Reverse-phase/phenylboronic-acid-type magnetic microspheres to eliminate the matrix effects in amatoxin and phallotoxin determination via ultrahigh-performance liquid chromatography–tandem mass spectrometry

Abstract In this study, we present the preparation of a new reverse-phase/phenylboronic-acid (RP/PBA)-type mixed-mode magnetic solid-phase extraction (MSPE) adsorbent for use in the cleanup of amatoxin- and phallotoxin-containing samples intended for ultrahigh-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) analysis. Further, the RP/PBA magnetic microspheres have phenyl and phenylboronic acid groups on their surfaces that selectively adsorb amatoxins and phallotoxins through hydrophobic, π–π, and boronate affinity, significantly reducing matrix effects in UPLC–MS/MS analysis. After systematic optimization, all the standard calibration curves expressed satisfactory linearity (r > 0.9930), limits of detection (0.3 μg/kg), and recovery (97.6%–114.2%). Compared with other reported methods, this method also has the advantages of simple, fast, and efficient operation using relatively small amounts of the MSPE adsorbent. Furthermore, the method was successfully applied in a poisoning incident caused by Lepiota brunneoincarnata Chodat & C. Martin ingestion.