A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry
A general screening method based on solid phase extraction (SPE) and liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) was developed and investigated with 124 different doping agents, including stimulants, β -blockers, narcotics, β 2 -adrenergic agonists, agents with anti-estrogenic...
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| Veröffentlicht in: | Analytica chimica acta 2007-02, Vol.585 (1), p.94-102 |
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| creator | Kolmonen, Marjo Leinonen, Antti Pelander, Anna Ojanperä, Ilkka |
| description | A general screening method based on solid phase extraction (SPE) and liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) was developed and investigated with 124 different doping agents, including stimulants,
β
-blockers, narcotics,
β
2
-adrenergic agonists, agents with anti-estrogenic activity, diuretics and cannabinoids. Mixed mode cation exchange/C8 cartridges were applied to SPE, and chromatography was based on gradient elution on a C18 column. Ionization of the analytes was achieved with electrospray ionization in the positive mode. Identification by LC/TOFMS was based on retention time, accurate mass and isotopic pattern. Validation of the method consisted of analysis of specificity, analytical recovery, limit of detection and repeatability. The minimum required performance limit (MRPL), established by World Anti-Doping Agency (WADA), was attained to 97 doping agents. The extraction recoveries varied between 33 and 98% and the median was 58%. Mass accuracy was always better than 5 ppm, corresponding to a maximum mass error of 0.7 mDa. The repeatability of the method for spiked urine samples, expressed as median of relative standard deviations (RSD%) at concentrations of MRPL and 10 times MRPL, were 14% and 9%, respectively. The suitability of the LC/TOFMS method for doping control was demonstrated with authentic urine samples. |
| doi_str_mv | 10.1016/j.aca.2006.12.028 |
| format | Article |
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β
-blockers, narcotics,
β
2
-adrenergic agonists, agents with anti-estrogenic activity, diuretics and cannabinoids. Mixed mode cation exchange/C8 cartridges were applied to SPE, and chromatography was based on gradient elution on a C18 column. Ionization of the analytes was achieved with electrospray ionization in the positive mode. Identification by LC/TOFMS was based on retention time, accurate mass and isotopic pattern. Validation of the method consisted of analysis of specificity, analytical recovery, limit of detection and repeatability. The minimum required performance limit (MRPL), established by World Anti-Doping Agency (WADA), was attained to 97 doping agents. The extraction recoveries varied between 33 and 98% and the median was 58%. Mass accuracy was always better than 5 ppm, corresponding to a maximum mass error of 0.7 mDa. The repeatability of the method for spiked urine samples, expressed as median of relative standard deviations (RSD%) at concentrations of MRPL and 10 times MRPL, were 14% and 9%, respectively. The suitability of the LC/TOFMS method for doping control was demonstrated with authentic urine samples.</description><identifier>ISSN: 0003-2670</identifier><identifier>EISSN: 1873-4324</identifier><identifier>DOI: 10.1016/j.aca.2006.12.028</identifier><identifier>PMID: 17386652</identifier><identifier>CODEN: ACACAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Anabolic Agents - urine ; Analytical chemistry ; Calibration ; Chemistry ; Chemistry Techniques, Analytical - methods ; Chromatographic methods and physical methods associated with chromatography ; Chromatography, Ion Exchange - methods ; Chromatography, Liquid - methods ; Doping analysis ; Doping in Sports ; Electrospray ionization ; Exact sciences and technology ; Humans ; Liquid chromatography ; Mass Spectrometry - methods ; Other chromatographic methods ; Reference Standards ; Reproducibility of Results ; Sensitivity and Specificity ; Solid phase extraction ; Solid Phase Extraction - methods ; Spectrometric and optical methods ; Spectrometry, Mass, Electrospray Ionization - methods ; Substance Abuse Detection - methods ; Time-of-flight mass spectrometry ; Urinalysis - methods</subject><ispartof>Analytica chimica acta, 2007-02, Vol.585 (1), p.94-102</ispartof><rights>2006 Elsevier B.V.</rights><rights>2007 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c447t-82344db8b9d5f22a401c1e79ac2bc513ec9ec12e96d56262e6e24e28224067143</citedby><cites>FETCH-LOGICAL-c447t-82344db8b9d5f22a401c1e79ac2bc513ec9ec12e96d56262e6e24e28224067143</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S0003267006024524$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3536,27903,27904,65309</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=18497819$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/17386652$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Kolmonen, Marjo</creatorcontrib><creatorcontrib>Leinonen, Antti</creatorcontrib><creatorcontrib>Pelander, Anna</creatorcontrib><creatorcontrib>Ojanperä, Ilkka</creatorcontrib><title>A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry</title><title>Analytica chimica acta</title><addtitle>Anal Chim Acta</addtitle><description>A general screening method based on solid phase extraction (SPE) and liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) was developed and investigated with 124 different doping agents, including stimulants,
β
-blockers, narcotics,
β
2
-adrenergic agonists, agents with anti-estrogenic activity, diuretics and cannabinoids. Mixed mode cation exchange/C8 cartridges were applied to SPE, and chromatography was based on gradient elution on a C18 column. Ionization of the analytes was achieved with electrospray ionization in the positive mode. Identification by LC/TOFMS was based on retention time, accurate mass and isotopic pattern. Validation of the method consisted of analysis of specificity, analytical recovery, limit of detection and repeatability. The minimum required performance limit (MRPL), established by World Anti-Doping Agency (WADA), was attained to 97 doping agents. The extraction recoveries varied between 33 and 98% and the median was 58%. Mass accuracy was always better than 5 ppm, corresponding to a maximum mass error of 0.7 mDa. The repeatability of the method for spiked urine samples, expressed as median of relative standard deviations (RSD%) at concentrations of MRPL and 10 times MRPL, were 14% and 9%, respectively. The suitability of the LC/TOFMS method for doping control was demonstrated with authentic urine samples.</description><subject>Anabolic Agents - urine</subject><subject>Analytical chemistry</subject><subject>Calibration</subject><subject>Chemistry</subject><subject>Chemistry Techniques, Analytical - methods</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Chromatography, Ion Exchange - methods</subject><subject>Chromatography, Liquid - methods</subject><subject>Doping analysis</subject><subject>Doping in Sports</subject><subject>Electrospray ionization</subject><subject>Exact sciences and technology</subject><subject>Humans</subject><subject>Liquid chromatography</subject><subject>Mass Spectrometry - methods</subject><subject>Other chromatographic methods</subject><subject>Reference Standards</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Solid phase extraction</subject><subject>Solid Phase Extraction - methods</subject><subject>Spectrometric and optical methods</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>Substance Abuse Detection - methods</subject><subject>Time-of-flight mass spectrometry</subject><subject>Urinalysis - methods</subject><issn>0003-2670</issn><issn>1873-4324</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2007</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9kcFu1DAQhiMEotvCA3BBvsAtqT1xnEScqgooUiUucLYce7LxKrFT20Hdt-CR8WpX6o3TaGa-fzT6_6L4wGjFKBO3h0ppVQGlomJQUeheFTvWtXXJa-Cvix2ltC5BtPSquI7xkFtglL8trlhbd0I0sCv-3pE9OgxqJlEHRGfdniyYJm_I6AMxfj1NVIZSJNaRaVuUI1uwDslwJNHP1pB1UhEJPqegdLLeEeUMme3Tlnd6Cn5Rye-DWqfjbbILln4sx9nup0QWFSOJK-qUKUzh-K54M6o54vtLvSl-f_v66_6hfPz5_cf93WOpOW9T2UHNuRm6oTfNCKA4ZZph2ysNg25YjbpHzQB7YRoBAlAgcIQOgFPRMl7fFJ_Pd9fgnzaMSS42apxn5dBvUba0ZiBYk0F2BnXwMQYc5RrsosJRMipPMciDzDHIUwySgcwxZM3Hy_FtWNC8KC6-Z-DTBVBRq3kMymkbX7iO923H-sx9OXOYrfhjMcioLTqNxobsmTTe_ueNf0yMp2c</recordid><startdate>20070228</startdate><enddate>20070228</enddate><creator>Kolmonen, Marjo</creator><creator>Leinonen, Antti</creator><creator>Pelander, Anna</creator><creator>Ojanperä, Ilkka</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>7X8</scope></search><sort><creationdate>20070228</creationdate><title>A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry</title><author>Kolmonen, Marjo ; Leinonen, Antti ; Pelander, Anna ; Ojanperä, Ilkka</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c447t-82344db8b9d5f22a401c1e79ac2bc513ec9ec12e96d56262e6e24e28224067143</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2007</creationdate><topic>Anabolic Agents - urine</topic><topic>Analytical chemistry</topic><topic>Calibration</topic><topic>Chemistry</topic><topic>Chemistry Techniques, Analytical - methods</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Chromatography, Ion Exchange - methods</topic><topic>Chromatography, Liquid - methods</topic><topic>Doping analysis</topic><topic>Doping in Sports</topic><topic>Electrospray ionization</topic><topic>Exact sciences and technology</topic><topic>Humans</topic><topic>Liquid chromatography</topic><topic>Mass Spectrometry - methods</topic><topic>Other chromatographic methods</topic><topic>Reference Standards</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Solid phase extraction</topic><topic>Solid Phase Extraction - methods</topic><topic>Spectrometric and optical methods</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>Substance Abuse Detection - methods</topic><topic>Time-of-flight mass spectrometry</topic><topic>Urinalysis - methods</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Kolmonen, Marjo</creatorcontrib><creatorcontrib>Leinonen, Antti</creatorcontrib><creatorcontrib>Pelander, Anna</creatorcontrib><creatorcontrib>Ojanperä, Ilkka</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>MEDLINE - Academic</collection><jtitle>Analytica chimica acta</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Kolmonen, Marjo</au><au>Leinonen, Antti</au><au>Pelander, Anna</au><au>Ojanperä, Ilkka</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry</atitle><jtitle>Analytica chimica acta</jtitle><addtitle>Anal Chim Acta</addtitle><date>2007-02-28</date><risdate>2007</risdate><volume>585</volume><issue>1</issue><spage>94</spage><epage>102</epage><pages>94-102</pages><issn>0003-2670</issn><eissn>1873-4324</eissn><coden>ACACAM</coden><abstract>A general screening method based on solid phase extraction (SPE) and liquid chromatography/time-of-flight mass spectrometry (LC/TOFMS) was developed and investigated with 124 different doping agents, including stimulants,
β
-blockers, narcotics,
β
2
-adrenergic agonists, agents with anti-estrogenic activity, diuretics and cannabinoids. Mixed mode cation exchange/C8 cartridges were applied to SPE, and chromatography was based on gradient elution on a C18 column. Ionization of the analytes was achieved with electrospray ionization in the positive mode. Identification by LC/TOFMS was based on retention time, accurate mass and isotopic pattern. Validation of the method consisted of analysis of specificity, analytical recovery, limit of detection and repeatability. The minimum required performance limit (MRPL), established by World Anti-Doping Agency (WADA), was attained to 97 doping agents. The extraction recoveries varied between 33 and 98% and the median was 58%. Mass accuracy was always better than 5 ppm, corresponding to a maximum mass error of 0.7 mDa. The repeatability of the method for spiked urine samples, expressed as median of relative standard deviations (RSD%) at concentrations of MRPL and 10 times MRPL, were 14% and 9%, respectively. The suitability of the LC/TOFMS method for doping control was demonstrated with authentic urine samples.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>17386652</pmid><doi>10.1016/j.aca.2006.12.028</doi><tpages>9</tpages></addata></record> |
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| source | MEDLINE; Elsevier ScienceDirect Journals |
| subjects | Anabolic Agents - urine Analytical chemistry Calibration Chemistry Chemistry Techniques, Analytical - methods Chromatographic methods and physical methods associated with chromatography Chromatography, Ion Exchange - methods Chromatography, Liquid - methods Doping analysis Doping in Sports Electrospray ionization Exact sciences and technology Humans Liquid chromatography Mass Spectrometry - methods Other chromatographic methods Reference Standards Reproducibility of Results Sensitivity and Specificity Solid phase extraction Solid Phase Extraction - methods Spectrometric and optical methods Spectrometry, Mass, Electrospray Ionization - methods Substance Abuse Detection - methods Time-of-flight mass spectrometry Urinalysis - methods |
| title | A general screening method for doping agents in human urine by solid phase extraction and liquid chromatography/time-of-flight mass spectrometry |
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