Imperial College London

Emeritus ProfessorJeremyNicholson

Faculty of MedicineDepartment of Metabolism, Digestion and Reproduction

Emeritus Professor of Biological Chemistry
 
 
 
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Contact

 

+44 (0)20 7594 3195j.nicholson Website

 
 
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Assistant

 

Ms Wendy Torto +44 (0)20 7594 3225

 
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Location

 

Office no. 665Sir Alexander Fleming BuildingSouth Kensington Campus

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Summary

 

Publications

Citation

BibTex format

@article{Sen:2016:10.1016/j.chroma.2016.04.040,
author = {Sen, A and Knappy, C and Lewis, MR and Plumb, RS and Wilson, ID and Nicholson, JK and Smith, NW},
doi = {10.1016/j.chroma.2016.04.040},
journal = {Journal of Chromatography A},
pages = {141--155},
title = {Analysis of polar urinary metabolites for metabolic phenotyping using supercritical fluid chromatography and mass spectrometry},
url = {http://dx.doi.org/10.1016/j.chroma.2016.04.040},
volume = {1449},
year = {2016}
}

RIS format (EndNote, RefMan)

TY  - JOUR
AB - Supercritical fluid chromatography (SFC) is frequently used for the analysis and separation of non-polar metabolites, but remains relatively underutilised for the study of polar molecules, even those which pose difficulties with established reversed-phase (RP) or hydrophilic interaction liquid chromatographic (HILIC) methodologies. Here, we present a fast SFC-MS method for the analysis of medium and high-polarity (−7 ≤ cLogP ≤ 2) compounds, designed for implementation in a high-throughput metabonomics setting. Sixty polar analytes were first screened to identify those most suitable for inclusion in chromatographic test mixtures; then, a multi-dimensional method development study was conducted to determine the optimal choice of stationary phase, modifier additive and temperature for the separation of such analytes using SFC. The test mixtures were separated on a total of twelve different column chemistries at three different temperatures, using CO2-methanol-based mobile phases containing a variety of polar additives. Chromatographic performance was evaluated with a particular emphasis on peak capacity, overall resolution, peak distribution and repeatability. The results suggest that a new generation of stationary phases, specifically designed for improved robustness in mixed CO2-methanol mobile phases, can improve peak shape, peak capacity and resolution for all classes of polar analytes. A significant enhancement in chromatographic performance was observed for these urinary metabolites on the majority of the stationary phases when polar additives such as ammonium salts (formate, acetate and hydroxide) were included in the organic modifier, and the use of water or alkylamine additives was found to be beneficial for specific subsets of polar analytes. The utility of these findings was confirmed by the separation of a mixture of polar metabolites in human urine using an optimised 7 min gradient SFC method, where the use of the recommended column and co-solv
AU - Sen,A
AU - Knappy,C
AU - Lewis,MR
AU - Plumb,RS
AU - Wilson,ID
AU - Nicholson,JK
AU - Smith,NW
DO - 10.1016/j.chroma.2016.04.040
EP - 155
PY - 2016///
SN - 0412-3425
SP - 141
TI - Analysis of polar urinary metabolites for metabolic phenotyping using supercritical fluid chromatography and mass spectrometry
T2 - Journal of Chromatography A
UR - http://dx.doi.org/10.1016/j.chroma.2016.04.040
UR - http://hdl.handle.net/10044/1/34265
VL - 1449
ER -