Extraction and quantitative determination of bile acids in feces

With rapid advances in gut microbiome research, fecal bile acids are increasingly being monitored as potential biomarkers of diet related disease susceptibility. As such, rapid, robust and reliable methods for their analysis are of increasing importance. Herein is described a simple extraction metho...

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Main Authors: Shafaei, A., Rees, J., Christophersen, Claus, Devine, A., Broadhurst, D., Boyce, M.C.
Format: Journal Article
Language:English
Published: ELSEVIER 2021
Subjects:
Online Access:http://hdl.handle.net/20.500.11937/86513
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author Shafaei, A.
Rees, J.
Christophersen, Claus
Devine, A.
Broadhurst, D.
Boyce, M.C.
author_facet Shafaei, A.
Rees, J.
Christophersen, Claus
Devine, A.
Broadhurst, D.
Boyce, M.C.
author_sort Shafaei, A.
building Curtin Institutional Repository
collection Online Access
description With rapid advances in gut microbiome research, fecal bile acids are increasingly being monitored as potential biomarkers of diet related disease susceptibility. As such, rapid, robust and reliable methods for their analysis are of increasing importance. Herein is described a simple extraction method for the analysis of bile acids in feces suitable for subsequent quantification by liquid chromatography and tandem mass spectrometry. A C18 column separated the analytes with excellent peak shape and retention time repeatability maintained across 800 injections. The intra-day and inter-day precision and accuracy was greater than 80%. Recoveries ranged from 83.58 to 122.41%. The limit of detection and limit of quantification were in the range 2.5–15 nM, respectively. The optimized method involved extracting bile acids from wet feces with minimal clean up. A second aliquot of fecal material was dried and weighed to correct for water content. Extracting from dried feces showed reduced recovery that could be corrected for by spiking the feces with deuterated standards prior to drying. Storage of the extracts and standards in a refrigerated autosampler prior to analysis on the LC-MS is necessary. Multiple freeze-thaws of both extracts and standards lead to poor recoveries for some bile acids. The method was successfully applied to 100 human fecal samples.
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spelling curtin-20.500.11937-865132021-11-29T06:42:44Z Extraction and quantitative determination of bile acids in feces Shafaei, A. Rees, J. Christophersen, Claus Devine, A. Broadhurst, D. Boyce, M.C. Science & Technology Physical Sciences Chemistry, Analytical Chemistry Bile acids Fecal LC-MS MS Extraction Stability With rapid advances in gut microbiome research, fecal bile acids are increasingly being monitored as potential biomarkers of diet related disease susceptibility. As such, rapid, robust and reliable methods for their analysis are of increasing importance. Herein is described a simple extraction method for the analysis of bile acids in feces suitable for subsequent quantification by liquid chromatography and tandem mass spectrometry. A C18 column separated the analytes with excellent peak shape and retention time repeatability maintained across 800 injections. The intra-day and inter-day precision and accuracy was greater than 80%. Recoveries ranged from 83.58 to 122.41%. The limit of detection and limit of quantification were in the range 2.5–15 nM, respectively. The optimized method involved extracting bile acids from wet feces with minimal clean up. A second aliquot of fecal material was dried and weighed to correct for water content. Extracting from dried feces showed reduced recovery that could be corrected for by spiking the feces with deuterated standards prior to drying. Storage of the extracts and standards in a refrigerated autosampler prior to analysis on the LC-MS is necessary. Multiple freeze-thaws of both extracts and standards lead to poor recoveries for some bile acids. The method was successfully applied to 100 human fecal samples. 2021 Journal Article http://hdl.handle.net/20.500.11937/86513 10.1016/j.aca.2021.338224 English ELSEVIER restricted
spellingShingle Science & Technology
Physical Sciences
Chemistry, Analytical
Chemistry
Bile acids
Fecal
LC-MS
MS
Extraction
Stability
Shafaei, A.
Rees, J.
Christophersen, Claus
Devine, A.
Broadhurst, D.
Boyce, M.C.
Extraction and quantitative determination of bile acids in feces
title Extraction and quantitative determination of bile acids in feces
title_full Extraction and quantitative determination of bile acids in feces
title_fullStr Extraction and quantitative determination of bile acids in feces
title_full_unstemmed Extraction and quantitative determination of bile acids in feces
title_short Extraction and quantitative determination of bile acids in feces
title_sort extraction and quantitative determination of bile acids in feces
topic Science & Technology
Physical Sciences
Chemistry, Analytical
Chemistry
Bile acids
Fecal
LC-MS
MS
Extraction
Stability
url http://hdl.handle.net/20.500.11937/86513