Implementing the Use of Collision Cross Section Database for Phycotoxin Screening Analysis

The increased consumption of blue-green algae (BGA)-based dietary supplements has raised concern about their food safety, especially about cyanotoxin presence. The hyphenation of liquid chromatography with ion mobility mass spectrometry represents a relevant tool to screen several compounds in a large variety of food matrices. In this work, ultrahigh-performance liquid chromatography coupled to traveling wave ion mobility spectrometry/quadrupole time-of-flight mass spectrometry (UHPLC-TWIMS-QTOF) was employed to establish the first comprehensive TWIMS-derived collision cross section database (^TWCCS_N2) for phycotoxins. The database included 20 cyanotoxins and 1 marine toxin. Accurate m/z, retention times, and ^TWCCS_N2 values were obtained for 81 adducts in positive and negative electrospray (ESI⁺/ESI^-) modes. Reproducibility and robustness of the ^TWCCS_N2 measurements were determined to be independent of the matrix. A screening was carried out on 19 commercial BGA dietary supplements of different composition. Cyanotoxins were confidently identified in five samples based on retention time, m/z, and ^TWCCS_N2.