TY - JOUR
T1 - Determination of alkylresorcinols and their metabolites in biological samples by gas chromatography-mass spectrometry
AU - Wierzbicka, Roksana
AU - Wu, Huaxing
AU - Franek, Milan
AU - Kamal-Eldin, Afaf
AU - Landberg, Rikard
N1 - Funding Information:
We would like to acknowledge Ms. Janicka Nilsson, MSc. Izabela Biskup and MSc. Karthik Balekudru Vishwanath for excellent technical assistance. Dr. Ali Moazzami is acknowledged for valuable discussions regarding some aspects of the method development. The Swedish Research Council for Environment, Agricultural Sciences and Spatial Planning (FORMAS) and the Swedish Research Council Medicine (VR-medicine) are acknowledged for financial support.
Publisher Copyright:
© 2015 The Authors.
PY - 2015/9/1
Y1 - 2015/9/1
N2 - High throughput GC-MS methods for quantification of alkylresorcinols (AR), biomarkers of whole grain wheat and rye intake, in plasma and adipose tissue and their metabolites in urine were developed and optimised. Alkylresorcinols in plasma (200. μL) and adipose tissues (10-50. mg) were extracted with diethyl ether, whereas main AR metabolites such as DHBA and DHPPA and newly identified metabolites in urine (50. μL) were extracted with ethyl acetate after enzymatic deconjugation. All extracts were purified on OASIS-MAX solid phase extraction cartridges. Plasma and adipose tissue sample extracts were then derivatised with trifluoroacetic anhydride and reconstituted in undecane, whereas AR metabolites in urine samples were derivatised with BSTFA + TMCS (99:1, v/v, 100. μL). Prepared samples were quantified by GC-MS (EI-SIM). Analysis of all compounds in the different matrices showed good selectivity, sensitivity, linearity, precision (<15% within and between batches), adequate recovery (75-108%), and short total run time (10-12. min). The methods developed are applicable to large-scale sample sets such as epidemiological studies.
AB - High throughput GC-MS methods for quantification of alkylresorcinols (AR), biomarkers of whole grain wheat and rye intake, in plasma and adipose tissue and their metabolites in urine were developed and optimised. Alkylresorcinols in plasma (200. μL) and adipose tissues (10-50. mg) were extracted with diethyl ether, whereas main AR metabolites such as DHBA and DHPPA and newly identified metabolites in urine (50. μL) were extracted with ethyl acetate after enzymatic deconjugation. All extracts were purified on OASIS-MAX solid phase extraction cartridges. Plasma and adipose tissue sample extracts were then derivatised with trifluoroacetic anhydride and reconstituted in undecane, whereas AR metabolites in urine samples were derivatised with BSTFA + TMCS (99:1, v/v, 100. μL). Prepared samples were quantified by GC-MS (EI-SIM). Analysis of all compounds in the different matrices showed good selectivity, sensitivity, linearity, precision (<15% within and between batches), adequate recovery (75-108%), and short total run time (10-12. min). The methods developed are applicable to large-scale sample sets such as epidemiological studies.
KW - Alkylresorcinol
KW - Alkylresorcinols metabolites
KW - Biomarker
KW - Gas chromatography-mass spectrometry
KW - Whole grain
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U2 - 10.1016/j.jchromb.2015.07.009
DO - 10.1016/j.jchromb.2015.07.009
M3 - Article
C2 - 26218771
AN - SCOPUS:84938093881
SN - 1570-0232
VL - 1000
SP - 120
EP - 129
JO - Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
JF - Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences
ER -