Dispersive magnetic solid-phase extraction for capsaicinoid compounds in human serum using LC-HRMS: targeted and non-targeted approaches

Abstract

A new analytical method based on the use of dispersive magnetic solid-phase extraction (DMSPE) is described for the preconcentration of capsaicin (CAP), dihydrocapsaicin (DCAP), and N-vanillylnonanamide (PCAP) from human serum samples. The influence of several experimental factors affecting the adsorption (nature and amount of magnetic material, adsorption time, and pH) and desorption (nature of solvent, its volume and desorption time) steps was studied. Among seven different nanomaterials studied, the best results were obtained using magnetic multiwalled carbon nanotubes, which were characterized by means of spectrometry- and microscopy-based techniques. Analyses were performed by ultra-high-performance liquid chromatography with quadrupole-time-of-flight mass spectrometry using electrospray ionization in positive mode (UHPLC-ESI-Q-TOF-MS). The developed method was validated by obtaining several parameters, including linearity (0.3–300 μg L−1 range), and limits of detection which were 0.1, 0.15, and 0.17 μg L−1 for CAP, DCAP, and PCAP, respectively. The repeatability of the method, expressed as relative standard deviation (RSD, n = 7), varied from 3.4 to 11%. The serum samples were also studied through a non-targeted approach in a search for capsaicinoid metabolites and related compounds. With this objective, the fragmentation pathway of this family of compounds was initially studied and a strategy was established for the identification of novel or less studied capsaicinoid-derived compounds. Graphical abstract

Magnetic materials as adsorbents for the pre‐concentration and separation of active ingredients from herbal medicine

“…Rodríguez‐Palazón et al. [68] employed magnetic nanomaterials composed of ferrite and MWCNTs in the DMSPE technique to effectively isolate capsaicin, dihydrocapsaicin, and N ‐vanillylnonanamide, demonstrating superior selectivity and sensitivity. Subsequent precise identification of capsaicinoids utilizing UHPLC‐QTOF‐MS technology and high‐resolution MS/MS (HRMS/MS) data, in combination with the proposed identification strategy, facilitated the discovery of novel or less studied capsaicinoid‐derived compounds.…”