Derivatization-targeted analysis of amino compounds in plant extracts in neutral loss acquisition mode by liquid chromatography-tandem mass spectrometry

Free Amino Acids and Biogenic Amines Profiling and Variation in Wild and Sub-Endemic Cardueae Species from Sardinia and Corse

“…macrocephalus , employed as a case study by [ 22 ], was here selected to perform all the extraction optimization experiments by applying a Design of Experiment (DoE) using the peak areas’ sum of the amino compounds as the output variable (response). As reported in [ 22 ], extraction with 0.1 M HCl in 30% methanol, ethanol or acetonitrile did not show any significant differences in the amino compound profile. The employment of other solvents, e.g., organic solvents without HCl, water or 0.1% formic acid, did not improve the selective extraction of these compounds (data not shown).…”

“…Nine additional compounds to those previously detected in C. nutans subsp . macrocephalus [ 22 ] were identified as a result of optimizing the extraction procedure and employing a slower gradient than previously used, thereby providing a better peak separation and allowing for the detection of more compounds. The newly identified compounds, which were reported for the first time in all the considered species, are taurine, histamine, glycine, glutamic acid, methylamine, ethylamine, dopamine, pyrrolidine and isopentylamine.…”

“…The supernatant was brought to a volume of 3 mL and filtered with a 25 mm diameter, 0.20 μm pore diameter hydrophilic regenerated cellulose syringe filter Chromafil ®® Xtra. An aliquote of the obtained extract was then derivatized following the procedure reported by [ 22 ].…”

“…In this contribution, we aimed at analyzing the extracts obtained from the five Cardueae species to elucidate their amino compounds profile and to improve the knowledge of these little-studied plants. For this purpose, a recently developed method for amino compounds detection, characterized by a prior derivatization step and a consequent analysis through high performance liquid chromatography coupled in tandem to a mass spectrometric detector (HPLC-MS/MS) was applied [ 22 ]. In this approach, which was called derivatization-targeted analysis, diethyl ethoxymethylenemalonate (DEEMM) was employed as the derivatization reagent, the reaction was quenched with hydroxylamine (NH 2 OH), and the analysis was carried out through HPLC-MS/MS in a neutral loss scan mode (NLS).…”

Determination of Biogenic Amines in Food and Beverage Samples

“…Najčastejšie využívané derivatizačné činidlá pri UV či fluorescenčnej detekcii sú o-ftaldialdehyd (OPA) 17,20 , 9-fluoroenylmetyloxykarbonyl chlorid (FMOC-Cl) 20 , dietyl-etoxymetylénmalonát (DEEMM) (cit. [21][22][23] ), dansyl chlorid (Dns-Cl) 15,20,24,25 , fenylizotiokyanát (PITC) 26,27 a 6-aminochinolyl-N-hydroxysukcinimidyl-karbamát (AQC) 9,28 .…”