A simplified one-pot derivatization/magnetic solid-phase extraction with integrated pH adjustment strategy coupled with liquid chromatography-fluorescence detection for fatty aldehyde analysis

A novel one-pot derivatization/magnetic solid-phase extraction with integrated pH adjustment (OPD/MSPE-pH) strategy was developed for the efficient and selective quantification of fatty aldehydes. This method seamlessly integrates pH regulation, derivatization, and magnetic separation in a single incubation step, where the sample solution, derivatization reagent, and magnetic composite (Fe₃O₄/MWCNTs-OH/CA) are processed together, significantly simplifying sample preparation. The magnetic composite, synthesized from Fe₃O₄ nanoparticles, hydroxylated multi-walled carbon nanotubes (MWCNTs-OH), and citric acid (CA), functions both as an acidic pH regulator and an efficient adsorbent for aldehyde-fluorenylmethyl carbazate (FMC) derivatives. Compared to conventional approaches, the OPD/MSPE-pH method exhibited superior operation efficiency, achieving low limits of detection (1.1–2.4 nM) and high recoveries (91.7–106.1%). The optimized procedure was successfully applied to plasma and spiked plasma samples, demonstrating its effectiveness in complex biological matrices. This streamlined technique eliminates the need for additional pH-adjusting reagents and centrifugation, offering a practical, rapid, and highly efficient solution for fatty aldehyde analysis. Overall, the proposed OPD/MSPE-pH method provides a robust, sensitive, and reliable analytical platform for fatty aldehyde analysis, with potential applications in broader fields with suitable modifications.