Production of Amphidinols and Other Bioproducts of Interest by the Marine Microalga Amphidinium carterae Unraveled by Nuclear Magnetic Resonance Metabolomics Approach Coupled to Multivariate Data Analysis Ana Cristina Abreu Alejandro Molina-Miras Luis M. Aguilera-Sáez Lorenzo López-Rosales María del Carmen Cerón-García Asterio Sánchez-Mirón Lucía Olmo-García Alegría Carrasco-Pancorbo Francisco García-Camacho Emilio Molina-Grima Ignacio Fernández 10.1021/acs.jafc.9b02821.s001 https://acs.figshare.com/articles/journal_contribution/Production_of_Amphidinols_and_Other_Bioproducts_of_Interest_by_the_Marine_Microalga_Amphidinium_carterae_Unraveled_by_Nuclear_Magnetic_Resonance_Metabolomics_Approach_Coupled_to_Multivariate_Data_Analysis/9636644 This study assessed the feasibility of an NMR metabolomics approach coupled to multivariate data analysis to monitor the naturally present or stresses-elicited metabolites from a long-term (>170 days) culture of the dinoflagellate marine microalgae Amphidinium carterae grown in a fiberglass paddlewheel-driven raceway photobioreactor. Metabolic contents, in particular, in two members of the amphidinol family, amphidinol A and its 7-sulfate derivative amphidinol B (referred as APDs), and other compounds of interest (fatty acids, carotenoids, oxylipins, etc.) were evaluated by altering concentration levels of the f/2 medium nutrients and daily mean irradiance. Operating with a 24 h sinusoidal light cycle allowed a 3-fold increase in APD production, which was also detected by an increase in hemolytic activity of the methanolic extract of A. carterae biomass. The presence of APDs was consistent with the antitumoral activity measured in the methanolic extracts of the biomass. Increased daily irradiance was accompanied by a general decrease in pigments and an increase in SFAs (saturated fatty acids), MUFAs (monounsaturated fatty acids), and DHA (docosahexaenoic acid), while increased nutrient availability lead to an increase in sugar, amino acid, and PUFA ω-3 contents and pigments and a decrease in SFAs and MUFAs. NMR-based metabolomics is shown to be a fast and suitable method to accompany the production of APD and bioactive compounds without the need of tedious isolation methods and bioassays. The two APD compounds were chemically identified by spectroscopic NMR and spectrometric ESI-IT MS (electrospray ionization ion trap mass spectrometry) and ESI-TOF MS (ESI time-of-flight mass spectrometry) methods. 2019-08-15 18:06:58 irradiance ESI-IT MS carterae biomass APD compounds Marine Microalga Amphidinium carterae Unraveled pigment stresses-elicited metabolites concentration levels light cycle dinoflagellate marine microalgae Amphidinium carterae acid amphidinol family PUFA ω-3 contents ESI time-of-flight mass spectrometry Other Bioproducts SFA antitumoral activity isolation methods methanolic extracts spectroscopic NMR 7- sulfate ESI-TOF MS MUFA multivariate data analysis NMR metabolomics approach electrospray ionization ion trap mass spectrometry fiberglass paddlewheel-driven raceway photobioreactor bioactive compounds 24 h NMR-based metabolomics DHA amphidinol B Resonance Metabolomics Approach APD production Multivariate Data Analysis Metabolic contents