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Open AccessArticle

Optimisation of Urine Sample Preparation for Headspace-Solid Phase Microextraction Gas Chromatography-Mass Spectrometry: Altering Sample pH, Sulphuric Acid Concentration and Phase Ratio

1
Department of Molecular and Clinical Cancer Medicine, Institute of Systems, Molecular and Integrative Biology, University of Liverpool, Liverpool L69 3BX, UK
2
School of Medicine, Cedar House, University of Liverpool, Liverpool L69 3GE, UK
3
Department of Molecular and Clinical Cancer Medicine, Institute of Systems, Molecular and Integrative Biology, Cancer Research Centre, University of Liverpool, Liverpool L3 9TA, UK
4
Palliative Care Institute Liverpool, Cancer Research Centre, University of Liverpool, Liverpool L3 9TA, UK
5
Clatterbridge Cancer Centre, Liverpool L7 8YA, UK
6
School of Medical Sciences, Bangor University, Bangor, Gwynedd LL57 2DG, UK
*
Author to whom correspondence should be addressed.
These authors contributed equally.
Metabolites 2020, 10(12), 482; https://doi.org/10.3390/metabo10120482
Received: 28 September 2020 / Revised: 17 November 2020 / Accepted: 17 November 2020 / Published: 25 November 2020
(This article belongs to the Section Metabolomic Profiling Technology)
Headspace-solid phase microextraction gas chromatography-mass spectrometry (HS-SPME-GC-MS) can be used to measure volatile organic compounds (VOCs) in human urine. However, there is no widely adopted standardised protocol for the preparation of urine samples for analysis resulting in an inability to compare studies reliably between laboratories. This paper investigated the effect of altering urine sample pH, volume, and vial size for optimising detection of VOCs when using HS-SPME-GC-MS. This is the first, direct comparison of H2SO4, HCl, and NaOH as treatment techniques prior to HS-SPME-GC-MS analysis. Altering urine sample pH indicates that H2SO4 is more effective at optimising detection of VOCs than HCl or NaOH. H2SO4 resulted in a significantly larger mean number of VOCs being identified per sample (on average, 33.5 VOCs to 24.3 in HCl or 12.2 in NaOH treated urine) and more unique VOCs, produced a more diverse range of classes of VOCs, and led to less HS-SPME-GC-MS degradation. We propose that adding 0.2 mL of 2.5 M H2SO4 to 1 mL of urine within a 10 mL headspace vial is the optimal sample preparation prior to HS-SPME-GC-MS analysis. We hope the use of our optimised method for urinary HS-SPME-GC-MS analysis will enhance our understanding of human disease and bolster metabolic biomarker identification. View Full-Text
Keywords: volatile organic compounds; VOCs; H2SO4; NaOH; HCl; sodium hydroxide; hydrochloric acid; HS-SPME-GC-MS; vials volatile organic compounds; VOCs; H2SO4; NaOH; HCl; sodium hydroxide; hydrochloric acid; HS-SPME-GC-MS; vials
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MDPI and ACS Style

Aggarwal, P.; Baker, J.; Boyd, M.T.; Coyle, S.; Probert, C.; Chapman, E.A. Optimisation of Urine Sample Preparation for Headspace-Solid Phase Microextraction Gas Chromatography-Mass Spectrometry: Altering Sample pH, Sulphuric Acid Concentration and Phase Ratio. Metabolites 2020, 10, 482. https://doi.org/10.3390/metabo10120482

AMA Style

Aggarwal P, Baker J, Boyd MT, Coyle S, Probert C, Chapman EA. Optimisation of Urine Sample Preparation for Headspace-Solid Phase Microextraction Gas Chromatography-Mass Spectrometry: Altering Sample pH, Sulphuric Acid Concentration and Phase Ratio. Metabolites. 2020; 10(12):482. https://doi.org/10.3390/metabo10120482

Chicago/Turabian Style

Aggarwal, Prashant; Baker, James; Boyd, Mark T.; Coyle, Séamus; Probert, Chris; Chapman, Elinor A. 2020. "Optimisation of Urine Sample Preparation for Headspace-Solid Phase Microextraction Gas Chromatography-Mass Spectrometry: Altering Sample pH, Sulphuric Acid Concentration and Phase Ratio" Metabolites 10, no. 12: 482. https://doi.org/10.3390/metabo10120482

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