazepine and carbamazepine-10,11-epoxide in mice

“…Initially, in vivo SPME was applied to study the pharmacokinetics (PK) of diazepam and its primary metabolites in the circulating blood of Beagle dogs because of their large blood vessel size which permitted direct intravenous sampling using an in-dwelling catheter [2][3][4][5]. More recently, in vivo SPME was successfully applied to fish to study bioaccumulation of pharmaceuticals using direct muscle sampling [6,7], and to rats for PK studies of benzodiazepine drugs in the bloodstream [8].…”

In-situ hydrothermal synthesis of titanium dioxide nanorods on titanium wire for solid-phase microextraction of polycyclic aromatic hydrocarbons

“…Although solid-phase extraction (SPE) is the most popular method of extracting organics from aqueous samples, SPME has various advantages over SPE, such as a shorter extraction time, a smaller sample volume, solvent-free extraction, and higher enrichment efficiency. As it is a rapid, sensitive, and economical method [6], SPME has been widely applied in environmental testing [7], biological analysis [8], drug monitoring [9], and food testing [10]. However, commercial SPME fibers are costly and have some disadvantages, including low thermal and chemical stability, coating fragility, it is relatively easy to strip off the coating, and they have a tendency to expand in organic solvents [11].…”

Phenyl-functionalization of titanium dioxide-nanosheets coating fabricated on a titanium wire for selective solid-phase microextraction of polycyclic aromatic hydrocarbons from environment water samples

“…It integrates sample extraction, concentration and introduction into one step, and easily couples to gas chromatography (GC) and high-performance liquid chromatography (HPLC). Hence, this technique has been successfully applied to environmental [2], biological [3] and food [4] analyses. Although the application of SPME is widespread, commercialized fibers are expensive and also suffer from some drawbacks such as low thermal and chemical stability, fragility, stripping of coatings and easily swelling in organic solvents [5].…”