Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry
The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and ele...
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| Veröffentlicht in: | Journal of mass spectrometry. 2008-03, Vol.43 (3), p.394-408 |
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| container_title | Journal of mass spectrometry. |
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| creator | Pozo, Oscar J Van Thuyne, Wim Deventer, Koen Van Eenoo, Peter Delbeke, Frans T |
| description | The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MSn experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples. Copyright © 2007 John Wiley & Sons, Ltd. |
| doi_str_mv | 10.1002/jms.1343 |
| format | Article |
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Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MSn experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples. Copyright © 2007 John Wiley & Sons, Ltd.</description><identifier>ISSN: 1076-5174</identifier><identifier>EISSN: 1096-9888</identifier><identifier>DOI: 10.1002/jms.1343</identifier><identifier>PMID: 18035854</identifier><language>eng</language><publisher>Chichester, UK: John Wiley & Sons, Ltd</publisher><subject>accurate mass ; Anabolic Agents - chemistry ; Anabolic Agents - metabolism ; Anabolic Agents - urine ; anabolic steroids ; Analysis ; Biological and medical sciences ; Chromatography, Liquid - methods ; doping analysis ; Doping in Sports ; fluoxymesterone ; Fluoxymesterone - metabolism ; Fluoxymesterone - standards ; Fluoxymesterone - urine ; Gas Chromatography-Mass Spectrometry - methods ; General pharmacology ; Humans ; Medical sciences ; Metabolic Networks and Pathways ; metabolites ; Molecular Structure ; neutral loss ; Pharmacology. Drug treatments ; QTOF-MS ; Reference Standards ; Spectrometry, Mass, Electrospray Ionization - methods ; Substance Abuse Detection - methods ; Tandem Mass Spectrometry - methods</subject><ispartof>Journal of mass spectrometry., 2008-03, Vol.43 (3), p.394-408</ispartof><rights>Copyright © 2007 John Wiley & Sons, Ltd.</rights><rights>2008 INIST-CNRS</rights><rights>Copyright (c) 2008 John Wiley & Sons, Ltd.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c4423-f3c622f885a0dcdd2dc3816c8966064b97202cd23299a5b6ab0f86b302ee6cd83</citedby><cites>FETCH-LOGICAL-c4423-f3c622f885a0dcdd2dc3816c8966064b97202cd23299a5b6ab0f86b302ee6cd83</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1002%2Fjms.1343$$EPDF$$P50$$Gwiley$$H</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Fjms.1343$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>314,780,784,1417,27924,27925,45574,45575</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=20140416$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/18035854$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Pozo, Oscar J</creatorcontrib><creatorcontrib>Van Thuyne, Wim</creatorcontrib><creatorcontrib>Deventer, Koen</creatorcontrib><creatorcontrib>Van Eenoo, Peter</creatorcontrib><creatorcontrib>Delbeke, Frans T</creatorcontrib><title>Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry</title><title>Journal of mass spectrometry.</title><addtitle>J. Mass Spectrom</addtitle><description>The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MSn experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples. Copyright © 2007 John Wiley & Sons, Ltd.</description><subject>accurate mass</subject><subject>Anabolic Agents - chemistry</subject><subject>Anabolic Agents - metabolism</subject><subject>Anabolic Agents - urine</subject><subject>anabolic steroids</subject><subject>Analysis</subject><subject>Biological and medical sciences</subject><subject>Chromatography, Liquid - methods</subject><subject>doping analysis</subject><subject>Doping in Sports</subject><subject>fluoxymesterone</subject><subject>Fluoxymesterone - metabolism</subject><subject>Fluoxymesterone - standards</subject><subject>Fluoxymesterone - urine</subject><subject>Gas Chromatography-Mass Spectrometry - methods</subject><subject>General pharmacology</subject><subject>Humans</subject><subject>Medical sciences</subject><subject>Metabolic Networks and Pathways</subject><subject>metabolites</subject><subject>Molecular Structure</subject><subject>neutral loss</subject><subject>Pharmacology. Drug treatments</subject><subject>QTOF-MS</subject><subject>Reference Standards</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>Substance Abuse Detection - methods</subject><subject>Tandem Mass Spectrometry - methods</subject><issn>1076-5174</issn><issn>1096-9888</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2008</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqF0c1u1DAQB_AIgegHSDwB5ALikjK2E8c-VlVZWBU4bKtKXKyJ7WxdknhrJ6L7Fn1kvNqoSCDEyZb904zH_yx7ReCEANAPt308IaxkT7JDApIXUgjxdLeveVGRujzIjmK8BQApS_48OyACWCWq8jB7OO8m7QyOzg-5b_MpuAHDNu_tiI3v3Gjj7rjtJn-_7W0cbfCDzZtt3rm7yZlc3wTf4-jXATc322LEwdg-7zHGPG6sHtOtHVPBdJ6vMf7p_4IvsmctdtG-nNfj7Orj-eXZp-Li2-Lz2elFocuSsqJlmlPaClEhGG0MNZoJwrWQnAMvG1lToNpQRqXEquHYQCt4w4Bay7UR7Dh7t6-7Cf5uSoOp3kVtuw4H66eo6vRDNa3kfyGjwOqqggTf76EOPsZgW7UJrk-fqQioXUwqxaR2MSX6eq45Nb01v-GcSwJvZ4BRY9cGHLSLj44CKaEkPLli7366zm7_2VAtv6zmxrN3Kcn7R4_hh-J1GkNdf12o1fLy-_ViWatV8m_2vkWvcB3SG65WqTsDEFyCrNgvFbHFsw</recordid><startdate>200803</startdate><enddate>200803</enddate><creator>Pozo, Oscar J</creator><creator>Van Thuyne, Wim</creator><creator>Deventer, Koen</creator><creator>Van Eenoo, Peter</creator><creator>Delbeke, Frans T</creator><general>John Wiley & Sons, Ltd</general><general>Wiley</general><scope>FBQ</scope><scope>BSCLL</scope><scope>IQODW</scope><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>7SR</scope><scope>7U5</scope><scope>8BQ</scope><scope>8FD</scope><scope>JG9</scope><scope>L7M</scope><scope>7X8</scope></search><sort><creationdate>200803</creationdate><title>Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry</title><author>Pozo, Oscar J ; Van Thuyne, Wim ; Deventer, Koen ; Van Eenoo, Peter ; Delbeke, Frans T</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c4423-f3c622f885a0dcdd2dc3816c8966064b97202cd23299a5b6ab0f86b302ee6cd83</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2008</creationdate><topic>accurate mass</topic><topic>Anabolic Agents - chemistry</topic><topic>Anabolic Agents - metabolism</topic><topic>Anabolic Agents - urine</topic><topic>anabolic steroids</topic><topic>Analysis</topic><topic>Biological and medical sciences</topic><topic>Chromatography, Liquid - methods</topic><topic>doping analysis</topic><topic>Doping in Sports</topic><topic>fluoxymesterone</topic><topic>Fluoxymesterone - metabolism</topic><topic>Fluoxymesterone - standards</topic><topic>Fluoxymesterone - urine</topic><topic>Gas Chromatography-Mass Spectrometry - methods</topic><topic>General pharmacology</topic><topic>Humans</topic><topic>Medical sciences</topic><topic>Metabolic Networks and Pathways</topic><topic>metabolites</topic><topic>Molecular Structure</topic><topic>neutral loss</topic><topic>Pharmacology. Drug treatments</topic><topic>QTOF-MS</topic><topic>Reference Standards</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>Substance Abuse Detection - methods</topic><topic>Tandem Mass Spectrometry - methods</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Pozo, Oscar J</creatorcontrib><creatorcontrib>Van Thuyne, Wim</creatorcontrib><creatorcontrib>Deventer, Koen</creatorcontrib><creatorcontrib>Van Eenoo, Peter</creatorcontrib><creatorcontrib>Delbeke, Frans T</creatorcontrib><collection>AGRIS</collection><collection>Istex</collection><collection>Pascal-Francis</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>Engineered Materials Abstracts</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>METADEX</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of mass spectrometry.</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Pozo, Oscar J</au><au>Van Thuyne, Wim</au><au>Deventer, Koen</au><au>Van Eenoo, Peter</au><au>Delbeke, Frans T</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry</atitle><jtitle>Journal of mass spectrometry.</jtitle><addtitle>J. Mass Spectrom</addtitle><date>2008-03</date><risdate>2008</risdate><volume>43</volume><issue>3</issue><spage>394</spage><epage>408</epage><pages>394-408</pages><issn>1076-5174</issn><eissn>1096-9888</eissn><abstract>The suitability of liquid chromatography tandem mass spectrometry (LC-MS/MS) and gas chromatography mass spectrometry (GC-MS) for the elucidation of fluoxymesterone metabolism has been evaluated. Electrospray ionization (ESI) and collision induced dissociation (CID) fragmentation in LC-MS/MS and electron impact spectra (EI) in GC-MS have been studied for fluoxymesterone and two commercially available metabolites. MSn experiments and accurate mass measurements performed by an ion-trap analyser and a QTOF instrument respectively have been used for the elucidation of the fragmentation pathway. The neutral loss scan of 20 Da (loss of HF) in LC-MS/MS has been applied for the selective detection of fluoxymesterone metabolites. In a positive fluoxymesterone doping control sample, 9 different analytes have been detected including the parent compound. Seven of these metabolites were also confirmed by GC-MS including 5 previously unreported metabolites. On the basis of the ionization, the CID fragmentation, the accurate mass of the product ions and the EI spectra of these analytes, a tentative elucidation as well as a proposal for the metabolic pathway of fluoxymesterone has been suggested. The presence of these compounds has also been confirmed by the analysis of five other positive fluoxymesterone urine samples. Copyright © 2007 John Wiley & Sons, Ltd.</abstract><cop>Chichester, UK</cop><pub>John Wiley & Sons, Ltd</pub><pmid>18035854</pmid><doi>10.1002/jms.1343</doi><tpages>15</tpages></addata></record> |
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| ispartof | Journal of mass spectrometry., 2008-03, Vol.43 (3), p.394-408 |
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| source | Wiley Online Library - AutoHoldings Journals; MEDLINE |
| subjects | accurate mass Anabolic Agents - chemistry Anabolic Agents - metabolism Anabolic Agents - urine anabolic steroids Analysis Biological and medical sciences Chromatography, Liquid - methods doping analysis Doping in Sports fluoxymesterone Fluoxymesterone - metabolism Fluoxymesterone - standards Fluoxymesterone - urine Gas Chromatography-Mass Spectrometry - methods General pharmacology Humans Medical sciences Metabolic Networks and Pathways metabolites Molecular Structure neutral loss Pharmacology. Drug treatments QTOF-MS Reference Standards Spectrometry, Mass, Electrospray Ionization - methods Substance Abuse Detection - methods Tandem Mass Spectrometry - methods |
| title | Elucidation of urinary metabolites of fluoxymesterone by liquid chromatography-tandem mass spectrometry and gas chromatography-mass spectrometry |
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