Summary of Study ST002292

This data is available at the NIH Common Fund's National Metabolomics Data Repository (NMDR) website, the Metabolomics Workbench, https://www.metabolomicsworkbench.org, where it has been assigned Project ID PR001470. The data can be accessed directly via it's Project DOI: 10.21228/M8Q99X This work is supported by NIH grant, U2C- DK119886.

See: https://www.metabolomicsworkbench.org/about/howtocite.php

This study contains a large results data set and is not available in the mwTab file. It is only available for download via FTP as data file(s) here.

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Study IDST002292
Study TitleQuantification of Dissolved Metabolites in Environmental Samples through Cation-Exchange Solid Phase Extraction (CX-SPE) paired with Liquid Chromatography-Mass Spectrometry
Study TypeMethod Development for Dissolved Metabolomics in Seawater
Study SummarySmall, biologically produced, organic molecules called metabolites play key roles in microbial systems where they directly mediate exchanges of nutrients, energy, and information. However, the study of dissolved polar metabolites in seawater and other environmental matrices has been hampered by analytical challenges including high inorganic ion concentrations, low analyte concentrations, and high chemical diversity. Here we show that a cation-exchange solid phase extraction (CX-SPE) sample preparation approach separates positively charged and zwitterionic metabolites from seawater and freshwater samples, allowing their analysis by liquid chromatography-mass spectrometry (LC-MS). We successfully extracted 69 known compounds from an in-house compound collection and evaluated the performance of the method by establishing extraction efficiencies and limits of detection (pM to low nM range) for these compounds. CX-SPE extracted a range of compounds including amino acids and compatible solutes, resulted in very low matrix effects, and performed robustly across large variations in salinity and dissolved organic matter (DOM) concentration. We compared CX-SPE to an established solid phase extraction procedure (PPL-SPE) and demonstrate that these two methods extract fundamentally different fractions of the dissolved metabolite pool with CX-SPE extracting compounds that are on average smaller and more polar. We use CX-SPE to analyze four environmental samples from distinct aquatic biomes, producing some of the first CX-SPE dissolved metabolomes. Quantified compounds ranged in concentration from 0.0093 nM to 49 nM and were composed primarily of amino acids (0.15 – 16 nM) and compatible solutes such as TMAO (0.89 – 49 nM) and glycine betaine (2.8 – 5.2 nM).
Institute
University of Washington
DepartmentOceanography
LaboratoryIngalls Lab
Last NameSacks
First NameJoshua
AddressOcean Sciences Building, 1492 NE Boat St. Seattle, WA 98105
Emailjssacks@uw.edu
Phone4074090052
Submit Date2022-08-30
Raw Data AvailableYes
Raw Data File Type(s)mzML
Analysis Type DetailLC-MS
Release Date2022-10-19
Release Version1
Joshua Sacks Joshua Sacks
https://dx.doi.org/10.21228/M8Q99X
ftp://www.metabolomicsworkbench.org/Studies/ application/zip

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Combined analysis:

Analysis ID AN003744 AN003745 AN003746
Analysis type MS MS MS
Chromatography type HILIC HILIC Reversed phase
Chromatography system Waters Acquity I-Class Waters Acquity I-Class Waters Acquity I-Class
Column SeQuant ZIC-pHILIC (150 x 2.1mm,5um) SeQuant ZIC-pHILIC (150 x 2.1mm,5um) Waters Acquity HSS Cyano (1.8um,2.1 mm x 100 mm)
MS Type ESI ESI ESI
MS instrument type Orbitrap Orbitrap Orbitrap
MS instrument name Thermo Q Exactive HF hybrid Orbitrap Thermo Q Exactive HF hybrid Orbitrap Thermo Q Exactive HF hybrid Orbitrap
Ion Mode POSITIVE NEGATIVE POSITIVE
Units Peak Area Peak Area Peak Area

MS:

MS ID:MS003491
Analysis ID:AN003744
Instrument Name:Thermo Q Exactive HF hybrid Orbitrap
Instrument Type:Orbitrap
MS Type:ESI
MS Comments:See Protocol
Ion Mode:POSITIVE
Analysis Protocol File:CXSPE_Method_Paper_MS_Methods.txt
  
MS ID:MS003492
Analysis ID:AN003745
Instrument Name:Thermo Q Exactive HF hybrid Orbitrap
Instrument Type:Orbitrap
MS Type:ESI
MS Comments:See Protocol
Ion Mode:NEGATIVE
Analysis Protocol File:CXSPE_Method_Paper_MS_Methods.txt
  
MS ID:MS003493
Analysis ID:AN003746
Instrument Name:Thermo Q Exactive HF hybrid Orbitrap
Instrument Type:Orbitrap
MS Type:ESI
MS Comments:See Protocol
Ion Mode:POSITIVE
Analysis Protocol File:CXSPE_Method_Paper_MS_Methods.txt
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