Validation of an LC-MS Method for the Detection and Quantification of BZP and TFMPP and their Hydroxylated Metabolites in Human Plasma and its Application to the Pharmacokinetic Study of TFMPP in Humans
: An LC–MS method was developed for benzylpiperazine (BZP) and trifluoromethylphenylpiperazine (TFMPP), constituents of “party pills” or “legal herbal highs,” and their metabolites in human blood plasma. Compounds were resolved using a mixture of ammonium formate (pH 4.5, 0.01 M) and acetonitrile (...
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Veröffentlicht in: | Journal of forensic sciences 2010-09, Vol.55 (5), p.1311-1318 |
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description | : An LC–MS method was developed for benzylpiperazine (BZP) and trifluoromethylphenylpiperazine (TFMPP), constituents of “party pills” or “legal herbal highs,” and their metabolites in human blood plasma. Compounds were resolved using a mixture of ammonium formate (pH 4.5, 0.01 M) and acetonitrile (flow rate of 1.0 mL/min) with a C18 column. Calibration curves were linear from 1 to 50 ng/mL (R2 > 0.99); the lower limit of quantification (LLOQ) was 5 ng/mL; the accuracy was >90%; the intra‐ and interday relative standard deviations (R.S.D) were |
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Compounds were resolved using a mixture of ammonium formate (pH 4.5, 0.01 M) and acetonitrile (flow rate of 1.0 mL/min) with a C18 column. Calibration curves were linear from 1 to 50 ng/mL (R2 > 0.99); the lower limit of quantification (LLOQ) was 5 ng/mL; the accuracy was >90%; the intra‐ and interday relative standard deviations (R.S.D) were <5% and <10%, respectively. Human plasma concentrations of TFMPP were measured in blood samples taken from healthy adults (n = 6) over 24 h following a 60‐mg oral dose of TFMPP: these peaked at 24.10 ng/mL (±1.8 ng/mL) (Cmax) after 90 min (Tmax). Plasma concentrations of 1‐(3‐trifluoromethyl‐4‐hydroxyphenyl) piperazine peaked at 20.2 ng/mL (±4.6 ng/mL) after 90 min. TFMPP had two disposition phases (t½ = 2.04 h (±0.19 h) and 5.95 h (±1.63 h). Apparent clearance (Cl/F) was 384 L/h (±45 L/h).</description><identifier>ISSN: 0022-1198</identifier><identifier>EISSN: 1556-4029</identifier><identifier>DOI: 10.1111/j.1556-4029.2010.01457.x</identifier><identifier>PMID: 20533987</identifier><identifier>CODEN: JFSCAS</identifier><language>eng</language><publisher>Oxford, UK: Blackwell Publishing Ltd</publisher><subject>Acetonitrile ; Acidity ; Adolescent ; Adult ; Blood ; BZP ; Chromatography, Liquid ; Female ; forensic science ; Forensic sciences ; Forensic Toxicology ; Humans ; liquid chromatography-mass spectrometry ; Male ; Mass Spectrometry ; metabolism ; Metabolites ; pharmacokinetics ; Pharmacology ; Piperazines - blood ; Piperazines - pharmacokinetics ; Piperazines - urine ; Plasma ; Psychotropic drugs ; Specimen Handling ; Street Drugs - blood ; Street Drugs - pharmacokinetics ; Street Drugs - urine ; TFMPP ; toxicology ; Young Adult</subject><ispartof>Journal of forensic sciences, 2010-09, Vol.55 (5), p.1311-1318</ispartof><rights>2010 American Academy of Forensic Sciences</rights><rights>2010 American Academy of Forensic Sciences.</rights><rights>Copyright American Society for Testing and Materials Sep 2010</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c5157-a89fb7703346d2674315c5f29364799015b8da8e8690b722cbbe1781d0712ac23</citedby><cites>FETCH-LOGICAL-c5157-a89fb7703346d2674315c5f29364799015b8da8e8690b722cbbe1781d0712ac23</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1111%2Fj.1556-4029.2010.01457.x$$EPDF$$P50$$Gwiley$$H</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1111%2Fj.1556-4029.2010.01457.x$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>314,780,784,1417,27924,27925,45574,45575</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/20533987$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Antia, Ushtana</creatorcontrib><creatorcontrib>Tingle, Malcolm D.</creatorcontrib><creatorcontrib>Russell, Bruce R.</creatorcontrib><title>Validation of an LC-MS Method for the Detection and Quantification of BZP and TFMPP and their Hydroxylated Metabolites in Human Plasma and its Application to the Pharmacokinetic Study of TFMPP in Humans</title><title>Journal of forensic sciences</title><addtitle>J Forensic Sci</addtitle><description>: An LC–MS method was developed for benzylpiperazine (BZP) and trifluoromethylphenylpiperazine (TFMPP), constituents of “party pills” or “legal herbal highs,” and their metabolites in human blood plasma. Compounds were resolved using a mixture of ammonium formate (pH 4.5, 0.01 M) and acetonitrile (flow rate of 1.0 mL/min) with a C18 column. Calibration curves were linear from 1 to 50 ng/mL (R2 > 0.99); the lower limit of quantification (LLOQ) was 5 ng/mL; the accuracy was >90%; the intra‐ and interday relative standard deviations (R.S.D) were <5% and <10%, respectively. Human plasma concentrations of TFMPP were measured in blood samples taken from healthy adults (n = 6) over 24 h following a 60‐mg oral dose of TFMPP: these peaked at 24.10 ng/mL (±1.8 ng/mL) (Cmax) after 90 min (Tmax). Plasma concentrations of 1‐(3‐trifluoromethyl‐4‐hydroxyphenyl) piperazine peaked at 20.2 ng/mL (±4.6 ng/mL) after 90 min. TFMPP had two disposition phases (t½ = 2.04 h (±0.19 h) and 5.95 h (±1.63 h). Apparent clearance (Cl/F) was 384 L/h (±45 L/h).</description><subject>Acetonitrile</subject><subject>Acidity</subject><subject>Adolescent</subject><subject>Adult</subject><subject>Blood</subject><subject>BZP</subject><subject>Chromatography, Liquid</subject><subject>Female</subject><subject>forensic science</subject><subject>Forensic sciences</subject><subject>Forensic Toxicology</subject><subject>Humans</subject><subject>liquid chromatography-mass spectrometry</subject><subject>Male</subject><subject>Mass Spectrometry</subject><subject>metabolism</subject><subject>Metabolites</subject><subject>pharmacokinetics</subject><subject>Pharmacology</subject><subject>Piperazines - blood</subject><subject>Piperazines - pharmacokinetics</subject><subject>Piperazines - urine</subject><subject>Plasma</subject><subject>Psychotropic drugs</subject><subject>Specimen Handling</subject><subject>Street Drugs - blood</subject><subject>Street Drugs - pharmacokinetics</subject><subject>Street Drugs - urine</subject><subject>TFMPP</subject><subject>toxicology</subject><subject>Young Adult</subject><issn>0022-1198</issn><issn>1556-4029</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2010</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqNUk1v0zAYjhCIlcFfQBYXTulsJ_7IgcPW0RXUsqINkLhYTuKo7pK42I5o_-J-FU6y9sAFfPErv8-H7feJIoDgFIV1sZ0iQmicQpxNMQynEKWETffPosmp8TyaQIhxjFDGz6JXzm0hhBRR9DI6w5AkScbZJHr8LmtdSq9NC0wFZAuWs3h1B1bKb0wJKmOB3yhwrbwqBpBsS_C1k63XlS5OvKuf66FzP1-txyqwtAWLQ2nN_lBLr8peU-am1l45oFuw6Jpgt66la-RA0d6By92uPup6M3ivN9I2sjAPulVeF-DOd-WhNx3NjkrudfSikrVTb5728-jb_OP9bBEvb28-zS6XcUEQYbHkWZUzBpMkpSWmLE0QKUiFs4SmLMsgIjkvJVecZjBnGBd5rhDjqIQMYVng5Dx6P-rurPnVKedFo12h6lq2ynROcMgwDx8M_4lkFFOe0gH57i_k1nS2Dc8QjKRJSiBlAcRHUGGNc1ZVYmd1I-1BICj6XIit6Mcv-vGLPhdiyIXYB-rbJ_0ub1R5Ih6DEAAfRsBvXavDfwuLz_Pbvgr8eORr59X-xJf2QYSbMyJ-fLkRlKxZen2ViVXyB7yB1Fg</recordid><startdate>201009</startdate><enddate>201009</enddate><creator>Antia, Ushtana</creator><creator>Tingle, Malcolm D.</creator><creator>Russell, Bruce R.</creator><general>Blackwell Publishing Ltd</general><general>Wiley Subscription Services, Inc</general><scope>BSCLL</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>K7.</scope><scope>7X8</scope><scope>7U7</scope><scope>C1K</scope></search><sort><creationdate>201009</creationdate><title>Validation of an LC-MS Method for the Detection and Quantification of BZP and TFMPP and their Hydroxylated Metabolites in Human Plasma and its Application to the Pharmacokinetic Study of TFMPP in Humans</title><author>Antia, Ushtana ; Tingle, Malcolm D. ; Russell, Bruce R.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c5157-a89fb7703346d2674315c5f29364799015b8da8e8690b722cbbe1781d0712ac23</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2010</creationdate><topic>Acetonitrile</topic><topic>Acidity</topic><topic>Adolescent</topic><topic>Adult</topic><topic>Blood</topic><topic>BZP</topic><topic>Chromatography, Liquid</topic><topic>Female</topic><topic>forensic science</topic><topic>Forensic sciences</topic><topic>Forensic Toxicology</topic><topic>Humans</topic><topic>liquid chromatography-mass spectrometry</topic><topic>Male</topic><topic>Mass Spectrometry</topic><topic>metabolism</topic><topic>Metabolites</topic><topic>pharmacokinetics</topic><topic>Pharmacology</topic><topic>Piperazines - blood</topic><topic>Piperazines - pharmacokinetics</topic><topic>Piperazines - urine</topic><topic>Plasma</topic><topic>Psychotropic drugs</topic><topic>Specimen Handling</topic><topic>Street Drugs - blood</topic><topic>Street Drugs - pharmacokinetics</topic><topic>Street Drugs - urine</topic><topic>TFMPP</topic><topic>toxicology</topic><topic>Young Adult</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Antia, Ushtana</creatorcontrib><creatorcontrib>Tingle, Malcolm D.</creatorcontrib><creatorcontrib>Russell, Bruce R.</creatorcontrib><collection>Istex</collection><collection>Medline</collection><collection>MEDLINE</collection><collection>MEDLINE (Ovid)</collection><collection>MEDLINE</collection><collection>MEDLINE</collection><collection>PubMed</collection><collection>CrossRef</collection><collection>ProQuest Criminal Justice (Alumni)</collection><collection>MEDLINE - Academic</collection><collection>Toxicology Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><jtitle>Journal of forensic sciences</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Antia, Ushtana</au><au>Tingle, Malcolm D.</au><au>Russell, Bruce R.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Validation of an LC-MS Method for the Detection and Quantification of BZP and TFMPP and their Hydroxylated Metabolites in Human Plasma and its Application to the Pharmacokinetic Study of TFMPP in Humans</atitle><jtitle>Journal of forensic sciences</jtitle><addtitle>J Forensic Sci</addtitle><date>2010-09</date><risdate>2010</risdate><volume>55</volume><issue>5</issue><spage>1311</spage><epage>1318</epage><pages>1311-1318</pages><issn>0022-1198</issn><eissn>1556-4029</eissn><coden>JFSCAS</coden><abstract>: An LC–MS method was developed for benzylpiperazine (BZP) and trifluoromethylphenylpiperazine (TFMPP), constituents of “party pills” or “legal herbal highs,” and their metabolites in human blood plasma. Compounds were resolved using a mixture of ammonium formate (pH 4.5, 0.01 M) and acetonitrile (flow rate of 1.0 mL/min) with a C18 column. Calibration curves were linear from 1 to 50 ng/mL (R2 > 0.99); the lower limit of quantification (LLOQ) was 5 ng/mL; the accuracy was >90%; the intra‐ and interday relative standard deviations (R.S.D) were <5% and <10%, respectively. Human plasma concentrations of TFMPP were measured in blood samples taken from healthy adults (n = 6) over 24 h following a 60‐mg oral dose of TFMPP: these peaked at 24.10 ng/mL (±1.8 ng/mL) (Cmax) after 90 min (Tmax). Plasma concentrations of 1‐(3‐trifluoromethyl‐4‐hydroxyphenyl) piperazine peaked at 20.2 ng/mL (±4.6 ng/mL) after 90 min. TFMPP had two disposition phases (t½ = 2.04 h (±0.19 h) and 5.95 h (±1.63 h). 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subjects | Acetonitrile Acidity Adolescent Adult Blood BZP Chromatography, Liquid Female forensic science Forensic sciences Forensic Toxicology Humans liquid chromatography-mass spectrometry Male Mass Spectrometry metabolism Metabolites pharmacokinetics Pharmacology Piperazines - blood Piperazines - pharmacokinetics Piperazines - urine Plasma Psychotropic drugs Specimen Handling Street Drugs - blood Street Drugs - pharmacokinetics Street Drugs - urine TFMPP toxicology Young Adult |
title | Validation of an LC-MS Method for the Detection and Quantification of BZP and TFMPP and their Hydroxylated Metabolites in Human Plasma and its Application to the Pharmacokinetic Study of TFMPP in Humans |
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