Development and validation of an UHPLC-HRMS protocol for the analysis of flavan-3-ol metabolites and catabolites in urine, plasma and feces of rats fed a red wine proanthocyanidin extract
•Validation of a new LC-HRMS method to determine in vivo metabolites/catabolites.•34 metabolites/catabolites from a red wine proanthocyanidin extract were quantified.•Enable quantification of metabolites/catabolites in rat plasma, urine and feces.•Full validation according to the EURACHEM guidelines...
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| Veröffentlicht in: | Food chemistry 2018-06, Vol.252, p.49-60 |
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| creator | Pereira-Caro, Gema Ordóñez, José Luis Ludwig, Iziar Gaillet, Sylvie Mena, Pedro Del Rio, Daniele Rouanet, Jean-Max Bindon, Keren A. Moreno-Rojas, José Manuel Crozier, Alan |
| description | •Validation of a new LC-HRMS method to determine in vivo metabolites/catabolites.•34 metabolites/catabolites from a red wine proanthocyanidin extract were quantified.•Enable quantification of metabolites/catabolites in rat plasma, urine and feces.•Full validation according to the EURACHEM guidelines.
This study developed, optimized and validated an ultra-high-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS) method to identify and quantify metabolites and microbial-derived catabolites in urine, plasma and feces of rats following ingestion of 50 mg of a red wine proanthocyanidin-rich extract. The method was validated for specificity, linearity, limit of detection (LD) and quantification (LQ), intra-day and inter-day precision, recovery and matrix effects, which were determined for 34 compounds in the three biological matrices. After method validation, three parent flavan-3-ols, four 5-carbon side chain ring fission metabolites, and 27 phenolic acid and aromatic catabolites were quantified in plasma, urine and feces after red wine proanthocyanidin intake. These results establish the value of the UHPLC-HRMS protocol in obtaining a detailed picture of proanthocyanidin metabolites and their microbial-derived catabolites, along with their phase II metabolites, in biological fluids of rat, and potentially in human clinical studies designed to evaluate the bioavailability of dietary flavan-3-ols. |
| doi_str_mv | 10.1016/j.foodchem.2018.01.083 |
| format | Article |
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This study developed, optimized and validated an ultra-high-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS) method to identify and quantify metabolites and microbial-derived catabolites in urine, plasma and feces of rats following ingestion of 50 mg of a red wine proanthocyanidin-rich extract. The method was validated for specificity, linearity, limit of detection (LD) and quantification (LQ), intra-day and inter-day precision, recovery and matrix effects, which were determined for 34 compounds in the three biological matrices. After method validation, three parent flavan-3-ols, four 5-carbon side chain ring fission metabolites, and 27 phenolic acid and aromatic catabolites were quantified in plasma, urine and feces after red wine proanthocyanidin intake. These results establish the value of the UHPLC-HRMS protocol in obtaining a detailed picture of proanthocyanidin metabolites and their microbial-derived catabolites, along with their phase II metabolites, in biological fluids of rat, and potentially in human clinical studies designed to evaluate the bioavailability of dietary flavan-3-ols.</description><identifier>ISSN: 0308-8146</identifier><identifier>EISSN: 1873-7072</identifier><identifier>DOI: 10.1016/j.foodchem.2018.01.083</identifier><identifier>PMID: 29478563</identifier><language>eng</language><publisher>England: Elsevier Ltd</publisher><subject>Animals ; Bioavailability ; Biological Availability ; Chromatography, High Pressure Liquid - methods ; Feces - chemistry ; Flavonoids - blood ; Flavonoids - metabolism ; Flavonoids - pharmacokinetics ; Flavonoids - urine ; Life Sciences ; Limit of Detection ; Male ; Mass Spectrometry - methods ; Method validation ; Microbial-derived catabolites ; Phenylvalerolactones ; Proanthocyanidins - pharmacology ; Rats ; UHPLC-HR-MS ; Wine - analysis ; Wine proanthocyanidins</subject><ispartof>Food chemistry, 2018-06, Vol.252, p.49-60</ispartof><rights>2018 Elsevier Ltd</rights><rights>Copyright © 2018 Elsevier Ltd. All rights reserved.</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c439t-5c0d323696112c926281e078464c93806ce112ba26e7bd85e4dfc2b9d98343ec3</citedby><cites>FETCH-LOGICAL-c439t-5c0d323696112c926281e078464c93806ce112ba26e7bd85e4dfc2b9d98343ec3</cites><orcidid>0000-0003-3162-0432 ; 0000-0003-2150-2977 ; 0000-0001-5394-1259 ; 0000-0002-6050-0870</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S0308814618300931$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>230,314,776,780,881,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/29478563$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink><backlink>$$Uhttps://hal.science/hal-01829215$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Pereira-Caro, Gema</creatorcontrib><creatorcontrib>Ordóñez, José Luis</creatorcontrib><creatorcontrib>Ludwig, Iziar</creatorcontrib><creatorcontrib>Gaillet, Sylvie</creatorcontrib><creatorcontrib>Mena, Pedro</creatorcontrib><creatorcontrib>Del Rio, Daniele</creatorcontrib><creatorcontrib>Rouanet, Jean-Max</creatorcontrib><creatorcontrib>Bindon, Keren A.</creatorcontrib><creatorcontrib>Moreno-Rojas, José Manuel</creatorcontrib><creatorcontrib>Crozier, Alan</creatorcontrib><title>Development and validation of an UHPLC-HRMS protocol for the analysis of flavan-3-ol metabolites and catabolites in urine, plasma and feces of rats fed a red wine proanthocyanidin extract</title><title>Food chemistry</title><addtitle>Food Chem</addtitle><description>•Validation of a new LC-HRMS method to determine in vivo metabolites/catabolites.•34 metabolites/catabolites from a red wine proanthocyanidin extract were quantified.•Enable quantification of metabolites/catabolites in rat plasma, urine and feces.•Full validation according to the EURACHEM guidelines.
This study developed, optimized and validated an ultra-high-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS) method to identify and quantify metabolites and microbial-derived catabolites in urine, plasma and feces of rats following ingestion of 50 mg of a red wine proanthocyanidin-rich extract. The method was validated for specificity, linearity, limit of detection (LD) and quantification (LQ), intra-day and inter-day precision, recovery and matrix effects, which were determined for 34 compounds in the three biological matrices. After method validation, three parent flavan-3-ols, four 5-carbon side chain ring fission metabolites, and 27 phenolic acid and aromatic catabolites were quantified in plasma, urine and feces after red wine proanthocyanidin intake. These results establish the value of the UHPLC-HRMS protocol in obtaining a detailed picture of proanthocyanidin metabolites and their microbial-derived catabolites, along with their phase II metabolites, in biological fluids of rat, and potentially in human clinical studies designed to evaluate the bioavailability of dietary flavan-3-ols.</description><subject>Animals</subject><subject>Bioavailability</subject><subject>Biological Availability</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Feces - chemistry</subject><subject>Flavonoids - blood</subject><subject>Flavonoids - metabolism</subject><subject>Flavonoids - pharmacokinetics</subject><subject>Flavonoids - urine</subject><subject>Life Sciences</subject><subject>Limit of Detection</subject><subject>Male</subject><subject>Mass Spectrometry - methods</subject><subject>Method validation</subject><subject>Microbial-derived catabolites</subject><subject>Phenylvalerolactones</subject><subject>Proanthocyanidins - pharmacology</subject><subject>Rats</subject><subject>UHPLC-HR-MS</subject><subject>Wine - analysis</subject><subject>Wine proanthocyanidins</subject><issn>0308-8146</issn><issn>1873-7072</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2018</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkd2O0zAQhSMEYsvCK6x8CRIJ_kkT545VWShSEQjYa2tqT1RXTlxst9Bn25fDaXeXS25seeabc6w5RXHFaMUoa95tq957ozc4VJwyWVFWUSmeFDMmW1G2tOVPixkVVJaS1c1F8SLGLaV0Yp8XF7yrWzlvxKy4-4AHdH434JgIjIYcwFkDyfqR-D5XyO3y22pRLr9_-UF2wSevvSO9DyRtMLfBHaONE9o7OMBYijL3B0yw9s4mjCdRDf_ediT7YEd8S3YO4gAnoEeNJ5UAKeaXIUBCPn9ncLKFMW28PsJoTZ7HPymATi-LZz24iK_u78vi9uPNz8WyXH399HlxvSp1LbpUzjU1goumaxjjuuMNlwxpK-um1p2QtNGYG2vgDbZrI-dYm17zdWc6KWqBWlwWb866G3BqF-wA4ag8WLW8XqmplpfKO87mB5bZ12c2f_rXHmNSg40anYMR_T4qTnNMLZ_LOqPNGdXBxxiwf9RmVE0hq616CFlNwWUflafz4NW9x349oHkce0g1A-_PAOatHCwGFbXFUaOxAXVSxtv_efwFqCS8xA</recordid><startdate>20180630</startdate><enddate>20180630</enddate><creator>Pereira-Caro, Gema</creator><creator>Ordóñez, José Luis</creator><creator>Ludwig, Iziar</creator><creator>Gaillet, Sylvie</creator><creator>Mena, Pedro</creator><creator>Del Rio, Daniele</creator><creator>Rouanet, Jean-Max</creator><creator>Bindon, Keren A.</creator><creator>Moreno-Rojas, José Manuel</creator><creator>Crozier, Alan</creator><general>Elsevier Ltd</general><general>Elsevier</general><scope>CGR</scope><scope>CUY</scope><scope>CVF</scope><scope>ECM</scope><scope>EIF</scope><scope>NPM</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7X8</scope><scope>1XC</scope><orcidid>https://orcid.org/0000-0003-3162-0432</orcidid><orcidid>https://orcid.org/0000-0003-2150-2977</orcidid><orcidid>https://orcid.org/0000-0001-5394-1259</orcidid><orcidid>https://orcid.org/0000-0002-6050-0870</orcidid></search><sort><creationdate>20180630</creationdate><title>Development and validation of an UHPLC-HRMS protocol for the analysis of flavan-3-ol metabolites and catabolites in urine, plasma and feces of rats fed a red wine proanthocyanidin extract</title><author>Pereira-Caro, Gema ; Ordóñez, José Luis ; Ludwig, Iziar ; Gaillet, Sylvie ; Mena, Pedro ; Del Rio, Daniele ; Rouanet, Jean-Max ; Bindon, Keren A. ; Moreno-Rojas, José Manuel ; Crozier, Alan</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c439t-5c0d323696112c926281e078464c93806ce112ba26e7bd85e4dfc2b9d98343ec3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2018</creationdate><topic>Animals</topic><topic>Bioavailability</topic><topic>Biological Availability</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Feces - chemistry</topic><topic>Flavonoids - blood</topic><topic>Flavonoids - metabolism</topic><topic>Flavonoids - pharmacokinetics</topic><topic>Flavonoids - urine</topic><topic>Life Sciences</topic><topic>Limit of Detection</topic><topic>Male</topic><topic>Mass Spectrometry - methods</topic><topic>Method validation</topic><topic>Microbial-derived catabolites</topic><topic>Phenylvalerolactones</topic><topic>Proanthocyanidins - pharmacology</topic><topic>Rats</topic><topic>UHPLC-HR-MS</topic><topic>Wine - analysis</topic><topic>Wine proanthocyanidins</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Pereira-Caro, Gema</creatorcontrib><creatorcontrib>Ordóñez, José Luis</creatorcontrib><creatorcontrib>Ludwig, Iziar</creatorcontrib><creatorcontrib>Gaillet, Sylvie</creatorcontrib><creatorcontrib>Mena, Pedro</creatorcontrib><creatorcontrib>Del Rio, Daniele</creatorcontrib><creatorcontrib>Rouanet, Jean-Max</creatorcontrib><creatorcontrib>Bindon, Keren A.</creatorcontrib><creatorcontrib>Moreno-Rojas, José Manuel</creatorcontrib><creatorcontrib>Crozier, Alan</creatorcontrib><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>MEDLINE - Academic</collection><collection>Hyper Article en Ligne (HAL)</collection><jtitle>Food chemistry</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Pereira-Caro, Gema</au><au>Ordóñez, José Luis</au><au>Ludwig, Iziar</au><au>Gaillet, Sylvie</au><au>Mena, Pedro</au><au>Del Rio, Daniele</au><au>Rouanet, Jean-Max</au><au>Bindon, Keren A.</au><au>Moreno-Rojas, José Manuel</au><au>Crozier, Alan</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Development and validation of an UHPLC-HRMS protocol for the analysis of flavan-3-ol metabolites and catabolites in urine, plasma and feces of rats fed a red wine proanthocyanidin extract</atitle><jtitle>Food chemistry</jtitle><addtitle>Food Chem</addtitle><date>2018-06-30</date><risdate>2018</risdate><volume>252</volume><spage>49</spage><epage>60</epage><pages>49-60</pages><issn>0308-8146</issn><eissn>1873-7072</eissn><abstract>•Validation of a new LC-HRMS method to determine in vivo metabolites/catabolites.•34 metabolites/catabolites from a red wine proanthocyanidin extract were quantified.•Enable quantification of metabolites/catabolites in rat plasma, urine and feces.•Full validation according to the EURACHEM guidelines.
This study developed, optimized and validated an ultra-high-performance liquid chromatography–high-resolution mass spectrometry (UHPLC-HRMS) method to identify and quantify metabolites and microbial-derived catabolites in urine, plasma and feces of rats following ingestion of 50 mg of a red wine proanthocyanidin-rich extract. The method was validated for specificity, linearity, limit of detection (LD) and quantification (LQ), intra-day and inter-day precision, recovery and matrix effects, which were determined for 34 compounds in the three biological matrices. After method validation, three parent flavan-3-ols, four 5-carbon side chain ring fission metabolites, and 27 phenolic acid and aromatic catabolites were quantified in plasma, urine and feces after red wine proanthocyanidin intake. These results establish the value of the UHPLC-HRMS protocol in obtaining a detailed picture of proanthocyanidin metabolites and their microbial-derived catabolites, along with their phase II metabolites, in biological fluids of rat, and potentially in human clinical studies designed to evaluate the bioavailability of dietary flavan-3-ols.</abstract><cop>England</cop><pub>Elsevier Ltd</pub><pmid>29478563</pmid><doi>10.1016/j.foodchem.2018.01.083</doi><tpages>12</tpages><orcidid>https://orcid.org/0000-0003-3162-0432</orcidid><orcidid>https://orcid.org/0000-0003-2150-2977</orcidid><orcidid>https://orcid.org/0000-0001-5394-1259</orcidid><orcidid>https://orcid.org/0000-0002-6050-0870</orcidid></addata></record> |
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| identifier | ISSN: 0308-8146 |
| ispartof | Food chemistry, 2018-06, Vol.252, p.49-60 |
| issn | 0308-8146 1873-7072 |
| language | eng |
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| source | MEDLINE; Elsevier ScienceDirect Journals |
| subjects | Animals Bioavailability Biological Availability Chromatography, High Pressure Liquid - methods Feces - chemistry Flavonoids - blood Flavonoids - metabolism Flavonoids - pharmacokinetics Flavonoids - urine Life Sciences Limit of Detection Male Mass Spectrometry - methods Method validation Microbial-derived catabolites Phenylvalerolactones Proanthocyanidins - pharmacology Rats UHPLC-HR-MS Wine - analysis Wine proanthocyanidins |
| title | Development and validation of an UHPLC-HRMS protocol for the analysis of flavan-3-ol metabolites and catabolites in urine, plasma and feces of rats fed a red wine proanthocyanidin extract |
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