Polyvinyl alcohol-based hydrogel sorbent for extraction of parabens in human milk samples by in-tube SPME-LC-UV.

In this work, we developed an in-tube solid-phase microextraction (SPME) device consisting of a fused silica capillary modified with a polyvinyl alcohol (PVOH) hydrogel. Methylparaben, ethylparaben, propylparaben, and butylparaben were determined in human milk samples by using the in-tube SPME device coupled with liquid chromatography with spectrophotometric detection in the ultraviolet region (LC-UV). The inner surface of the fused silica capillary was silanized to allow covalent modification with the PVOH-hydrogel, using glutaraldehyde as cross-linking agent. The developed device was used up to 250 times with no reduction in the analytes' peak areas or carryover effect, besides having a low production cost. The human milk samples showed a significant matrix effect for parabens with higher logKo/w. Low limits of quantification (LLOQ) between 10.0 and 15.0 ng mL-1 were obtained with RSD values in the range of 1.18 to 18.3%. For the intra- and inter-day assays, RSD values from 5.6 to 16.5% and accuracy from 74.5 to 128.8% were achieved. The PVOH-based hydrogel sorbent allowed the use of water as desorption solvent, eliminating the use of organic solvents, which follows the principles of green chemistry. The results showed a great application potential of the PVOH-based hydrogel sorbent for the extraction of organic compounds from high-complexity samples.

Miniaturized systems for gas chromatography: Developments in sample preparation and instrumentation.

An important field of research is the miniaturization of analytical systems for laboratory applications and on-field analysis. In particular, gas chromatography (GC) has benefited from the recent advances in enabling technologies like photolithography, micromachining, hot embossing, and 3D-printing to improve sampling and sample preparation, microcolumn technologies, and detection. In this article, the developments and applications reported since 2015 were reviewed and summarized. Important applications using benchtop instruments, portable GCs, and micro-GCs (µGCs) were showcased to illustrate the current challenges associated with each miniaturized interfaces and systems. For instance, portable instruments need to be energy-efficient and ideally depend on renewable sources for carrier gas generation. Lastly, multidimensional separations were addressed using miniaturized systems to effectively improve the peak capacity of portable systems.