#METABOLOMICS WORKBENCH lerland_20191220_161535 DATATRACK_ID:1881 STUDY_ID:ST001296 ANALYSIS_ID:AN002157 VERSION 1 CREATED_ON 03-03-2022 #PROJECT PR:PROJECT_TITLE Metabolomics and Hormonomics to Crack the Code of Filbert Growth PR:PROJECT_TYPE Plant Untargeted MS Metabolomics PR:PROJECT_SUMMARY Introduction: Plants respond to changes in their environments through hormonal PR:PROJECT_SUMMARY activation of a physiological cascade that redirects metabolic resources and PR:PROJECT_SUMMARY growth. In filberts (Corylus sp.), chelated iron promotes the growth of new PR:PROJECT_SUMMARY shoots but the mechanism(s) are not understood. Objectives: To use untargeted PR:PROJECT_SUMMARY metabolomics and hormonomics approaches to generate novel hypotheses for the PR:PROJECT_SUMMARY morphoregulatory role of ferric ethylenediamine-N,N'-di-(ortho-hydroxyphenyl) PR:PROJECT_SUMMARY acetic acid (Fe-EDDHA) in filbert shoot organogenesis in vitro. Methods: Data PR:PROJECT_SUMMARY were generated using previously optimized standardized untargeted metabolomics PR:PROJECT_SUMMARY protocols with time of flight mass spectrometry. Multivariate statistical tools PR:PROJECT_SUMMARY (principal component and partial least squares discriminant analysis) did not PR:PROJECT_SUMMARY detect significant differences. Discovery tools Significance Analysis of PR:PROJECT_SUMMARY Microarrays (SAM), multiple linear regression analysis, Bayesian analysis, PR:PROJECT_SUMMARY logical algorithms, machine learning, synthetic biotransformations, targeted PR:PROJECT_SUMMARY hormonomics, and online resources including MetaboAnalyst were used. Results: PR:PROJECT_SUMMARY Starch/sucrose metabolism and shikimate pathway metabolites were increased. Dose PR:PROJECT_SUMMARY dependent decreases were found in polyphenol metabolism, specifically ellagic PR:PROJECT_SUMMARY acid and its methylated derivative 3,4,3'-tri-O-methylellagic acid. Hormonomics PR:PROJECT_SUMMARY analysis revealed significant differences in phytohormones and their conjugates. PR:PROJECT_SUMMARY FeEDDHA treatment reduced indole-3-acetic acid, abscisic acid, salicylic acid, PR:PROJECT_SUMMARY jasmonic acid conjugates (JA-Trp, JA-Ile, OH-JA) and dihydrozeatinglucoside in PR:PROJECT_SUMMARY regenerating explants. Serotonin (5HT) was decreased in FeEDDHA-treated PR:PROJECT_SUMMARY regenerating tissues while the related metabolite melatonin was increased. Eight PR:PROJECT_SUMMARY phenolic conjugates of 5HT and eight catabolites were affected by FeEDDHA PR:PROJECT_SUMMARY indicating that metabolism to sequester, deactivate and metabolize 5HT was PR:PROJECT_SUMMARY induced by Fe(III). Tryptophan was metabolized through kynurenine but not PR:PROJECT_SUMMARY anthranilate. Conclusion: Seven novel hypotheses were generated to guide future PR:PROJECT_SUMMARY studies to understand the regulatory control(s) of shoot organogenesis. PR:INSTITUTE University of British Columbia PR:DEPARTMENT Chemistry PR:LABORATORY PlantSMART PR:LAST_NAME Murch PR:FIRST_NAME Susan PR:ADDRESS 3247 University Way PR:EMAIL susan.murch@ubc.ca PR:PHONE 250-807-9566 PR:DOI http://dx.doi.org/10.21228/M8B382 PR:CONTRIBUTORS Lauren A E Erland, Christina E Turi, Praveen K Saxena, Susan J Murch #STUDY ST:STUDY_TITLE Metabolomics and Hormonomics to Crack the Code of Filbert Growth ST:STUDY_SUMMARY Introduction: Plants respond to changes in their environments through hormonal ST:STUDY_SUMMARY activation of a physiological cascade that redirects metabolic resources and ST:STUDY_SUMMARY growth. In filberts (Corylus sp.), chelated iron promotes the growth of new ST:STUDY_SUMMARY shoots but the mechanism(s) are not understood. Objectives: To use untargeted ST:STUDY_SUMMARY metabolomics and hormonomics approaches to generate novel hypotheses for the ST:STUDY_SUMMARY morphoregulatory role of ferric ethylenediamine-N,N'-di-(ortho-hydroxyphenyl) ST:STUDY_SUMMARY acetic acid (Fe-EDDHA) in filbert shoot organogenesis in vitro. Methods: Data ST:STUDY_SUMMARY were generated using previously optimized standardized untargeted metabolomics ST:STUDY_SUMMARY protocols with time of flight mass spectrometry. Multivariate statistical tools ST:STUDY_SUMMARY (principal component and partial least squares discriminant analysis) did not ST:STUDY_SUMMARY detect significant differences. Discovery tools Significance Analysis of ST:STUDY_SUMMARY Microarrays (SAM), multiple linear regression analysis, Bayesian analysis, ST:STUDY_SUMMARY logical algorithms, machine learning, synthetic biotransformations, targeted ST:STUDY_SUMMARY hormonomics, and online resources including MetaboAnalyst were used. Results: ST:STUDY_SUMMARY Starch/sucrose metabolism and shikimate pathway metabolites were increased. Dose ST:STUDY_SUMMARY dependent decreases were found in polyphenol metabolism, specifically ellagic ST:STUDY_SUMMARY acid and its methylated derivative 3,4,3'-tri-O-methylellagic acid. Hormonomics ST:STUDY_SUMMARY analysis revealed significant differences in phytohormones and their conjugates. ST:STUDY_SUMMARY FeEDDHA treatment reduced indole-3-acetic acid, abscisic acid, salicylic acid, ST:STUDY_SUMMARY jasmonic acid conjugates (JA-Trp, JA-Ile, OH-JA) and dihydrozeatinglucoside in ST:STUDY_SUMMARY regenerating explants. Serotonin (5HT) was decreased in FeEDDHA-treated ST:STUDY_SUMMARY regenerating tissues while the related metabolite melatonin was increased. Eight ST:STUDY_SUMMARY phenolic conjugates of 5HT and eight catabolites were affected by FeEDDHA ST:STUDY_SUMMARY indicating that metabolism to sequester, deactivate and metabolize 5HT was ST:STUDY_SUMMARY induced by Fe(III). Tryptophan was metabolized through kynurenine but not ST:STUDY_SUMMARY anthranilate. Conclusion: Seven novel hypotheses were generated to guide future ST:STUDY_SUMMARY studies to understand the regulatory control(s) of shoot organogenesis. ST:INSTITUTE University of British Columbia ST:DEPARTMENT Chemistry ST:LABORATORY PlantSMART ST:LAST_NAME Murch ST:FIRST_NAME Susan ST:ADDRESS 3247 University Way ST:EMAIL susan.murch@ubc.ca ST:PHONE 250-807-9566 ST:SUBMIT_DATE 2019-12-20 #SUBJECT SU:SUBJECT_TYPE Plant SU:SUBJECT_SPECIES Corylus avellana;Corylus americana SU:TAXONOMY_ID 13451;78632 SU:GENOTYPE_STRAIN Corylus avellana;Corylus americana(cv Geneva) #SUBJECT_SAMPLE_FACTORS: SUBJECT(optional)[tab]SAMPLE[tab]FACTORS(NAME:VALUE pairs separated by |)[tab]Additional sample data SUBJECT_SAMPLE_FACTORS - 10_18_2011 M1A FeEDDHA (µM):- RAW_FILE_NAME=10_18_2011 M1A.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M1B FeEDDHA (µM):- RAW_FILE_NAME=10_18_2011 M1B.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M1C FeEDDHA (µM):- RAW_FILE_NAME=10_18_2011 M1C.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M2A FeEDDHA (µM):230 RAW_FILE_NAME=10_18_2011 M2A.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M2B FeEDDHA (µM):230 RAW_FILE_NAME=10_18_2011 M2B.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M2C FeEDDHA (µM):230 RAW_FILE_NAME=10_18_2011 M2C.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M3A FeEDDHA (µM):460 RAW_FILE_NAME=10_18_2011 M3A.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M3B FeEDDHA (µM):460 RAW_FILE_NAME=10_18_2011 M3B.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M3C FeEDDHA (µM):460 RAW_FILE_NAME=10_18_2011 M3C.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M4A FeEDDHA (µM):690 RAW_FILE_NAME=10_18_2011 M4A.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M4B FeEDDHA (µM):690 RAW_FILE_NAME=10_18_2011 M4B.raw SUBJECT_SAMPLE_FACTORS - 10_18_2011 M4C FeEDDHA (µM):690 RAW_FILE_NAME=10_18_2011 M4C.raw #COLLECTION CO:COLLECTION_SUMMARY Cultures were sampled in triplicate on day 35 of the culture period, CO:SAMPLE_TYPE Plant #TREATMENT TR:TREATMENT_SUMMARY Filbert (C. avellana L. × C. americana Marshall cv. Geneva; Grimo Nut Nursery, TR:TREATMENT_SUMMARY Niagara-on-the-Lake, ON, Canada) shoot cultures were provided from germplasm TR:TREATMENT_SUMMARY maintained at the Gosling Research Institute for Plant Preservation (GRIPP; TR:TREATMENT_SUMMARY University of Guelph, Guelph, ON). Plantlets were grown in GA-7 vessels TR:TREATMENT_SUMMARY according to methods previously described (Garrison et al. 2013; Latawa et al. TR:TREATMENT_SUMMARY 2016). In brief, cultures were grown on semi-solid modified NCGR-COR medium (Yu TR:TREATMENT_SUMMARY and Reed 1995) supplemented with 10 g L-1 myo-inositol, 200 mg L-1 glycine, 100 TR:TREATMENT_SUMMARY mg L-1 nicotinic acid, 100 mg L-1 thiamine (PhytoTechnology Laboratories), 17.6 TR:TREATMENT_SUMMARY µM benzylaminopurine (BAP; Sigma-Aldrich), 0.014 µM indole-3-butyric acid TR:TREATMENT_SUMMARY (IBA; Sigma-Aldrich), 0.29 µM gibberellic acid (GA3; PhytoTechnology TR:TREATMENT_SUMMARY Laboratories), and 30 g L-1 glucose with 0, 230, 460 and 690 µM Fe-EDDHA TR:TREATMENT_SUMMARY (Sigma, St. Louis, MO) and the pH of the medium was adjusted to 5.7 before TR:TREATMENT_SUMMARY autoclaving at 121 ºC for 20 min. Cultures were maintained in a growth room at TR:TREATMENT_SUMMARY 23 ± 2oC with a 16 h photoperiod of 40 µmol m-2 s-1 provided by cool-white TR:TREATMENT_SUMMARY fluorescent lamps (Osram Sylvania Ltd., Mississauga, ON, Canada). #SAMPLEPREP SP:SAMPLEPREP_SUMMARY Cultures were sampled in triplicate on day 35 of the culture period, accurately SP:SAMPLEPREP_SUMMARY weighed (50 mg), and homogenized in 1 mL of 70% ethanol for 30 s (Kontes Pellet SP:SAMPLEPREP_SUMMARY Pestle, Fisher Scientific). Samples were centrifuged (16,000 x g) for 3 min to SP:SAMPLEPREP_SUMMARY settle particulate matter and the supernatant was filtered (0.1 µm, SP:SAMPLEPREP_SUMMARY Ultrafree-MC filtered centrifuge tubes; Millipore, MS, USA) prior to SP:SAMPLEPREP_SUMMARY chromatography. #CHROMATOGRAPHY CH:CHROMATOGRAPHY_SUMMARY Extracts and 70% ethanol blanks (n=3 for each treatment) were separated using a CH:CHROMATOGRAPHY_SUMMARY Waters BEH Acquity C18 (2.1 X 150 mm, 1.7 µm) column with the following CH:CHROMATOGRAPHY_SUMMARY gradient: 0.1% aqueous formic acid:acetonitrile (0.0-25 min, 95:5-5:95 v/v, CH:CHROMATOGRAPHY_SUMMARY 25.01-30.0 min, 95:5 v/v). The flow rate was set to 0.25 mL min-1 for 30 mins at CH:CHROMATOGRAPHY_SUMMARY 30 ◦C (Waters Acquity UPLC). CH:INSTRUMENT_NAME Waters Acquity CH:COLUMN_NAME Waters BEH Acquity C18 (2.1 X 150 mm, 1.7 um) CH:COLUMN_TEMPERATURE 30 CH:FLOW_GRADIENT 0.0 - 10.0 min, : 95:5-5:95 v/v, 10.0-15.0 min, 5:95 v/v, 15.0-20.0min, CH:FLOW_GRADIENT 5:95-95:5 v/v, 20.0-25.0min, 95:5 v/v) CH:FLOW_RATE 0.25 ml/min CH:SOLVENT_A 1% aqueous formic acid CH:SOLVENT_B acetonitrile CH:CHROMATOGRAPHY_TYPE Reversed phase #ANALYSIS AN:ANALYSIS_TYPE MS #MS MS:INSTRUMENT_NAME Waters Micromass QTOF Premier MS:INSTRUMENT_TYPE QTOF MS:MS_TYPE ESI MS:MS_COMMENTS A steady flow of leucine enkephalin (Waters 1525 HPLC binary solvent manager, 2 MS:MS_COMMENTS ng mL-1) was used as the internal standard for calibration of the Micromass LCT MS:MS_COMMENTS Premier series ToF-MS (Waters Inc.). Time of flight mass spectrometry was used MS:MS_COMMENTS with previously published optimized conditions (Brown, Murch, et al. 2012; Brown MS:MS_COMMENTS et al. 2012) including: electrospray ionization and positive ion detection in W MS:MS_COMMENTS mode, mass range of 100-1000 amu and a scan time of 0.1s. Data were collected MS:MS_COMMENTS with MassLynx V4.1 and exported via MarkerLynx. Data were processed in Excel™ MS:MS_COMMENTS to align retention times and remove multiply charged ions as described MS:MS_COMMENTS previously (Brown et al. 2012; Brown et al. 2012; Turi and Murch 2013; Turi et MS:MS_COMMENTS al. 2014). MS:ION_MODE POSITIVE MS:MS_RESULTS_FILE ST001296_AN002157_Results.txt UNITS:Peak Intensity Has m/z:Yes Has RT:Yes RT units:Minutes #END