Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold
► We developed a fully automated method for total captopril. ► Total captopril was determined in human urine. ► Sequential injection was coupled to liquid chromatography. ► Sample preparation was carried out on-line. ► Captopril was determined after post column derivatization. The present study repo...
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| Veröffentlicht in: | Talanta (Oxford) 2012-01, Vol.88, p.561-566 |
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| creator | Karakosta, Theano D. Tzanavaras, Paraskevas D. Themelis, Demetrius G. |
| description | ► We developed a fully automated method for total captopril. ► Total captopril was determined in human urine. ► Sequential injection was coupled to liquid chromatography. ► Sample preparation was carried out on-line. ► Captopril was determined after post column derivatization.
The present study reports a new liquid chromatographic (HPLC) method for the determination of the anti-hypertension drug captopril (CAP) in human urine. After its separation from the sample matrix in a reversed phase HPLC column, CAP reacts with the thiol-selective reagent ethyl-propiolate (EP) in a post-column configuration and the formed thioacrylate derivative is detected at 285nm. Automated 4-fold preconcentration of the analyte prior to analysis was achieved by an on-line solid phase extraction (SPE) step using a sequential injection (SI) manifold. The Oasis HLB SPE cartridges offered quantitative recoveries and effective sample cleaning by applying a simple SPE protocol. The limits of detection and quantitation were 10μgL−1 and 35μgL−1 respectively. The percent recoveries for the analysis of human urine samples ranged between 90 and 96% and 95 and 104% using aqueous and matrix matched calibration curves respectively. |
| doi_str_mv | 10.1016/j.talanta.2011.11.034 |
| format | Article |
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The present study reports a new liquid chromatographic (HPLC) method for the determination of the anti-hypertension drug captopril (CAP) in human urine. After its separation from the sample matrix in a reversed phase HPLC column, CAP reacts with the thiol-selective reagent ethyl-propiolate (EP) in a post-column configuration and the formed thioacrylate derivative is detected at 285nm. Automated 4-fold preconcentration of the analyte prior to analysis was achieved by an on-line solid phase extraction (SPE) step using a sequential injection (SI) manifold. The Oasis HLB SPE cartridges offered quantitative recoveries and effective sample cleaning by applying a simple SPE protocol. The limits of detection and quantitation were 10μgL−1 and 35μgL−1 respectively. The percent recoveries for the analysis of human urine samples ranged between 90 and 96% and 95 and 104% using aqueous and matrix matched calibration curves respectively.</description><identifier>ISSN: 0039-9140</identifier><identifier>EISSN: 1873-3573</identifier><identifier>DOI: 10.1016/j.talanta.2011.11.034</identifier><identifier>PMID: 22265541</identifier><identifier>CODEN: TLNTA2</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Acrylates - analysis ; Alkynes - chemistry ; Analytical chemistry ; Antihypertensive Agents - urine ; Automated solid phase extraction ; Automation, Laboratory ; Calibration ; Captopril ; Captopril - urine ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Chromatography, High Pressure Liquid - methods ; Ethyl propiolate ; Exact sciences and technology ; Extraction ; Flow Injection Analysis ; Human ; Human urine ; Humans ; Manifolds ; On-line systems ; Other chromatographic methods ; Post-column derivatization ; Propionates - chemistry ; Recovery ; Reproducibility of Results ; Sensitivity and Specificity ; Solid Phase Extraction ; Solid phases ; Urine</subject><ispartof>Talanta (Oxford), 2012-01, Vol.88, p.561-566</ispartof><rights>2011 Elsevier B.V.</rights><rights>2015 INIST-CNRS</rights><rights>Copyright © 2011 Elsevier B.V. All rights reserved.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c427t-13bbd145edb30cf37ff73e21953413e4f08f830052c85c27f7850938e66890083</citedby><cites>FETCH-LOGICAL-c427t-13bbd145edb30cf37ff73e21953413e4f08f830052c85c27f7850938e66890083</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S0039914011010162$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=25652525$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/22265541$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Karakosta, Theano D.</creatorcontrib><creatorcontrib>Tzanavaras, Paraskevas D.</creatorcontrib><creatorcontrib>Themelis, Demetrius G.</creatorcontrib><title>Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold</title><title>Talanta (Oxford)</title><addtitle>Talanta</addtitle><description>► We developed a fully automated method for total captopril. ► Total captopril was determined in human urine. ► Sequential injection was coupled to liquid chromatography. ► Sample preparation was carried out on-line. ► Captopril was determined after post column derivatization.
The present study reports a new liquid chromatographic (HPLC) method for the determination of the anti-hypertension drug captopril (CAP) in human urine. After its separation from the sample matrix in a reversed phase HPLC column, CAP reacts with the thiol-selective reagent ethyl-propiolate (EP) in a post-column configuration and the formed thioacrylate derivative is detected at 285nm. Automated 4-fold preconcentration of the analyte prior to analysis was achieved by an on-line solid phase extraction (SPE) step using a sequential injection (SI) manifold. The Oasis HLB SPE cartridges offered quantitative recoveries and effective sample cleaning by applying a simple SPE protocol. The limits of detection and quantitation were 10μgL−1 and 35μgL−1 respectively. The percent recoveries for the analysis of human urine samples ranged between 90 and 96% and 95 and 104% using aqueous and matrix matched calibration curves respectively.</description><subject>Acrylates - analysis</subject><subject>Alkynes - chemistry</subject><subject>Analytical chemistry</subject><subject>Antihypertensive Agents - urine</subject><subject>Automated solid phase extraction</subject><subject>Automation, Laboratory</subject><subject>Calibration</subject><subject>Captopril</subject><subject>Captopril - urine</subject><subject>Chemistry</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Ethyl propiolate</subject><subject>Exact sciences and technology</subject><subject>Extraction</subject><subject>Flow Injection Analysis</subject><subject>Human</subject><subject>Human urine</subject><subject>Humans</subject><subject>Manifolds</subject><subject>On-line systems</subject><subject>Other chromatographic methods</subject><subject>Post-column derivatization</subject><subject>Propionates - chemistry</subject><subject>Recovery</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Solid Phase Extraction</subject><subject>Solid phases</subject><subject>Urine</subject><issn>0039-9140</issn><issn>1873-3573</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2012</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkc2OFCEUhYnROD2tj6BhY3RTLRRF_azMZKKjySRudF2hqYtNh4IaoEbbN_PtvGW1utNAwoLvnnNzDiHPONtxxuvXx11WTvmsdiXjfIeXieoB2fC2EYWQjXhINoyJruh4xS7IZUpHxlgpmHhMLsqyrKWs-Ib8uJpzGFWGgQ6QIY7Wq2yDp8HQHNCCajXlMEXrqPV0jtYD3Z-os3ezHag-xGU6fIlqOpzoV5sPdAopFzq4efSoGe09Cn5fRXWYJ4dWOdDgC7dopeBQZzqoBBS-5aj0LxK9FE1wN4PPVi3eR1h_RuWtCW54Qh4Z5RI8Pb9b8vnd20_X74vbjzcfrq9uC12VTS642O8HXkkY9oJpIxpjGgEl76SouIDKsNa0gjFZ6lbqsjFNK1knWqjrtmOsFVvyctWdYsB1Uu5HmzQ4DB_CnPqON7KppFjIV_8ksTfWsUYgvCVyRXUMKUUwPSY8qnhCaOHq_tif--2Xfnu82C_OPT9bzPsRhj9TvwtF4MUZUEkrZ6Ly2qa_nKxliQe5NysHGN29hdgnbcFrGGzEoPsh2P-s8hP_D8pu</recordid><startdate>20120115</startdate><enddate>20120115</enddate><creator>Karakosta, Theano D.</creator><creator>Tzanavaras, Paraskevas D.</creator><creator>Themelis, Demetrius G.</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>7QQ</scope><scope>7SR</scope><scope>8FD</scope><scope>JG9</scope><scope>7X8</scope></search><sort><creationdate>20120115</creationdate><title>Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold</title><author>Karakosta, Theano D. ; Tzanavaras, Paraskevas D. ; Themelis, Demetrius G.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c427t-13bbd145edb30cf37ff73e21953413e4f08f830052c85c27f7850938e66890083</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2012</creationdate><topic>Acrylates - analysis</topic><topic>Alkynes - chemistry</topic><topic>Analytical chemistry</topic><topic>Antihypertensive Agents - urine</topic><topic>Automated solid phase extraction</topic><topic>Automation, Laboratory</topic><topic>Calibration</topic><topic>Captopril</topic><topic>Captopril - urine</topic><topic>Chemistry</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Ethyl propiolate</topic><topic>Exact sciences and technology</topic><topic>Extraction</topic><topic>Flow Injection Analysis</topic><topic>Human</topic><topic>Human urine</topic><topic>Humans</topic><topic>Manifolds</topic><topic>On-line systems</topic><topic>Other chromatographic methods</topic><topic>Post-column derivatization</topic><topic>Propionates - chemistry</topic><topic>Recovery</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Solid Phase Extraction</topic><topic>Solid phases</topic><topic>Urine</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Karakosta, Theano D.</creatorcontrib><creatorcontrib>Tzanavaras, Paraskevas D.</creatorcontrib><creatorcontrib>Themelis, Demetrius G.</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>Ceramic Abstracts</collection><collection>Engineered Materials Abstracts</collection><collection>Technology Research Database</collection><collection>Materials Research Database</collection><collection>MEDLINE - Academic</collection><jtitle>Talanta (Oxford)</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Karakosta, Theano D.</au><au>Tzanavaras, Paraskevas D.</au><au>Themelis, Demetrius G.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold</atitle><jtitle>Talanta (Oxford)</jtitle><addtitle>Talanta</addtitle><date>2012-01-15</date><risdate>2012</risdate><volume>88</volume><spage>561</spage><epage>566</epage><pages>561-566</pages><issn>0039-9140</issn><eissn>1873-3573</eissn><coden>TLNTA2</coden><abstract>► We developed a fully automated method for total captopril. ► Total captopril was determined in human urine. ► Sequential injection was coupled to liquid chromatography. ► Sample preparation was carried out on-line. ► Captopril was determined after post column derivatization.
The present study reports a new liquid chromatographic (HPLC) method for the determination of the anti-hypertension drug captopril (CAP) in human urine. After its separation from the sample matrix in a reversed phase HPLC column, CAP reacts with the thiol-selective reagent ethyl-propiolate (EP) in a post-column configuration and the formed thioacrylate derivative is detected at 285nm. Automated 4-fold preconcentration of the analyte prior to analysis was achieved by an on-line solid phase extraction (SPE) step using a sequential injection (SI) manifold. The Oasis HLB SPE cartridges offered quantitative recoveries and effective sample cleaning by applying a simple SPE protocol. The limits of detection and quantitation were 10μgL−1 and 35μgL−1 respectively. The percent recoveries for the analysis of human urine samples ranged between 90 and 96% and 95 and 104% using aqueous and matrix matched calibration curves respectively.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>22265541</pmid><doi>10.1016/j.talanta.2011.11.034</doi><tpages>6</tpages></addata></record> |
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| subjects | Acrylates - analysis Alkynes - chemistry Analytical chemistry Antihypertensive Agents - urine Automated solid phase extraction Automation, Laboratory Calibration Captopril Captopril - urine Chemistry Chromatographic methods and physical methods associated with chromatography Chromatography, High Pressure Liquid - methods Ethyl propiolate Exact sciences and technology Extraction Flow Injection Analysis Human Human urine Humans Manifolds On-line systems Other chromatographic methods Post-column derivatization Propionates - chemistry Recovery Reproducibility of Results Sensitivity and Specificity Solid Phase Extraction Solid phases Urine |
| title | Automated determination of total captopril in urine by liquid chromatography with post-column derivatization coupled to on-line solid phase extraction in a sequential injection manifold |
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