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
Hauptverfasser: Stefansson, Morgan, Hoffmann, Kurt-Jürgen
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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><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 &amp; 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 &amp; 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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