Rapid and Sensitive Analysis of 3,4-Methylenedioxypyrovalerone in Equine Plasma Using Liquid Chromatography-Tandem Mass Spectrometry
3,4-Methylenedioxypyrovalerone (MDPV) is a psychoactive drug with potent stimulant properties and potential for abuse and drug dependency. MDPV was recently classified as a Class I drug by Racing Commissioners International, indicating that it is a banned substance in equine athletes because it lack...
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| Veröffentlicht in: | Journal of analytical toxicology 2012-06, Vol.36 (5), p.327-333 |
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| container_title | Journal of analytical toxicology |
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| creator | Wang, Caroline C. Hartmann-Fischbach, Petra Krueger, Tim R. Wells, Terry L. Feineman, Amy R. Compton, Joanne C. |
| description | 3,4-Methylenedioxypyrovalerone (MDPV) is a psychoactive drug with potent stimulant properties and potential for abuse and drug dependency. MDPV was recently classified as a Class I drug by Racing Commissioners International, indicating that it is a banned substance in equine athletes because it lacks therapeutic value in horses. To enforce this ban, a sensitive and fast liquid chromatography-tandem mass spectrometry method was needed. It is for this reason that this method was developed for quantification and confirmation of MDPV in equine plasma. Sample preparation involved liquid-liquid extraction. The analyte was analyzed by a triple-quadrupole linear ion trap mass spectrometer in positive multiple-reaction-monitoring and enhanced product ion scan modes. The method was validated for precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), linearity, stability, extraction recovery, matrix effect, dilution accuracy and selectivity. The extraction recovery was >90%. The linearity range was from 5 to 15,000 pg/mL. LOD and LOQ were 2 and 5 pg/mL, respectively. Intra-day and inter-day accuracies were nearly 100%. The method is suitable for screening, quantification and confirmation of MDPV in equine plasma and has been successfully used to detect and confirm the presence of MDPV in equine plasma obtained post-competition. |
| doi_str_mv | 10.1093/jat/bks033 |
| format | Article |
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MDPV was recently classified as a Class I drug by Racing Commissioners International, indicating that it is a banned substance in equine athletes because it lacks therapeutic value in horses. To enforce this ban, a sensitive and fast liquid chromatography-tandem mass spectrometry method was needed. It is for this reason that this method was developed for quantification and confirmation of MDPV in equine plasma. Sample preparation involved liquid-liquid extraction. The analyte was analyzed by a triple-quadrupole linear ion trap mass spectrometer in positive multiple-reaction-monitoring and enhanced product ion scan modes. The method was validated for precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), linearity, stability, extraction recovery, matrix effect, dilution accuracy and selectivity. The extraction recovery was >90%. The linearity range was from 5 to 15,000 pg/mL. LOD and LOQ were 2 and 5 pg/mL, respectively. Intra-day and inter-day accuracies were nearly 100%. The method is suitable for screening, quantification and confirmation of MDPV in equine plasma and has been successfully used to detect and confirm the presence of MDPV in equine plasma obtained post-competition.</description><identifier>ISSN: 0146-4760</identifier><identifier>EISSN: 1945-2403</identifier><identifier>DOI: 10.1093/jat/bks033</identifier><identifier>PMID: 22582267</identifier><identifier>CODEN: JATOD3</identifier><language>eng</language><publisher>Niles, IL: Oxford University Press</publisher><subject>Analysis ; Animals ; Benzodioxoles - blood ; Biological and medical sciences ; Chromatography, High Pressure Liquid ; Doping in Sports - prevention & control ; Drug abuse ; General pharmacology ; High-Throughput Screening Assays - veterinary ; Horses ; Mass spectroscopy ; Medical sciences ; Pharmacology. Drug treatments ; Psychotropic Drugs - blood ; Pyrrolidines - blood ; Reproducibility of Results ; Sensitivity and Specificity ; Spectrometry, Mass, Electrospray Ionization - methods ; Spectrometry, Mass, Electrospray Ionization - veterinary ; Stimulants ; Substance Abuse Detection - veterinary ; Tandem Mass Spectrometry - methods ; Tandem Mass Spectrometry - veterinary</subject><ispartof>Journal of analytical toxicology, 2012-06, Vol.36 (5), p.327-333</ispartof><rights>The Author [2012]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com 2012</rights><rights>2015 INIST-CNRS</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c3313-640745967028c277e5f7f7379dc4cc2e069a5467e73ed5092ba6b603f4221eaa3</citedby><cites>FETCH-LOGICAL-c3313-640745967028c277e5f7f7379dc4cc2e069a5467e73ed5092ba6b603f4221eaa3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,776,780,1578,27901,27902</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=25923419$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/22582267$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Wang, Caroline C.</creatorcontrib><creatorcontrib>Hartmann-Fischbach, Petra</creatorcontrib><creatorcontrib>Krueger, Tim R.</creatorcontrib><creatorcontrib>Wells, Terry L.</creatorcontrib><creatorcontrib>Feineman, Amy R.</creatorcontrib><creatorcontrib>Compton, Joanne C.</creatorcontrib><title>Rapid and Sensitive Analysis of 3,4-Methylenedioxypyrovalerone in Equine Plasma Using Liquid Chromatography-Tandem Mass Spectrometry</title><title>Journal of analytical toxicology</title><addtitle>J Anal Toxicol</addtitle><description>3,4-Methylenedioxypyrovalerone (MDPV) is a psychoactive drug with potent stimulant properties and potential for abuse and drug dependency. MDPV was recently classified as a Class I drug by Racing Commissioners International, indicating that it is a banned substance in equine athletes because it lacks therapeutic value in horses. To enforce this ban, a sensitive and fast liquid chromatography-tandem mass spectrometry method was needed. It is for this reason that this method was developed for quantification and confirmation of MDPV in equine plasma. Sample preparation involved liquid-liquid extraction. The analyte was analyzed by a triple-quadrupole linear ion trap mass spectrometer in positive multiple-reaction-monitoring and enhanced product ion scan modes. The method was validated for precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), linearity, stability, extraction recovery, matrix effect, dilution accuracy and selectivity. The extraction recovery was >90%. The linearity range was from 5 to 15,000 pg/mL. LOD and LOQ were 2 and 5 pg/mL, respectively. Intra-day and inter-day accuracies were nearly 100%. The method is suitable for screening, quantification and confirmation of MDPV in equine plasma and has been successfully used to detect and confirm the presence of MDPV in equine plasma obtained post-competition.</description><subject>Analysis</subject><subject>Animals</subject><subject>Benzodioxoles - blood</subject><subject>Biological and medical sciences</subject><subject>Chromatography, High Pressure Liquid</subject><subject>Doping in Sports - prevention & control</subject><subject>Drug abuse</subject><subject>General pharmacology</subject><subject>High-Throughput Screening Assays - veterinary</subject><subject>Horses</subject><subject>Mass spectroscopy</subject><subject>Medical sciences</subject><subject>Pharmacology. Drug treatments</subject><subject>Psychotropic Drugs - blood</subject><subject>Pyrrolidines - blood</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Spectrometry, Mass, Electrospray Ionization - methods</subject><subject>Spectrometry, Mass, Electrospray Ionization - veterinary</subject><subject>Stimulants</subject><subject>Substance Abuse Detection - veterinary</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Tandem Mass Spectrometry - veterinary</subject><issn>0146-4760</issn><issn>1945-2403</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2012</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkU1v1DAQhi0EosvChR-AfEFCiLT-ir05VqvyIW1VRNtzNOtMui6JndpJRe78cFztQm_lNNb40ftK8xDylrNjzip5cgvjyfZnYlI-IwteqbIQisnnZMG40oUymh2RVyndMsb1SsuX5EiIciWENgvy-wcMrqHgG3qJPrnR3SM99dDNySUaWio_qeIcx93cocfGhV_zMMdwDx3G4JE6T8_uJpdf3ztIPdDr5PwN3bi8bOh6F0MPY7iJMOzm4irXYE_PISV6OaAd8y-OcX5NXrTQJXxzmEty_fnsav212Fx8-bY-3RRWSi4LrZhRZaUNEysrjMGyNa2RpmqsslYg0xWUShs0EpuSVWILequZbJUQHAHkknzY5w4x3E2Yxrp3yWLXgccwpZoLI3Je7vg_yrg0ulT50EvycY_aGFKK2NZDdD3EOUP1g6A6C6r3gjL87pA7bXts_qF_jWTg_QGAZKFrI3jr0iNXVkIqXj1yYRqeKvwD7vOmlQ</recordid><startdate>20120601</startdate><enddate>20120601</enddate><creator>Wang, Caroline C.</creator><creator>Hartmann-Fischbach, Petra</creator><creator>Krueger, Tim R.</creator><creator>Wells, Terry L.</creator><creator>Feineman, Amy R.</creator><creator>Compton, Joanne C.</creator><general>Oxford University Press</general><general>Preston Publications</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><scope>7U7</scope><scope>C1K</scope></search><sort><creationdate>20120601</creationdate><title>Rapid and Sensitive Analysis of 3,4-Methylenedioxypyrovalerone in Equine Plasma Using Liquid Chromatography-Tandem Mass Spectrometry</title><author>Wang, Caroline C. ; Hartmann-Fischbach, Petra ; Krueger, Tim R. ; Wells, Terry L. ; Feineman, Amy R. ; Compton, Joanne C.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c3313-640745967028c277e5f7f7379dc4cc2e069a5467e73ed5092ba6b603f4221eaa3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2012</creationdate><topic>Analysis</topic><topic>Animals</topic><topic>Benzodioxoles - blood</topic><topic>Biological and medical sciences</topic><topic>Chromatography, High Pressure Liquid</topic><topic>Doping in Sports - prevention & control</topic><topic>Drug abuse</topic><topic>General pharmacology</topic><topic>High-Throughput Screening Assays - veterinary</topic><topic>Horses</topic><topic>Mass spectroscopy</topic><topic>Medical sciences</topic><topic>Pharmacology. Drug treatments</topic><topic>Psychotropic Drugs - blood</topic><topic>Pyrrolidines - blood</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Spectrometry, Mass, Electrospray Ionization - methods</topic><topic>Spectrometry, Mass, Electrospray Ionization - veterinary</topic><topic>Stimulants</topic><topic>Substance Abuse Detection - veterinary</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Tandem Mass Spectrometry - veterinary</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Wang, Caroline C.</creatorcontrib><creatorcontrib>Hartmann-Fischbach, Petra</creatorcontrib><creatorcontrib>Krueger, Tim R.</creatorcontrib><creatorcontrib>Wells, Terry L.</creatorcontrib><creatorcontrib>Feineman, Amy R.</creatorcontrib><creatorcontrib>Compton, Joanne C.</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><collection>Toxicology Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><jtitle>Journal of analytical toxicology</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Wang, Caroline C.</au><au>Hartmann-Fischbach, Petra</au><au>Krueger, Tim R.</au><au>Wells, Terry L.</au><au>Feineman, Amy R.</au><au>Compton, Joanne C.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Rapid and Sensitive Analysis of 3,4-Methylenedioxypyrovalerone in Equine Plasma Using Liquid Chromatography-Tandem Mass Spectrometry</atitle><jtitle>Journal of analytical toxicology</jtitle><addtitle>J Anal Toxicol</addtitle><date>2012-06-01</date><risdate>2012</risdate><volume>36</volume><issue>5</issue><spage>327</spage><epage>333</epage><pages>327-333</pages><issn>0146-4760</issn><eissn>1945-2403</eissn><coden>JATOD3</coden><abstract>3,4-Methylenedioxypyrovalerone (MDPV) is a psychoactive drug with potent stimulant properties and potential for abuse and drug dependency. MDPV was recently classified as a Class I drug by Racing Commissioners International, indicating that it is a banned substance in equine athletes because it lacks therapeutic value in horses. To enforce this ban, a sensitive and fast liquid chromatography-tandem mass spectrometry method was needed. It is for this reason that this method was developed for quantification and confirmation of MDPV in equine plasma. Sample preparation involved liquid-liquid extraction. The analyte was analyzed by a triple-quadrupole linear ion trap mass spectrometer in positive multiple-reaction-monitoring and enhanced product ion scan modes. The method was validated for precision, accuracy, limit of detection (LOD), limit of quantification (LOQ), linearity, stability, extraction recovery, matrix effect, dilution accuracy and selectivity. The extraction recovery was >90%. The linearity range was from 5 to 15,000 pg/mL. LOD and LOQ were 2 and 5 pg/mL, respectively. Intra-day and inter-day accuracies were nearly 100%. The method is suitable for screening, quantification and confirmation of MDPV in equine plasma and has been successfully used to detect and confirm the presence of MDPV in equine plasma obtained post-competition.</abstract><cop>Niles, IL</cop><pub>Oxford University Press</pub><pmid>22582267</pmid><doi>10.1093/jat/bks033</doi><tpages>7</tpages><oa>free_for_read</oa></addata></record> |
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| ispartof | Journal of analytical toxicology, 2012-06, Vol.36 (5), p.327-333 |
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| source | Oxford University Press Journals All Titles (1996-Current); MEDLINE; Elektronische Zeitschriftenbibliothek - Frei zugängliche E-Journals; Alma/SFX Local Collection |
| subjects | Analysis Animals Benzodioxoles - blood Biological and medical sciences Chromatography, High Pressure Liquid Doping in Sports - prevention & control Drug abuse General pharmacology High-Throughput Screening Assays - veterinary Horses Mass spectroscopy Medical sciences Pharmacology. Drug treatments Psychotropic Drugs - blood Pyrrolidines - blood Reproducibility of Results Sensitivity and Specificity Spectrometry, Mass, Electrospray Ionization - methods Spectrometry, Mass, Electrospray Ionization - veterinary Stimulants Substance Abuse Detection - veterinary Tandem Mass Spectrometry - methods Tandem Mass Spectrometry - veterinary |
| title | Rapid and Sensitive Analysis of 3,4-Methylenedioxypyrovalerone in Equine Plasma Using Liquid Chromatography-Tandem Mass Spectrometry |
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