Determination of Buprenorphine and Norbuprenorphine in Whole Blood by Liquid Chromatography-Mass Spectrometry
A sensitive and highly specific method for the determination of buprenorphine and norbuprenorphine in postmortem and hemolyzed whole blood using combined liquid chromatography and mass spectrometry (LC-MS) with electrospray ionization was developed. After enzymatic hydrolysis and deproteinization wi...
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Veröffentlicht in: | Journal of analytical toxicology 1997-03, Vol.21 (2), p.160-165 |
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creator | Hoja, Harald Marquet, Pierre Verneuil, Bernard Lotfi, Hayat Dupuy, Jean-Louis Lachâtre, Gérard |
description | A sensitive and highly specific method for the determination of buprenorphine and norbuprenorphine in postmortem and hemolyzed whole blood using combined liquid chromatography and mass spectrometry (LC-MS) with electrospray ionization was developed. After enzymatic hydrolysis and deproteinization with acetonitrile, Extrelut-3 cartridges were used for a preliminary basic sample cleanup. Elution by toluene-ether (50:50, v/v) was followed by an acid wash with 0.05M H3PO4 and a basic re-extraction into ether. A Nucleosil C18 (150 × 1-mm i.d.) reversed-phase column was used for the chromatographic separation together with a mixture of 2mM ammonium formate buffer (pH 3) and acetonitrile (55:45, v/v) as the mobile phase. Recoveries were between 56 and 60%, and detection limits were 0.05 ng/mL for both analytes. The coefficient of variation for repeatability was lower than 4%. Limits of quantitation were 0.1 ng/mL for buprenorphine and norbuprenorphine. Reproducibility was good, and linearity was excellent in the range of 0.1 to 100 ng/mL (r > 0.9999, n = 7). |
doi_str_mv | 10.1093/jat/21.2.160 |
format | Article |
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After enzymatic hydrolysis and deproteinization with acetonitrile, Extrelut-3 cartridges were used for a preliminary basic sample cleanup. Elution by toluene-ether (50:50, v/v) was followed by an acid wash with 0.05M H3PO4 and a basic re-extraction into ether. A Nucleosil C18 (150 × 1-mm i.d.) reversed-phase column was used for the chromatographic separation together with a mixture of 2mM ammonium formate buffer (pH 3) and acetonitrile (55:45, v/v) as the mobile phase. Recoveries were between 56 and 60%, and detection limits were 0.05 ng/mL for both analytes. The coefficient of variation for repeatability was lower than 4%. Limits of quantitation were 0.1 ng/mL for buprenorphine and norbuprenorphine. Reproducibility was good, and linearity was excellent in the range of 0.1 to 100 ng/mL (r > 0.9999, n = 7).</description><identifier>ISSN: 0146-4760</identifier><identifier>EISSN: 1945-2403</identifier><identifier>DOI: 10.1093/jat/21.2.160</identifier><identifier>PMID: 9083835</identifier><identifier>CODEN: JATOD3</identifier><language>eng</language><publisher>Niles, IL: Oxford University Press</publisher><subject>Adult ; Biological and medical sciences ; Buprenorphine - analogs & derivatives ; Buprenorphine - blood ; Buprenorphine - urine ; Chromatography, Liquid ; Drug addictions ; Humans ; Male ; Mass Spectrometry ; Medical sciences ; Narcotics - blood ; Narcotics - urine ; Reproducibility of Results ; Sensitivity and Specificity ; Toxicology</subject><ispartof>Journal of analytical toxicology, 1997-03, Vol.21 (2), p.160-165</ispartof><rights>1997</rights><rights>1997 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c441t-3b247492d1d767cc7d9ae19e0abbbf15eaf55a53d4658c4613f93399dae72a803</citedby></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>314,780,784,1584,27924,27925</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=2606057$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/9083835$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Hoja, Harald</creatorcontrib><creatorcontrib>Marquet, Pierre</creatorcontrib><creatorcontrib>Verneuil, Bernard</creatorcontrib><creatorcontrib>Lotfi, Hayat</creatorcontrib><creatorcontrib>Dupuy, Jean-Louis</creatorcontrib><creatorcontrib>Lachâtre, Gérard</creatorcontrib><title>Determination of Buprenorphine and Norbuprenorphine in Whole Blood by Liquid Chromatography-Mass Spectrometry</title><title>Journal of analytical toxicology</title><addtitle>Journal of Analytical Toxicology</addtitle><addtitle>Journal of Analytical Toxicology</addtitle><description>A sensitive and highly specific method for the determination of buprenorphine and norbuprenorphine in postmortem and hemolyzed whole blood using combined liquid chromatography and mass spectrometry (LC-MS) with electrospray ionization was developed. After enzymatic hydrolysis and deproteinization with acetonitrile, Extrelut-3 cartridges were used for a preliminary basic sample cleanup. Elution by toluene-ether (50:50, v/v) was followed by an acid wash with 0.05M H3PO4 and a basic re-extraction into ether. A Nucleosil C18 (150 × 1-mm i.d.) reversed-phase column was used for the chromatographic separation together with a mixture of 2mM ammonium formate buffer (pH 3) and acetonitrile (55:45, v/v) as the mobile phase. Recoveries were between 56 and 60%, and detection limits were 0.05 ng/mL for both analytes. The coefficient of variation for repeatability was lower than 4%. Limits of quantitation were 0.1 ng/mL for buprenorphine and norbuprenorphine. Reproducibility was good, and linearity was excellent in the range of 0.1 to 100 ng/mL (r > 0.9999, n = 7).</description><subject>Adult</subject><subject>Biological and medical sciences</subject><subject>Buprenorphine - analogs & derivatives</subject><subject>Buprenorphine - blood</subject><subject>Buprenorphine - urine</subject><subject>Chromatography, Liquid</subject><subject>Drug addictions</subject><subject>Humans</subject><subject>Male</subject><subject>Mass Spectrometry</subject><subject>Medical sciences</subject><subject>Narcotics - blood</subject><subject>Narcotics - urine</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Toxicology</subject><issn>0146-4760</issn><issn>1945-2403</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1997</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqF0U1v00AQBuAVApVQuHFF2gOiF5zu98eRpNAgBTgUVMRlNbbXZIvtdXdtifx7XCWKxKmnkWYezUjzIvSakiUlll_ewXjJ6JItqSJP0IJaIQsmCH-KFoQKVQityHP0Iuc7Qqgyip-hM0sMN1wuUHflR5-60MMYYo9jg1fTkHwf07ALvcfQ1_hrTOV_zdDj211sPV61Mda43ONtuJ9Cjde7FDsY4-8Ew25ffIGc8c3gq3Fu-zHtX6JnDbTZvzrWc_Tj08fv602x_Xb9ef1hW1RC0LHgJRNaWFbTWitdVbq24Kn1BMqybKj00EgJktdCSVMJRXljObe2Bq8ZGMLP0bvD3iHF-8nn0XUhV75tofdxyk4bY5mR8lFIpTXWKDbD9wdYpZhz8o0bUugg7R0l7iEGN8fgGHXMzTHM_M1x71R2vj7h49_n-dvjHHIFbZOgr0I-MaaIIlLP7OLA4jQ8drA4yJBH__dkIf1xSnMt3ebnL3dL5OZmZZRT_B-lO61R</recordid><startdate>19970301</startdate><enddate>19970301</enddate><creator>Hoja, Harald</creator><creator>Marquet, Pierre</creator><creator>Verneuil, Bernard</creator><creator>Lotfi, Hayat</creator><creator>Dupuy, Jean-Louis</creator><creator>Lachâtre, Gérard</creator><general>Oxford University Press</general><general>Preston</general><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>7U7</scope><scope>C1K</scope><scope>7X8</scope></search><sort><creationdate>19970301</creationdate><title>Determination of Buprenorphine and Norbuprenorphine in Whole Blood by Liquid Chromatography-Mass Spectrometry</title><author>Hoja, Harald ; Marquet, Pierre ; Verneuil, Bernard ; Lotfi, Hayat ; Dupuy, Jean-Louis ; Lachâtre, Gérard</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c441t-3b247492d1d767cc7d9ae19e0abbbf15eaf55a53d4658c4613f93399dae72a803</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1997</creationdate><topic>Adult</topic><topic>Biological and medical sciences</topic><topic>Buprenorphine - analogs & derivatives</topic><topic>Buprenorphine - blood</topic><topic>Buprenorphine - urine</topic><topic>Chromatography, Liquid</topic><topic>Drug addictions</topic><topic>Humans</topic><topic>Male</topic><topic>Mass Spectrometry</topic><topic>Medical sciences</topic><topic>Narcotics - blood</topic><topic>Narcotics - urine</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Toxicology</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Hoja, Harald</creatorcontrib><creatorcontrib>Marquet, Pierre</creatorcontrib><creatorcontrib>Verneuil, Bernard</creatorcontrib><creatorcontrib>Lotfi, Hayat</creatorcontrib><creatorcontrib>Dupuy, Jean-Louis</creatorcontrib><creatorcontrib>Lachâtre, Gérard</creatorcontrib><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>Toxicology Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><collection>MEDLINE - Academic</collection><jtitle>Journal of analytical toxicology</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Hoja, Harald</au><au>Marquet, Pierre</au><au>Verneuil, Bernard</au><au>Lotfi, Hayat</au><au>Dupuy, Jean-Louis</au><au>Lachâtre, Gérard</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Determination of Buprenorphine and Norbuprenorphine in Whole Blood by Liquid Chromatography-Mass Spectrometry</atitle><jtitle>Journal of analytical toxicology</jtitle><stitle>Journal of Analytical Toxicology</stitle><addtitle>Journal of Analytical Toxicology</addtitle><date>1997-03-01</date><risdate>1997</risdate><volume>21</volume><issue>2</issue><spage>160</spage><epage>165</epage><pages>160-165</pages><issn>0146-4760</issn><eissn>1945-2403</eissn><coden>JATOD3</coden><abstract>A sensitive and highly specific method for the determination of buprenorphine and norbuprenorphine in postmortem and hemolyzed whole blood using combined liquid chromatography and mass spectrometry (LC-MS) with electrospray ionization was developed. After enzymatic hydrolysis and deproteinization with acetonitrile, Extrelut-3 cartridges were used for a preliminary basic sample cleanup. Elution by toluene-ether (50:50, v/v) was followed by an acid wash with 0.05M H3PO4 and a basic re-extraction into ether. A Nucleosil C18 (150 × 1-mm i.d.) reversed-phase column was used for the chromatographic separation together with a mixture of 2mM ammonium formate buffer (pH 3) and acetonitrile (55:45, v/v) as the mobile phase. Recoveries were between 56 and 60%, and detection limits were 0.05 ng/mL for both analytes. The coefficient of variation for repeatability was lower than 4%. Limits of quantitation were 0.1 ng/mL for buprenorphine and norbuprenorphine. Reproducibility was good, and linearity was excellent in the range of 0.1 to 100 ng/mL (r > 0.9999, n = 7).</abstract><cop>Niles, IL</cop><pub>Oxford University Press</pub><pmid>9083835</pmid><doi>10.1093/jat/21.2.160</doi><tpages>6</tpages></addata></record> |
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source | MEDLINE; Oxford University Press Journals All Titles (1996-Current); EZB-FREE-00999 freely available EZB journals; Alma/SFX Local Collection |
subjects | Adult Biological and medical sciences Buprenorphine - analogs & derivatives Buprenorphine - blood Buprenorphine - urine Chromatography, Liquid Drug addictions Humans Male Mass Spectrometry Medical sciences Narcotics - blood Narcotics - urine Reproducibility of Results Sensitivity and Specificity Toxicology |
title | Determination of Buprenorphine and Norbuprenorphine in Whole Blood by Liquid Chromatography-Mass Spectrometry |
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