In an attempt to improve the utility of RuAAC derivatization for specific, untargeted detection of internal alkynes, we carried out three separate leave-one-out mock derivatization reactions (no-catalyst, no-azide, and no-plant) in parallel with a fourth full RuAAC derivatization, and subsequently removed excess ruthenium catalyst from derivatized or mockderivatized reaction mixtures by DMSO treatment and filtration through silica gel. We carried out this analysis on a panel of commercially obtained plant materials, including fresh carrot leaf and root, fresh burdock root, safflower oil, and tarragon essential oil. Each of the mock-and RuAAC-derivatized samples were injected in triplicate.