MetaboLightsapplication/xmlftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204/m_MTBLS13204_LC-MS_positive_reverse-phase_metabolite_profiling_v2_maf.tsvftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204/m_MTBLS13204_LC-MS_negative_reverse-phase_metabolite_profiling_v2_maf.tsvftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204/a_MTBLS13204_LC-MS_positive_reverse-phase_metabolite_profiling.txtftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204/s_MTBLS13204.txtftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204/a_MTBLS13204_LC-MS_negative_reverse-phase_metabolite_profiling.txtftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204/i_Investigation.txtprimaryOK200ftp://ftp.ebi.ac.uk/pub/databases/metabolights/studies/public/MTBLS13204<p>Compound annotation in mzmine was performed against publicly available databases (https://systemsomicslab.github.io/compms/msdial/main.html MSP) and using SIRIUS+CSI:FingerID version 6.2.2 with the integrated tools of CSI:FingerID (with COSMIC), ZODIAC and CANOPUS/ClassyFire.</p>MetaboLightsPublicLiquid Chromatography MS - negative - reverse phaseLiquid Chromatography MS - positive - reverse phase<p>Chromatographic separation was performed with an Acquity HSS T3 column (1.7 µm, 100 x 2.1 mm, Waters Ltd., Elstree, U.K.). The column temperature was set to 40°C, and the samples were maintained at 18°C in the autosampler. The injected sample volume was 5 µL, and the eluent flow was set to 400 µL/min. The chromatographic system used a binary gradient of Solvent A (water with 0.1% formic acid) and Solvent B (acetonitrile with 0.1% formic acid). The gradient started at 5% of solvent B pre-equilibration for 0.1 minutes, followed by a linear increase to 100% B over 20 minutes. The gradient followed a 2-minute isocratic step at 100% solvent B. The gradient returned to 5% B followed by a post-equilibration period of the column for 3 min. The full chromatographic run was 25 minutes long.</p>Metabolomic insights into the phytochemical profiles and seasonal shifts of Fucus serratus and F. vesiculosus harvested in Danish coastal waters (Aarhus Bay) – an untargeted high-resolution mass-spectrometry approach.Aarhus University DenmarkMihai-Victor Curtasuthallusmass spectrometry<p>For untargeted metabolomics profiling, a sample preparation method was used based on methanol (100%) extraction. Firstly, 50 mg of seaweed material were weighed and added to 1.25 mL of methanol containing internal standards (IS) for LC-MS analyses (p-chlorophenylalanine and glychocholic acid (glycine-1-13C)), then mixed and sonicated for 15 min and vortexed for 1 h at room temperature. The supernatant (200 µL) was diluted with 0.1% formic acid in MILLIQ water 1:3 supernatant:water and centrifuged for 10 min at 4 °C at 29,700× g and transferred to an HPLC glass vial.</p>Fucus vesiculosusblankFucus serratusQuality Controlhttps://www.ebi.ac.uk/metabolights/MTBLS13204Mihai Curtasu. DK-8830 Tjele, Denmark. mihai.curtasu@anivet.au.dk.<p>Data acquisition was performed using LabSolutions software version 5.96 (Shimadzu Corporation, Kyoto, Japan). The collected raw spectra files were converted to mzML format and used for preprocessing in MZmine version 4.7.9 by mzio GmbH.</p>TreatmentTimemihai.curtasu@anivet.au.dk<p>Seaweed material, Fucus serratus (FS) and F. vesiculosus (FV), was manually harvested every month from 29.01.2023 to 13.12.2023 in Begtrup Vig (56°16'N 10°52'E), a small inlet within Aarhus Bay, Denmark. Five individual biological replicates of each species were collected in clear plastic bags, each containing a minimum of 50 g of wet biomass. The collected seaweeds were transported in thermocol boxes on the same day and stored at -20°C until processing for analysis. Before freeze-drying, the seaweed material was placed at −80 °C for 24 h. The freeze-dryer ScanVac CoolSafe (LaboGene A/S Lillerød, Denmark) operated at −40 °C for 72 h. After freeze-drying, the samples were placed into an exicator for 10 min before the final weighing. The freeze-dried material was then ground using a Retsch ZM200 Grinder - Gemini BV rotor grind mill and passed through a 0.5 mm particle size ring screen.</p>Metabolomicsultra-performance liquid chromatography-mass spectrometrySeaweedFucusuntargeted metabolitesultra-performance liquid chromatography-mass spectrometrySeaweedFucusuntargeted metabolites<p>Please update this protocol descriptionExtracts were analyzed by ultra-high pressure liquid chromatography (UHPLC) using a Nexera X2 liquid chromatography system and an LCMS-9030 quadrupole time-of-flight mass spectrometry (Q-TOF MS) system (Shimadzu Corporation, Kyoto, Japan) in positive and negative electrospray ionization (ESI+/ESI-) mode. Data collection was performed in MS1 mode covering 50-700 m/z range, and quality control (QC) samples were analyzed in data-dependent acquisition (DDA) mode covering 50-700 m/z range, where 10 dependent events (precursor ions) were selected continuously for fragmentation during the run. A precursor intensity threshold was set at 1800, and precursor ions were fragmented with 20 eV collision energy (CE) with a ±10 eV CE spread. The following MS parameters were used: ion-source temperature, 300°C; heated capillary temperature, 250°C; heat block temperature, 400°C; electrospray voltage 4.0 kV (ESI+) or -3.5 kV (ESI-); electrospray nebulization gas flow, 3 L/min; drying gas flow, 10 L/min; detector voltage, 2.02 kV and Ar was used as a collision gas for mass fragmentation. Mass calibration was performed externally using a sodium iodide solution (400 ppm in methanol) from m/z 50-1000.</p>Butyl (E)-3,6-dihydro-5-((methoxyimino)methyl)-1(2H)-pyridinecarboxylate5-(Ethyliminomethyl)-3',6'-dihydroxy-3-oxospiro[2-benzofuran-1,9'-xanthene]-4,6-dicarboxylic acidL-Phe4-(trimethylazaniumyl)butanoate1,3-diethyl 2,4-dioxocyclopentane-1,3-dicarboxylateGln-Gln9-hydroxy-7-(3-hydroxy-4-{[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy}phenyl)-2H,8H-[1,3]dioxolo[4,5-g]chromen-8-one2-[[5-Amino-2-[(2,5-diamino-5-oxopentanoyl)amino]-5-oxopentanoyl]amino]-3-phenylpropanoic acid[[(2S)-2-(gamma-Glutamylamino)-3-oxo-3-(carboxymethylamino)propyl]thio]radicalH-DL-xiThr-DL-Asn-DL-Glu-DL-His-OHN6^-[(1r)-2-[(1s)-1-Carboxy-2-(Methylsulfanyl)ethoxy]-2-Oxo-1-(Sulfanylmethyl)ethyl]-6-Oxo-L-Lysine2,5-Bis(3,4-diamino-1-methyl-1-oxidopyrrol-1-ium-2-yl)-1-methyl-1-oxidopyrrol-1-ium-3,4-diamineAlleAc-Gly-Gly-Asp-Pro-Gly-Gly-NH2Aconitic Acid14-oxa-7-azatetracyclo[6.6.1.0¹,¹¹.0²,⁷]pentadecan-13-one2-[(2S,3R,4S,5R,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyethyl 2-methylprop-2-enoate5-Amino-2-[2-(2-aminopropanoylamino)propanoylamino]-5-oxopentanoic acid2-[3-(Difluoromethyl)azetidin-1-yl]-2-methylpropanalL-TyrH-DL-Ala-DL-Ala-DL-Asn-DL-Asn-OH3-[2-(2-aminoethoxymethyl)-2-[[(3Z)-3-amino-3-hydroxyiminopropoxy]methyl]-3-hydroxypropoxy]-N'-hydroxypropanimidamideHydroxyoctadecadienylcarnitine3-(3-chlorophenyl)prop-2-enoic acid4-((2-Bromo-4,6-dinitrophenyl)azo)-N-(3-methoxypropyl)naphthalen-1-amine2-(2-amino-4-carbamoylbutanamido)-3-methylbutanoic acidMyocol3-(4-Azidophenyl)sulfanyl-3-(2,5-dihydroxypyrrol-1-yl)-3-sulfopropanoic acidMethyl 5,9-anhydro-2,4-dideoxy-D-glycero-D-gulo-dec-3-ulosonate2,3,4,5,6-pentahydroxyhexyl acetate5-Amino-2-[[2-[(2,5-diamino-5-oxopentanoyl)amino]-3-methylbutanoyl]amino]-5-oxopentanoic acid6-Amino-6-deoxy-chitosan[Ethyl(2-hydroxyethyl)amino]methanesulfonic acidGlu-OmeIsoorientin 2''-O-GallatePyroglutamylglutamineTrans-3-Indoleacrylic AcidL-Glu3-carbamoyl-2-[(5-oxopyrrolidin-2-yl)formamido]propanoic acidGuanine3,6,8-Trihydroxy-1-methyl-9,10-dioxo-7-[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]anthracene-2-carboxylic acid2-(2-chloro-4-nitrophenoxy)-N-(2,2,2-trifluoroethylcarbamoyl)acetamide2,5,8-Trioxa-11-azatridecan-13-oic acid2-[1-Hydroxybutan-2-yl(dimethoxy)silyl]butan-1-ol3,4,5-Trihydroxy-6-(6-methyl-2-oxochromen-7-yl)oxyoxane-2-carboxylic acid5-Isobenzofurancarboxylic acid, 1,3-dihydro-1,3-dioxo-, oxybis(methyleneoxymethylene) esterH-DL-Asn-DL-Asn-DL-xiIle-DL-Asn-OH[2-(4-Acetamidoanilino)-2-oxoethyl] 3-(4-acetamidophenyl)sulfonylpropanoate7-ChloroindolineDiamino 2-[[4-(3-aminooxy-2-aminooxycarbonyl-3-oxoprop-1-enyl)phenyl]methylidene]propanedioate1,3-dihydroxy-9-oxo-5-{[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy}-9H-xanthene-4-sulfonic acidN-Decyladenosine(3-Carboxy-2-hydroxypropyl)-tris(trideuteriomethyl)azaniumG-Ol2-[[5-Amino-2-[(2,5-diamino-5-oxopentanoyl)amino]-5-oxopentanoyl]amino]propanoic acid2-(1,2-dihydroxyethyl)oxolane-3,4-diol4-Amino-5-[[1-[(4-amino-1-carboxy-4-oxobutyl)amino]-1-oxopropan-2-yl]amino]-5-oxopentanoic acidN-{[4-hydroxy-5-(hydroxymethyl)-3-[4-(pyridin-2-yl)piperazin-1-yl]oxolan-2-yl]methyl}methanesulfonamide6-Amino-6-nitro-3-(2-phenylethenyl)cyclohexa-2,4-diene-1,2-disulfonic acid5-Amino-2-[[2-[(2,5-diamino-5-oxopentanoyl)amino]-4-methylpentanoyl]amino]-5-oxopentanoic acid2-[2-(2-Aminopropanoylamino)propanoylamino]pentanedioic acidH-DL-Asn-DL-Glu-DL-xiThr-DL-His-OHPidolic Acid2-(2-amino-4-carbamoylbutanamido)-3-phenylpropanoic acid2-EthylsulfanylpropanoatePado(2S,3R)-2-acetamido-N-[(2S)-5-(diaminomethylideneamino)-1-oxopentan-2-yl]-3-hydroxybutanamide(2-Acetyloxy-3-oxobutyl) acetate3-Oxoglutaric Acid(5S,7R)-3-hydroxyadamantane-1-carboxylateBenzyl bis(ethenyl) aminomethanetricarboxylateEthanol, 2,2'-(octylimino)bis-6-{[5,7-dihydroxy-2-(4-hydroxyphenyl)-4-oxo-4H-chromen-3-yl]oxy}-3,4-dihydroxy-5-(3,4,5-trihydroxybenzoyloxy)oxane-2-carboxylic acidCitrateN-[3-[1-(3,3-dimethylbutyl)-4-hydroxy-2-oxo-pyrrolo[1,2-b]pyridazin-3-yl]-1,1-dioxo-4H-1$l^{6},2,4-benzothiadiazin-7-yl]-N-methyl-methanesulfonamideN,N'-[(Methylimino)bisethylene]bis(carbamic acid 2-amino-2-hydroxyethyl) esterN-[3-[2-[2-(3-aminopropoxy)ethoxy]ethoxy]propyl]-2-(2-hydroxyethoxy)acetamideN-(5,6-Dimethoxy-4-pyrimidinyl)-4-(3,3-dimethyl-1-triazenyl)benzenesulfonamide4-carbamoyl-2-{4-carbamoyl-2-[(5-oxopyrrolidin-2-yl)formamido]butanamido}butanoic acid[2-Amino-4-[bis(prop-2-enyl)amino]-6-(dimethylamino)-1,3,5-triazin-1-ium-1-yl] hydrogen sulfateNiuhinone CBotryosphaerinoneN,N-bis(1-ethoxyethyl)-3-trimethoxysilylpropan-1-amine(13R)-5-[(3-chloro-4-fluorophenyl)methyl]-11-ethyl-8-hydroxy-N,13-dimethyl-6,10-dioxo-1,4,5,11-tetrazatricyclo[7.4.0.02,7]trideca-2(7),3,8-triene-3-carboxamidedimethyl (E)-2-(1,1-dioxo-1,2-benzothiazol-3-yl)but-2-enedioate(2S)-5-(diaminomethylideneamino)-2-[[(2S)-2-[[(2R)-3-hydroxy-2-(2-phenylethylsulfonylamino)propanoyl]amino]propanoyl]amino]pentanoic acidnyssoside. pteleoellagic acid glucoside.2-Azido-3,3,3-trifluoropropan-1-ol(5S)-5-ethenyl-1-phenylimidazolidine-2-thioneDiacetyl citral3'-Dehydrocarminate2-Nitrophenyl 4-O-beta-D-galactopyranosyl-beta-D-glucopyranoside2-{[2-(3,4-dihydroxyphenyl)-5,7-dihydroxy-4-oxo-4H-chromen-3-yl]oxy}-4,5-dihydroxy-6-(hydroxymethyl)oxan-3-yl 3,4-dihydroxybenzoate5-Amino-2-[[4-carboxy-2-[(2,5-diamino-5-oxopentanoyl)amino]butanoyl]amino]-5-oxopentanoic acidGlu-Glu-His-Thr1,4,7-Trioxacyclotridecane-8,13-dione3,5,6,8-tetrahydroxy-1-methyl-9,10-dioxo-7-{[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy}-9,10-dihydroanthracene-2-carboxylic acidmethyl 2-amino-3-(4-chlorophenyl)propanoateH-DL-xiThr-DL-Asp-DL-His-OHbeta-D-Tyvp-(1->3)-beta-D-GalpN6,OMe21,6-bis({[3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy})hexane-2,3,4,5-tetrolO-MethylperezoneEllagic Acid 4-O-α-L-3''-O-Acetylrhamnopyranosidena5-Amino-2-[[5-amino-2-[(2,5-diamino-5-oxopentanoyl)amino]-5-oxopentanoyl]amino]-5-oxopentanoic acid(2S,3R,4R,5S)-3-ethenoxy-6-(hydroxymethyl)oxane-2,4,5-triol4-[6-Amino-5-(3-hydroxypropoxyiminomethyl)pyrimidin-4-yl]piperazine-1-carboxylic acid[3-({5-[(dimethylarsoryl)methyl]-3,4-dihydroxyoxolan-2-yl}oxy)-2-hydroxypropoxy]sulfonic acid2-(3-Amino-3-Carboxypropyl)-L-Histidine2-amino-4-({1-[(carboxymethyl)carbamoyl]-2-{[3-(4-hydroxy-3,5-dimethoxyphenyl)prop-2-en-1-yl]sulfanyl}ethyl}carbamoyl)butanoic acid4-amino-5-[[(1R)-4-amino-1-carboxy-4-oxobutyl]amino]-5-oxopentanoic acid2-(2-Carbamoylhydrazinyl)-3,3,3-trifluoropropanoic acidMethyl NicotinateAdeninN-[2-(formamidomethyl)-2-(methylaminomethyl)-3-(2,3,4,5,6-pentahydroxyhexanoylamino)propyl]-2,3,4,5,6-pentahydroxyhexanamideEthanol, 2,2'-(decylimino)bis-Itoside L[3-({5-[(dimethylarsoryl)methyl]-3,4-dihydroxyoxolan-2-yl}oxy)-2-hydroxypropoxy]sulfinic acid2-hydroxy-2-(2-methoxy-2-oxoethyl)butanedioic acid1,1-Dimethylpyrrolidinium-2-carboxylate2-[(2,5-Diamino-5-oxopentanoyl)amino]-4-methylpentanoic acid5-Amino-2-[[2-[(2,5-diamino-5-oxopentanoyl)amino]-3-hydroxybutanoyl]amino]-5-oxopentanoic acid2-[(E)-2-[(E)-2-hydroxyethenoxy]ethenoxy]ethanol5,6,7,8-tetrahydroxy-2-(2,3,5-trihydroxy-4-methoxyphenyl)-3,4-dihydro-2H-1-benzopyran-4-oneGlucitol-lysine4-oxo-5-[(2S,3R,4R,5S,6R)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]pentanoic acid7,14-dimethoxy-3,10-dioxo-13-[(3,4,5-trihydroxyoxan-2-yl)oxy]-2,9-dioxatetracyclo[6.6.2.0⁴,¹⁶.0¹¹,¹⁵]hexadeca-1(14),4,6,8(16),11(15),12-hexaen-6-yl 3,4,5-trihydroxybenzoate2,3-dihydro-1H-indole6-O-methyl-d-glycero-alpha-l-gluco-heptopyranose2-Hydroxyethyl(3-sulfopropyl)azaniumH-DL-Ala-DL-Ala-DL-Gln-DL-Gln-OHGomphrenol 3-GlucosideMethanol, (((1-methyl-2-(5-methyl-3-oxazolidinyl)ethoxy)methoxy)methoxy)-(2R,4R)-1-[(2S)-5-[[Imino(nitroamino)methyl]amino]-2-[[(3-methyl-8-quinolinyl)sulfonyl]amino]-1-oxopentyl]-4-methyl-2-piperidinecarboxylic acid ethyl esterfalseMetabolomic insights into the phytochemical profiles and seasonal shifts of Fucus serratus and F. vesiculosus harvested in Danish coastal waters (Aarhus Bay) – an untargeted high-resolution mass-spectrometry approach<p>This study investigated the year-round metabolomic variation in Fucus serratus (FS) and F. vesiculosus (FV) collected monthly from Danish costal water around Aarhus Bay. Untargeted high-resolution liquid chromatography-mass spectrometry profiling (LC-HRMS), combined with multivariate data analysis and temporal clustering analysis, revealed that species identity was the primary driver of metabolic separation, followed by seasonal variation. FS showed higher levels of hydrolyzable tannins, flavonoid derivatives, aromatic amino acids, and glutamine-rich peptides, whereas FV was enriched in complex phlorotannins, tricarboxylic acid cycle intermediates, and carnitine derivatives. Temporal analysis identified recurring seasonal patterns across both species, including spring increases in amino acids, purine metabolites, and osmolytes; mid-summer peaks in mannitol and sulfated derivatives; and late-autumn elevations in phenolic compounds and betaine-type osmolytes. Despite apparent interspecific differences, several metabolite groups exhibited similar seasonal dynamics, suggesting shared physiological strategies associated with growth activation in spring, metabolic adjustment during summer to possible increased grazing pressure, and nutrient reallocation prior to winter. These findings provide a comprehensive, high-resolution view of seasonal metabolomic patterns in Fucus spp., offering new insights into their biochemical ecology and supporting the targeted utilization of these species for applications requiring specific metabolite profiles. Finally, this study contributes to the creation or expansion of metabolomic libraries for HRMS specific to Fucus seaweeds.</p>2025-10-232025-10-23MTBLS13204