Direct coupled column separation and determination of the diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine
A reversed‐phase coupled column separation (CCS) system for the analysis of two diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine is described. After direct injection of urine samples (50 μl) the glucuronides were isolated by complex formation on a terbiu...
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Veröffentlicht in: | Chirality (New York, N.Y.) N.Y.), 1992, Vol.4 (8), p.509-514 |
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description | A reversed‐phase coupled column separation (CCS) system for the analysis of two diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine is described. After direct injection of urine samples (50 μl) the glucuronides were isolated by complex formation on a terbium(III) loaded strong cation exchanger at alkaline pH. The solutes were eluted from the precolumn by an acidic mobile phase, enriched and separated on Hypercarb (porous graphitic carbon) as analytical column with 0.1 M acetic acid pH 2.8 and 30% acetonitrile as mobile phase. The calibration graph was linear (r2 = 0.9999) and the detection limits were in the low picomole (UV) or femtomole (fluorescence) range. Optimization of the analytical column revealed that elution order and selectivity for the glucuronides were dependent on the buffer agent and temperature used. By appropriate choice of mobile phase conditions all four diastereomers could be separated. © 1992 Wiley‐Liss, Inc. |
doi_str_mv | 10.1002/chir.530040809 |
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After direct injection of urine samples (50 μl) the glucuronides were isolated by complex formation on a terbium(III) loaded strong cation exchanger at alkaline pH. The solutes were eluted from the precolumn by an acidic mobile phase, enriched and separated on Hypercarb (porous graphitic carbon) as analytical column with 0.1 M acetic acid pH 2.8 and 30% acetonitrile as mobile phase. The calibration graph was linear (r2 = 0.9999) and the detection limits were in the low picomole (UV) or femtomole (fluorescence) range. Optimization of the analytical column revealed that elution order and selectivity for the glucuronides were dependent on the buffer agent and temperature used. By appropriate choice of mobile phase conditions all four diastereomers could be separated. © 1992 Wiley‐Liss, Inc.</description><identifier>ISSN: 0899-0042</identifier><identifier>EISSN: 1520-636X</identifier><identifier>DOI: 10.1002/chir.530040809</identifier><identifier>PMID: 1476861</identifier><identifier>CODEN: CHRLEP</identifier><language>eng</language><publisher>New York: Alan R. Liss, Inc</publisher><subject>almokalant glucuronides ; Analysis ; Anti-Arrhythmia Agents - chemistry ; Anti-Arrhythmia Agents - classification ; Anti-Arrhythmia Agents - urine ; bioanalysis ; Biological and medical sciences ; Buffers ; Chromatography, Ion Exchange - instrumentation ; Chromatography, Ion Exchange - methods ; Chromatography, Ion Exchange - statistics & numerical data ; diastereomers ; General pharmacology ; Glucuronates - chemistry ; Glucuronates - urine ; Humans ; Medical sciences ; metal complexes ; Pharmacology. Drug treatments ; porous graphitic carbon ; Propanolamines - chemistry ; Propanolamines - urine ; Reproducibility of Results ; Sensitivity and Specificity ; Stereoisomerism ; Temperature</subject><ispartof>Chirality (New York, N.Y.), 1992, Vol.4 (8), p.509-514</ispartof><rights>Copyright © 1992 Wiley‐Liss, Inc.</rights><rights>1993 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c4079-39603361ffc96617eae2ea6532af4501c9264b4c29b9eac31208a2eac58b9caa3</citedby><cites>FETCH-LOGICAL-c4079-39603361ffc96617eae2ea6532af4501c9264b4c29b9eac31208a2eac58b9caa3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1002%2Fchir.530040809$$EPDF$$P50$$Gwiley$$H</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1002%2Fchir.530040809$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>314,778,782,1414,4012,27906,27907,27908,45557,45558</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=4524581$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/1476861$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Stefansson, Morgan</creatorcontrib><creatorcontrib>Hoffmann, Kurt-Jürgen</creatorcontrib><title>Direct coupled column separation and determination of the diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine</title><title>Chirality (New York, N.Y.)</title><addtitle>Chirality</addtitle><description>A reversed‐phase coupled column separation (CCS) system for the analysis of two diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine is described. After direct injection of urine samples (50 μl) the glucuronides were isolated by complex formation on a terbium(III) loaded strong cation exchanger at alkaline pH. The solutes were eluted from the precolumn by an acidic mobile phase, enriched and separated on Hypercarb (porous graphitic carbon) as analytical column with 0.1 M acetic acid pH 2.8 and 30% acetonitrile as mobile phase. The calibration graph was linear (r2 = 0.9999) and the detection limits were in the low picomole (UV) or femtomole (fluorescence) range. Optimization of the analytical column revealed that elution order and selectivity for the glucuronides were dependent on the buffer agent and temperature used. By appropriate choice of mobile phase conditions all four diastereomers could be separated. © 1992 Wiley‐Liss, Inc.</description><subject>almokalant glucuronides</subject><subject>Analysis</subject><subject>Anti-Arrhythmia Agents - chemistry</subject><subject>Anti-Arrhythmia Agents - classification</subject><subject>Anti-Arrhythmia Agents - urine</subject><subject>bioanalysis</subject><subject>Biological and medical sciences</subject><subject>Buffers</subject><subject>Chromatography, Ion Exchange - instrumentation</subject><subject>Chromatography, Ion Exchange - methods</subject><subject>Chromatography, Ion Exchange - statistics & numerical data</subject><subject>diastereomers</subject><subject>General pharmacology</subject><subject>Glucuronates - chemistry</subject><subject>Glucuronates - urine</subject><subject>Humans</subject><subject>Medical sciences</subject><subject>metal complexes</subject><subject>Pharmacology. Drug treatments</subject><subject>porous graphitic carbon</subject><subject>Propanolamines - chemistry</subject><subject>Propanolamines - urine</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Stereoisomerism</subject><subject>Temperature</subject><issn>0899-0042</issn><issn>1520-636X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1992</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkUFv1DAQhS0EKsvClRuSD4hTszh24sRHtEAbaYGqgMrNmnUmjWnibO1EZf8JPxevslq4cRpp5ntvRvMIeZmyVcoYf2ta61e5YCxjJVOPyCLNOUukkD8ekwUrlUriiD8lz0L4yRhTUmRn5CzNClnKdEF-v7cezUjNMO06rGPtpt7RgDvwMNrBUXA1rXFE31s3d4aGji3S2kKIbRx69NbQ224ykx-crTEcEOj64Q46cOM5BerwgZoOQqBVVUXP0YL37X5s-yit_XR7Tq2j7dSDo5O3Dp-TJw10AV8c65J8__jh2_oy2Xy5qNbvNonJWKESoSQTQqZNY5SUaYGAHEHmgkOT5Sw1istsmxmutgrBiJSzEiJh8nKrDIBYkjez784P9xOGUfc2GOzi4ThMQRciK4SKb1uS1QwaP4TgsdE7b3vwe50yfYhCH6LQpyii4NXRedr2WP_F59_H-evjHIKBrvHgjA0nLMt5lpcHTM3Yg-1w_5-len1ZXf97QjJrbUzq10kL_k7LQhS5vvl8ofnN5urTV36lr8UfCw-06w</recordid><startdate>1992</startdate><enddate>1992</enddate><creator>Stefansson, Morgan</creator><creator>Hoffmann, Kurt-Jürgen</creator><general>Alan R. Liss, Inc</general><general>Wiley</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>7X8</scope></search><sort><creationdate>1992</creationdate><title>Direct coupled column separation and determination of the diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine</title><author>Stefansson, Morgan ; Hoffmann, Kurt-Jürgen</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c4079-39603361ffc96617eae2ea6532af4501c9264b4c29b9eac31208a2eac58b9caa3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1992</creationdate><topic>almokalant glucuronides</topic><topic>Analysis</topic><topic>Anti-Arrhythmia Agents - chemistry</topic><topic>Anti-Arrhythmia Agents - classification</topic><topic>Anti-Arrhythmia Agents - urine</topic><topic>bioanalysis</topic><topic>Biological and medical sciences</topic><topic>Buffers</topic><topic>Chromatography, Ion Exchange - instrumentation</topic><topic>Chromatography, Ion Exchange - methods</topic><topic>Chromatography, Ion Exchange - statistics & numerical data</topic><topic>diastereomers</topic><topic>General pharmacology</topic><topic>Glucuronates - chemistry</topic><topic>Glucuronates - urine</topic><topic>Humans</topic><topic>Medical sciences</topic><topic>metal complexes</topic><topic>Pharmacology. Drug treatments</topic><topic>porous graphitic carbon</topic><topic>Propanolamines - chemistry</topic><topic>Propanolamines - urine</topic><topic>Reproducibility of Results</topic><topic>Sensitivity and Specificity</topic><topic>Stereoisomerism</topic><topic>Temperature</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Stefansson, Morgan</creatorcontrib><creatorcontrib>Hoffmann, Kurt-Jürgen</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>MEDLINE - Academic</collection><jtitle>Chirality (New York, N.Y.)</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Stefansson, Morgan</au><au>Hoffmann, Kurt-Jürgen</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Direct coupled column separation and determination of the diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine</atitle><jtitle>Chirality (New York, N.Y.)</jtitle><addtitle>Chirality</addtitle><date>1992</date><risdate>1992</risdate><volume>4</volume><issue>8</issue><spage>509</spage><epage>514</epage><pages>509-514</pages><issn>0899-0042</issn><eissn>1520-636X</eissn><coden>CHRLEP</coden><abstract>A reversed‐phase coupled column separation (CCS) system for the analysis of two diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine is described. After direct injection of urine samples (50 μl) the glucuronides were isolated by complex formation on a terbium(III) loaded strong cation exchanger at alkaline pH. The solutes were eluted from the precolumn by an acidic mobile phase, enriched and separated on Hypercarb (porous graphitic carbon) as analytical column with 0.1 M acetic acid pH 2.8 and 30% acetonitrile as mobile phase. The calibration graph was linear (r2 = 0.9999) and the detection limits were in the low picomole (UV) or femtomole (fluorescence) range. Optimization of the analytical column revealed that elution order and selectivity for the glucuronides were dependent on the buffer agent and temperature used. By appropriate choice of mobile phase conditions all four diastereomers could be separated. © 1992 Wiley‐Liss, Inc.</abstract><cop>New York</cop><pub>Alan R. Liss, Inc</pub><pmid>1476861</pmid><doi>10.1002/chir.530040809</doi><tpages>6</tpages></addata></record> |
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subjects | almokalant glucuronides Analysis Anti-Arrhythmia Agents - chemistry Anti-Arrhythmia Agents - classification Anti-Arrhythmia Agents - urine bioanalysis Biological and medical sciences Buffers Chromatography, Ion Exchange - instrumentation Chromatography, Ion Exchange - methods Chromatography, Ion Exchange - statistics & numerical data diastereomers General pharmacology Glucuronates - chemistry Glucuronates - urine Humans Medical sciences metal complexes Pharmacology. Drug treatments porous graphitic carbon Propanolamines - chemistry Propanolamines - urine Reproducibility of Results Sensitivity and Specificity Stereoisomerism Temperature |
title | Direct coupled column separation and determination of the diastereomeric glucuronides of almokalant, a new class III antiarrhythmic drug, in human urine |
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