Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry
•Alkylamines are the stimulant agents with smaller molecular size.•Liquid chromatography tandem mass spectrometry is the most suitable for screening.•Gas chromatography–mass spectrometry is the most suitable for confirmation.•Different derivatization reactions are necessary for adequate characteriza...
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| Veröffentlicht in: | Journal of Chromatography A 2013-07, Vol.1298, p.76-85 |
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| creator | Sardela, Vinícius F. Sardela, Patrícia D.O. Deventer, Koen Araujo, Amanda L.D. Cavalcante, Karina M. Padilha, Monica C. Pereira, Henrique M.G. Van Eenoo, Peter Aquino Neto, Francisco R. |
| description | •Alkylamines are the stimulant agents with smaller molecular size.•Liquid chromatography tandem mass spectrometry is the most suitable for screening.•Gas chromatography–mass spectrometry is the most suitable for confirmation.•Different derivatization reactions are necessary for adequate characterization.
The detection of 11 sympathomimetic alkylamines in urine was presented with a focus on human doping control is proposed using liquid chromatography tandem mass spectrometry (LC-QqQ) and high resolution mass spectrometry (LC–HRMS) as a screening tool after a dilute-and-shoot (DS) approach. For the LC–HRMS analyses, several compounds exhibited better limits of detection (L.O.D.) than the LC-QqQ. However, due to their small differences in structure, co-elution among the alkylamines was observed. Therefore, the chemical conversion of the alkylamines into an appropriate derivative for the confirmation analyses using gas chromatography–mass spectrometry (GC–MS) was evaluated. Five derivatization approaches were evaluated in an attempt to increase the analytical response and the confidence of the identification. The choice of the appropriated derivative for each alkylamine makes their spectra more easily interpretable, fulfills the WADA's rather strict identification criteria and enables the unequivocal identification of alkylamines in urine. |
| doi_str_mv | 10.1016/j.chroma.2013.05.016 |
| format | Article |
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The detection of 11 sympathomimetic alkylamines in urine was presented with a focus on human doping control is proposed using liquid chromatography tandem mass spectrometry (LC-QqQ) and high resolution mass spectrometry (LC–HRMS) as a screening tool after a dilute-and-shoot (DS) approach. For the LC–HRMS analyses, several compounds exhibited better limits of detection (L.O.D.) than the LC-QqQ. However, due to their small differences in structure, co-elution among the alkylamines was observed. Therefore, the chemical conversion of the alkylamines into an appropriate derivative for the confirmation analyses using gas chromatography–mass spectrometry (GC–MS) was evaluated. Five derivatization approaches were evaluated in an attempt to increase the analytical response and the confidence of the identification. The choice of the appropriated derivative for each alkylamine makes their spectra more easily interpretable, fulfills the WADA's rather strict identification criteria and enables the unequivocal identification of alkylamines in urine.</description><identifier>ISSN: 0021-9673</identifier><identifier>EISSN: 1873-3778</identifier><identifier>DOI: 10.1016/j.chroma.2013.05.016</identifier><identifier>PMID: 23746644</identifier><identifier>CODEN: JOCRAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Alkylamines ; Analysis ; Anti-doping ; Biological and medical sciences ; Chromatography ; Chromatography, Liquid - methods ; Derivatives ; Derivatization ; Doping ; Gas chromatography ; Gas Chromatography-Mass Spectrometry - methods ; General pharmacology ; Humans ; Liquid chromatography ; Mass spectrometry ; Medical sciences ; Pharmacology. Drug treatments ; Stimulants ; Sympathomimetic agents ; Sympathomimetics - analysis ; Tandem Mass Spectrometry - methods ; Urine</subject><ispartof>Journal of Chromatography A, 2013-07, Vol.1298, p.76-85</ispartof><rights>2013 Elsevier B.V.</rights><rights>2014 INIST-CNRS</rights><rights>Copyright © 2013 Elsevier B.V. All rights reserved.</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c504t-5f79b51480b1249fea075600c5c8200745c43b8bacd2bb5f288994daddb7a3033</citedby><cites>FETCH-LOGICAL-c504t-5f79b51480b1249fea075600c5c8200745c43b8bacd2bb5f288994daddb7a3033</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.chroma.2013.05.016$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3536,27903,27904,45974</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=27499249$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/23746644$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Sardela, Vinícius F.</creatorcontrib><creatorcontrib>Sardela, Patrícia D.O.</creatorcontrib><creatorcontrib>Deventer, Koen</creatorcontrib><creatorcontrib>Araujo, Amanda L.D.</creatorcontrib><creatorcontrib>Cavalcante, Karina M.</creatorcontrib><creatorcontrib>Padilha, Monica C.</creatorcontrib><creatorcontrib>Pereira, Henrique M.G.</creatorcontrib><creatorcontrib>Van Eenoo, Peter</creatorcontrib><creatorcontrib>Aquino Neto, Francisco R.</creatorcontrib><title>Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry</title><title>Journal of Chromatography A</title><addtitle>J Chromatogr A</addtitle><description>•Alkylamines are the stimulant agents with smaller molecular size.•Liquid chromatography tandem mass spectrometry is the most suitable for screening.•Gas chromatography–mass spectrometry is the most suitable for confirmation.•Different derivatization reactions are necessary for adequate characterization.
The detection of 11 sympathomimetic alkylamines in urine was presented with a focus on human doping control is proposed using liquid chromatography tandem mass spectrometry (LC-QqQ) and high resolution mass spectrometry (LC–HRMS) as a screening tool after a dilute-and-shoot (DS) approach. For the LC–HRMS analyses, several compounds exhibited better limits of detection (L.O.D.) than the LC-QqQ. However, due to their small differences in structure, co-elution among the alkylamines was observed. Therefore, the chemical conversion of the alkylamines into an appropriate derivative for the confirmation analyses using gas chromatography–mass spectrometry (GC–MS) was evaluated. Five derivatization approaches were evaluated in an attempt to increase the analytical response and the confidence of the identification. The choice of the appropriated derivative for each alkylamine makes their spectra more easily interpretable, fulfills the WADA's rather strict identification criteria and enables the unequivocal identification of alkylamines in urine.</description><subject>Alkylamines</subject><subject>Analysis</subject><subject>Anti-doping</subject><subject>Biological and medical sciences</subject><subject>Chromatography</subject><subject>Chromatography, Liquid - methods</subject><subject>Derivatives</subject><subject>Derivatization</subject><subject>Doping</subject><subject>Gas chromatography</subject><subject>Gas Chromatography-Mass Spectrometry - methods</subject><subject>General pharmacology</subject><subject>Humans</subject><subject>Liquid chromatography</subject><subject>Mass spectrometry</subject><subject>Medical sciences</subject><subject>Pharmacology. Drug treatments</subject><subject>Stimulants</subject><subject>Sympathomimetic agents</subject><subject>Sympathomimetics - analysis</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Urine</subject><issn>0021-9673</issn><issn>1873-3778</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2013</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqNkU2O1DAQhSMEYpqBGyDkDRKbBDt24mSDhEb8jDQSG1hbFdvpdpPYGVcyUlhxB07HlpPgVhrYASvLVV_VK72XZU8ZLRhl9ctjoQ8xjFCUlPGCVkUq3st2rJE851I297MdpSXL21ryi-wR4pFSJqksH2YXJZeiroXYZd-vjfWz652G2QVPQk9wHSeYD2F0o52dJjB8XgcYnbcE9glG4jxZ4um_oPN7MrjbxRmynTOHfYTpsP74-m0ERIKT1XNq2DmuBHzCQlofHW5ixkZ3l6S_bPIJOwSDpA8xgb53cdwa4GFY0SLpVrIH_A-xx9mDHga0T87vZfbp7ZuPV-_zmw_vrq9e3-S6omLOq162XcVEQztWira3QGVVU6or3ZSUSlFpwbumA23Krqv6smnaVhgwppPAKeeX2Ytt7xTD7WJxVqNDbYcBvA0LKtZQKjjjvPw3WleibmrRNgkVG6pjQIy2V1N0I8RVMapO-auj2jxQp_wVrVQqprFnZ4WlG635PfQr8AQ8PwOAGoY-gtcO_3BStG2yIXGvNs4m6-6cjQq1s15b42LyWJng_n7JT6JU2lI</recordid><startdate>20130712</startdate><enddate>20130712</enddate><creator>Sardela, Vinícius F.</creator><creator>Sardela, Patrícia D.O.</creator><creator>Deventer, Koen</creator><creator>Araujo, Amanda L.D.</creator><creator>Cavalcante, Karina M.</creator><creator>Padilha, Monica C.</creator><creator>Pereira, Henrique M.G.</creator><creator>Van Eenoo, Peter</creator><creator>Aquino Neto, Francisco R.</creator><general>Elsevier B.V</general><general>Elsevier</general><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>7QH</scope><scope>7UA</scope><scope>C1K</scope><scope>F1W</scope><scope>H97</scope><scope>L.G</scope><scope>7U5</scope><scope>8FD</scope><scope>L7M</scope></search><sort><creationdate>20130712</creationdate><title>Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry</title><author>Sardela, Vinícius F. ; Sardela, Patrícia D.O. ; Deventer, Koen ; Araujo, Amanda L.D. ; Cavalcante, Karina M. ; Padilha, Monica C. ; Pereira, Henrique M.G. ; Van Eenoo, Peter ; Aquino Neto, Francisco R.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c504t-5f79b51480b1249fea075600c5c8200745c43b8bacd2bb5f288994daddb7a3033</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2013</creationdate><topic>Alkylamines</topic><topic>Analysis</topic><topic>Anti-doping</topic><topic>Biological and medical sciences</topic><topic>Chromatography</topic><topic>Chromatography, Liquid - methods</topic><topic>Derivatives</topic><topic>Derivatization</topic><topic>Doping</topic><topic>Gas chromatography</topic><topic>Gas Chromatography-Mass Spectrometry - methods</topic><topic>General pharmacology</topic><topic>Humans</topic><topic>Liquid chromatography</topic><topic>Mass spectrometry</topic><topic>Medical sciences</topic><topic>Pharmacology. Drug treatments</topic><topic>Stimulants</topic><topic>Sympathomimetic agents</topic><topic>Sympathomimetics - analysis</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Urine</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Sardela, Vinícius F.</creatorcontrib><creatorcontrib>Sardela, Patrícia D.O.</creatorcontrib><creatorcontrib>Deventer, Koen</creatorcontrib><creatorcontrib>Araujo, Amanda L.D.</creatorcontrib><creatorcontrib>Cavalcante, Karina M.</creatorcontrib><creatorcontrib>Padilha, Monica C.</creatorcontrib><creatorcontrib>Pereira, Henrique M.G.</creatorcontrib><creatorcontrib>Van Eenoo, Peter</creatorcontrib><creatorcontrib>Aquino Neto, Francisco R.</creatorcontrib><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>Aqualine</collection><collection>Water Resources Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>ASFA: Aquatic Sciences and Fisheries Abstracts</collection><collection>Aquatic Science & Fisheries Abstracts (ASFA) 3: Aquatic Pollution & Environmental Quality</collection><collection>Aquatic Science & Fisheries Abstracts (ASFA) Professional</collection><collection>Solid State and Superconductivity Abstracts</collection><collection>Technology Research Database</collection><collection>Advanced Technologies Database with Aerospace</collection><jtitle>Journal of Chromatography A</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Sardela, Vinícius F.</au><au>Sardela, Patrícia D.O.</au><au>Deventer, Koen</au><au>Araujo, Amanda L.D.</au><au>Cavalcante, Karina M.</au><au>Padilha, Monica C.</au><au>Pereira, Henrique M.G.</au><au>Van Eenoo, Peter</au><au>Aquino Neto, Francisco R.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry</atitle><jtitle>Journal of Chromatography A</jtitle><addtitle>J Chromatogr A</addtitle><date>2013-07-12</date><risdate>2013</risdate><volume>1298</volume><spage>76</spage><epage>85</epage><pages>76-85</pages><issn>0021-9673</issn><eissn>1873-3778</eissn><coden>JOCRAM</coden><abstract>•Alkylamines are the stimulant agents with smaller molecular size.•Liquid chromatography tandem mass spectrometry is the most suitable for screening.•Gas chromatography–mass spectrometry is the most suitable for confirmation.•Different derivatization reactions are necessary for adequate characterization.
The detection of 11 sympathomimetic alkylamines in urine was presented with a focus on human doping control is proposed using liquid chromatography tandem mass spectrometry (LC-QqQ) and high resolution mass spectrometry (LC–HRMS) as a screening tool after a dilute-and-shoot (DS) approach. For the LC–HRMS analyses, several compounds exhibited better limits of detection (L.O.D.) than the LC-QqQ. However, due to their small differences in structure, co-elution among the alkylamines was observed. Therefore, the chemical conversion of the alkylamines into an appropriate derivative for the confirmation analyses using gas chromatography–mass spectrometry (GC–MS) was evaluated. Five derivatization approaches were evaluated in an attempt to increase the analytical response and the confidence of the identification. The choice of the appropriated derivative for each alkylamine makes their spectra more easily interpretable, fulfills the WADA's rather strict identification criteria and enables the unequivocal identification of alkylamines in urine.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>23746644</pmid><doi>10.1016/j.chroma.2013.05.016</doi><tpages>10</tpages><oa>free_for_read</oa></addata></record> |
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| subjects | Alkylamines Analysis Anti-doping Biological and medical sciences Chromatography Chromatography, Liquid - methods Derivatives Derivatization Doping Gas chromatography Gas Chromatography-Mass Spectrometry - methods General pharmacology Humans Liquid chromatography Mass spectrometry Medical sciences Pharmacology. Drug treatments Stimulants Sympathomimetic agents Sympathomimetics - analysis Tandem Mass Spectrometry - methods Urine |
| title | Identification of sympathomimetic alkylamine agents in urine using liquid chromatography–mass spectrometry and comparison of derivatization methods for confirmation analyses by gas chromatography–mass spectrometry |
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