Solventless Microextration Techniques for Pharmaceutical Analysis: The Greener Solution

Extensive efforts have been made in the last decades to simplify the holistic sample preparation process. The idea of maximizing the extraction efficiency along with the reduction of extraction time, minimization/elimination of hazardous solvents, and miniaturization of the extraction device, eliminating sample pre- and posttreatment steps and reducing the sample volume requirement is always the goal for an analyst as it ensures the method’s congruency with the green analytical chemistry (GAC) principles and steps toward sustainability. In this context, the microextraction techniques such as solid-phase microextraction (SPME), stir bar sorptive extraction (SBSE), microextraction by packed sorbent (MEPS), fabric phase sorptive extraction (FPSE), in-tube extraction dynamic headspace (ITEX-DHS), and PAL SPME Arrow are being very active areas of research. To help transition into wider applications, the new solventless microextraction techniques have to be commercialized, automated, and validated, and their operating principles to be anchored to theory. In this work, the benefits and drawbacks of the advanced microextraction techniques will be discussed and compared, together with their applicability to the analysis of pharmaceuticals in different matrices.

Ionic liquid-Functionalized Poly-N-phenylpyrrole coating on NiTi Alloy Substrate for highly efficient Solid-phase Microextraction

A novel ionic liquid (i.e. 1-butyl-3-methylimidazolium hexafluorophosphate, [C4MIM]PF6) doped poly-N-phenylpyrrole (PPPy) composite coating ([C4MIM]PF6@PPPy) was successfully fabricated by direct electrochemical polymerization on the surface of NiTi substrate as solid phase...

Molecularly Imprinted Polymers as Solid-Phase Microextraction Fibers for the Isolation of Selected Antibiotics from Human Plasma

The aim of this study was to examine the synthesis of novel molecularly imprinted polymer (MIP)-coated polythiophene and poly(3-methylthiophene) solid-phase microextraction fibers using the direct electropolymerization method. Synthesized SPME fibers were characterized with the use of various physicochemical instrumental techniques. MIP-SPME coatings were successfully applied to carry out the selective extraction of selected antibiotic drugs (amoxicillin, cefotaxime, metronidazole) and their metabolites (amoxycilloic acid, amoxicillin diketopiperazine, desacetyl cefotaxime, 3-desacetyl cefotaxime lactone, hydroxymetronidazole). Solid-phase microextraction parameters for the simultaneous determination and identification of target compounds were optimized using the central composite design (CCD), and they accounted for 5–15 min for desorption time, 3–10 for the pH of the desorption solvent, and 30–100 μL for the volume of the desorption solvent. High-performance liquid chromatography and mass spectrometry (MS) detectors such as quadrupole time-of-flight (Q-TOF MS) and triple quadrupole (QqQ MS) were applied to determine and to identify selected antibiotic drugs and their metabolites. The MIP-coated SPME are suitable for the selective extraction of target compounds in biological samples from patients in intensive care units.

Destabilization of Immersed Dense Granular Material Submitted to Localized Fluidization: An Experimental and Numerical Study

An alternative experimental approach and a numerical analysis for the study of destabilization by localized fluidization of an immersed dense granular material are presented. To visualize the evolutions of the internal structure of the granular medium, the hydrogel beads, composed of about 99% of water and having substantially the same refraction indexes, are used as solid phase. A LED lighting system is used in place of a laser lighting system. As a result, the optical access restriction of porous structure is removed. A real economic alternative for the experimental study of fluid-grain coupling during destabilization by localized fluidization of a granular material is created. The experimental phenomenology presented in the literature is verified: the system passes successively through three different stationary regimes: static regime, fluidized cavity regime, and fluidized chimney regime. Some restrictions of using hydrogel beads as particles in the study of liquid-solid interaction are also discussed.