Summary of Study ST000786

This data is available at the NIH Common Fund's National Metabolomics Data Repository (NMDR) website, the Metabolomics Workbench,, where it has been assigned Project ID PR000572. The data can be accessed directly via it's Project DOI: 10.21228/M8QX13 This work is supported by NIH grant, U2C- DK119886.


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 IDST000786
Study TitleN-acetylisoputreanine-g-lactam Identification
Study SummaryAn untargeted metabolomics approach was utilized to determine urinary metabolites that could serve as small molecule biomarkers for treatment response to standard tuberculosis treatment. However, the majority of metabolites that most accurately distinguished patient samples at time of diagnosis from those at one month after the start of therapy lacked structural identification. The detection of unknown metabolite structures is a well-known limitation of untargeted metabolomics, and underscores a need for continued elucidation of novel metabolite structures. In this study, we sought to define the structure of a urine metabolite with an experimentally determined mass of 202.1326 Da, classified as molecular feature (MF) 202.1326. A hypothesized structure of N1-acetylisoputreanine was developed for MF 202.1326 using in silico tools and liquid chromatography-tandem mass spectrometry (LC-MS/MS). In the absence of a commercial standard, synthetic N1-acetylisoputreanine was generated using enzymatic and chemical synthesis and LC-MS/MS was used to confirm the structure of MF 202.1326 as N1-acetylisoputreanine, a proposed terminal polyamine catabolite that had not been previously detected in biological samples. Further analysis demonstrated that N1-acetylisoputreanine and an alternative form of this metabolite, N1-acetylisoputreanine-γ-lactam, are both present in human urine and are likely end-products of polyamine metabolism.
Colorado State University
Last NameFitzgerald
First NameBryna
Address3185 Rampart Rd
Submit Date2017-06-26
Raw Data AvailableYes
Raw Data File Type(s)d
Analysis Type DetailLC-MS
Release Date2017-10-11
Release Version1
Bryna Fitzgerald Bryna Fitzgerald application/zip

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Project ID:PR000572
Project DOI:doi: 10.21228/M8QX13
Project Title:Urine Metabolite Identification
Project Type:MS and MS/MS analyses
Project Summary:Structural identification of unknown metabolites in human urine
Institute:Colorado State University
Department:Department of Microbiology, Immunology, and Pathology
Last Name:Fitzgerald
First Name:Bryna
Address:3185 Rampart Rd, Fort Collins, CO, 80521, USA


Subject ID:SU000811
Subject Type:Human
Subject Species:Homo sapiens
Taxonomy ID:9606
Species Group:Human


Subject type: Human; Subject species: Homo sapiens (Factor headings shown in green)

mb_sample_id local_sample_id Treatment
Showing results 1 to 5 of 5


Collection ID:CO000805
Collection Summary:Urine was collected and frozen at -20 for storage. Prior to analysis, urine was thawed and centrifuged to remove particulates. Synthetic NACIP-gl material was stored in water at 4 and diluted in water prior to analysis.
Sample Type:Urine


Treatment ID:TR000825
Treatment Summary:Urine, urine spiked with synthetic standard, and synthetic standard alone were analyzed by LC-MS and LC-MS/MS

Sample Preparation:

Sampleprep ID:SP000818
Sampleprep Summary:Urine was thawed on ice and centrifuged to remove particulates prior to analysis. N1-acetylisoputreanine-γ-lactam was synthesized as previously described. Acetylation was performed with N-(3-Aminopropyl) pyrrolidin-2-one (0.75 M) and acetyl chloride (0.75 M) in methanol and 0.5 M PBS (1:1) adjusted to pH 7.0 with sodium hydroxide. The reaction products were extracted with dichloromethane, dried, suspended in 2 ml LC-MS grade water and stored at 4˚C. Prior to LC-MS analyses, the synthetic compound was diluted 1:100 in water or human urine.

Combined analysis:

Analysis ID AN001245
Analysis type MS
Chromatography type Reversed phase
Chromatography system Agilent 1200
Column Atlantis T3 reverse-phase C18 (150 x 2.1mm,3.5um)
MS instrument type QTOF
MS instrument name Agilent
Units counts*min


Chromatography ID:CH000869
Instrument Name:Agilent 1200
Column Name:Atlantis T3 reverse-phase C18 (150 x 2.1mm,3.5um)
Column Temperature:30
Flow Gradient:100% Solvent A to 90% Solvent B
Flow Rate:0.25 ml/min
Solvent A:100% water; 0.1% formic acid
Solvent B:100% methanol; 0.1% formic acid
Chromatography Type:Reversed phase


MS ID:MS001138
Analysis ID:AN001245
Instrument Name:Agilent
Instrument Type:QTOF