Using temperature to optimize resolution and reduce analysis times for bioanalytical diastereomer LC–MS/MS separations
A rugged and reproducible liquid chromatographic tandem mass spectrometric bioanalytical method was developed for the quantitation of drug stereoisomers in human plasma. Column temperature was shown to be an important variable toward optimizing diastereomer selectivity, resolution and analysis cycle...
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| Veröffentlicht in: | Journal of pharmaceutical and biomedical analysis 2011-01, Vol.54 (1), p.179-185 |
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| container_title | Journal of pharmaceutical and biomedical analysis |
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| creator | Cunliffe, Jennifer M. Dreyer, Daniel P. Hayes, Roger N. Clement, Robert P. Shen, Jim X. |
| description | A rugged and reproducible liquid chromatographic tandem mass spectrometric bioanalytical method was developed for the quantitation of drug stereoisomers in human plasma. Column temperature was shown to be an important variable toward optimizing diastereomer selectivity, resolution and analysis cycle time. Non-linear Van’t Hoff plots and changes in peak shape with temperature suggested that selectivity was governed by multiple retention mechanisms. The high temperature chromatography method was validated and used to analyze samples from human clinical trials. Utilization of high temperature chromatography offered alternative selectivity and is a viable approach for difficult separations in regulated bioanalysis. |
| doi_str_mv | 10.1016/j.jpba.2010.08.017 |
| format | Article |
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Column temperature was shown to be an important variable toward optimizing diastereomer selectivity, resolution and analysis cycle time. Non-linear Van’t Hoff plots and changes in peak shape with temperature suggested that selectivity was governed by multiple retention mechanisms. The high temperature chromatography method was validated and used to analyze samples from human clinical trials. Utilization of high temperature chromatography offered alternative selectivity and is a viable approach for difficult separations in regulated bioanalysis.</description><identifier>ISSN: 0731-7085</identifier><identifier>EISSN: 1873-264X</identifier><identifier>DOI: 10.1016/j.jpba.2010.08.017</identifier><identifier>PMID: 20837385</identifier><identifier>CODEN: JPBADA</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analysis ; Analytical, structural and metabolic biochemistry ; Bioanalytical ; Biological and medical sciences ; Chemistry Techniques, Analytical ; Chemistry, Pharmaceutical - methods ; Chromatography - methods ; Chromatography, High Pressure Liquid - methods ; Chromatography, Liquid - methods ; clinical trials ; Diastereomer separations ; diastereomers ; Dipeptides - analysis ; Dipeptides - chemistry ; drugs ; Fundamental and applied biological sciences. Psychology ; General pharmacology ; High temperature HPLC ; Humans ; liquid chromatography ; Medical sciences ; Pharmacology. Drug treatments ; Reproducibility of Results ; Resolution ; Stereoisomerism ; Sulfones - analysis ; Sulfones - chemistry ; tandem mass spectrometry ; Tandem Mass Spectrometry - methods ; Temperature ; Time Factors</subject><ispartof>Journal of pharmaceutical and biomedical analysis, 2011-01, Vol.54 (1), p.179-185</ispartof><rights>2010 Elsevier B.V.</rights><rights>2015 INIST-CNRS</rights><rights>Copyright © 2010 Elsevier B.V. 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Column temperature was shown to be an important variable toward optimizing diastereomer selectivity, resolution and analysis cycle time. Non-linear Van’t Hoff plots and changes in peak shape with temperature suggested that selectivity was governed by multiple retention mechanisms. The high temperature chromatography method was validated and used to analyze samples from human clinical trials. Utilization of high temperature chromatography offered alternative selectivity and is a viable approach for difficult separations in regulated bioanalysis.</description><subject>Analysis</subject><subject>Analytical, structural and metabolic biochemistry</subject><subject>Bioanalytical</subject><subject>Biological and medical sciences</subject><subject>Chemistry Techniques, Analytical</subject><subject>Chemistry, Pharmaceutical - methods</subject><subject>Chromatography - methods</subject><subject>Chromatography, High Pressure Liquid - methods</subject><subject>Chromatography, Liquid - methods</subject><subject>clinical trials</subject><subject>Diastereomer separations</subject><subject>diastereomers</subject><subject>Dipeptides - analysis</subject><subject>Dipeptides - chemistry</subject><subject>drugs</subject><subject>Fundamental and applied biological sciences. Psychology</subject><subject>General pharmacology</subject><subject>High temperature HPLC</subject><subject>Humans</subject><subject>liquid chromatography</subject><subject>Medical sciences</subject><subject>Pharmacology. Drug treatments</subject><subject>Reproducibility of Results</subject><subject>Resolution</subject><subject>Stereoisomerism</subject><subject>Sulfones - analysis</subject><subject>Sulfones - chemistry</subject><subject>tandem mass spectrometry</subject><subject>Tandem Mass Spectrometry - methods</subject><subject>Temperature</subject><subject>Time Factors</subject><issn>0731-7085</issn><issn>1873-264X</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2011</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNp9kMuO0zAUhi0EYsrAC7AAbxCrdI4vuUlsUMVN6ohFqcTOOnFORq6SONgJYljxDrwhT4I7LbBjZfvoO_9vfYw9FbAWIIqrw_owNbiWkAZQrUGU99hKVKXKZKE_32crKJXISqjyC_YoxgMA5KLWD9mFhEqVqspX7Ns-uvGGzzRMFHBeAvHZcz_NbnDfiQeKvl9m50eOY5ue7WIpXbG_jS7yRFHknQ-8cf5uOjuLPW8dxpkC-YEC325-_fh5vbu63vFIE6aWFBcfswcd9pGenM9Ltn_75tPmfbb9-O7D5vU2sxrqObNVh4VGlLpUhc2FBSGEtY1spC0VWI0Cm0pWGmVZoCBssdNdkSsrqqKupbpkL0-5U_BfFoqzGVy01Pc4kl-iKfNcg5Q1JFKeSBt8jIE6MwU3YLg1AsxRuDmYo3BzFG6gMkl4Wnp2jl-agdq_K38MJ-DFGcCY1HQBR-viP04pAaXQiXt-4jr0Bm9CYva71JQDCAnqrurViaCk66ujYKJ1NFpqXSA7m9a7__30N-uUqsk</recordid><startdate>201101</startdate><enddate>201101</enddate><creator>Cunliffe, Jennifer M.</creator><creator>Dreyer, Daniel P.</creator><creator>Hayes, Roger N.</creator><creator>Clement, Robert P.</creator><creator>Shen, Jim X.</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>FBQ</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>201101</creationdate><title>Using temperature to optimize resolution and reduce analysis times for bioanalytical diastereomer LC–MS/MS separations</title><author>Cunliffe, Jennifer M. ; Dreyer, Daniel P. ; Hayes, Roger N. ; Clement, Robert P. ; Shen, Jim X.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c409t-c8fa64aa24736c51c0111ccb2b2c730c4a1ab8284a276a1eadaf4f653c1869923</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2011</creationdate><topic>Analysis</topic><topic>Analytical, structural and metabolic biochemistry</topic><topic>Bioanalytical</topic><topic>Biological and medical sciences</topic><topic>Chemistry Techniques, Analytical</topic><topic>Chemistry, Pharmaceutical - methods</topic><topic>Chromatography - methods</topic><topic>Chromatography, High Pressure Liquid - methods</topic><topic>Chromatography, Liquid - methods</topic><topic>clinical trials</topic><topic>Diastereomer separations</topic><topic>diastereomers</topic><topic>Dipeptides - analysis</topic><topic>Dipeptides - chemistry</topic><topic>drugs</topic><topic>Fundamental and applied biological sciences. Psychology</topic><topic>General pharmacology</topic><topic>High temperature HPLC</topic><topic>Humans</topic><topic>liquid chromatography</topic><topic>Medical sciences</topic><topic>Pharmacology. Drug treatments</topic><topic>Reproducibility of Results</topic><topic>Resolution</topic><topic>Stereoisomerism</topic><topic>Sulfones - analysis</topic><topic>Sulfones - chemistry</topic><topic>tandem mass spectrometry</topic><topic>Tandem Mass Spectrometry - methods</topic><topic>Temperature</topic><topic>Time Factors</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Cunliffe, Jennifer M.</creatorcontrib><creatorcontrib>Dreyer, Daniel P.</creatorcontrib><creatorcontrib>Hayes, Roger N.</creatorcontrib><creatorcontrib>Clement, Robert P.</creatorcontrib><creatorcontrib>Shen, Jim X.</creatorcontrib><collection>AGRIS</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>Journal of pharmaceutical and biomedical analysis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Cunliffe, Jennifer M.</au><au>Dreyer, Daniel P.</au><au>Hayes, Roger N.</au><au>Clement, Robert P.</au><au>Shen, Jim X.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Using temperature to optimize resolution and reduce analysis times for bioanalytical diastereomer LC–MS/MS separations</atitle><jtitle>Journal of pharmaceutical and biomedical analysis</jtitle><addtitle>J Pharm Biomed Anal</addtitle><date>2011-01</date><risdate>2011</risdate><volume>54</volume><issue>1</issue><spage>179</spage><epage>185</epage><pages>179-185</pages><issn>0731-7085</issn><eissn>1873-264X</eissn><coden>JPBADA</coden><abstract>A rugged and reproducible liquid chromatographic tandem mass spectrometric bioanalytical method was developed for the quantitation of drug stereoisomers in human plasma. Column temperature was shown to be an important variable toward optimizing diastereomer selectivity, resolution and analysis cycle time. Non-linear Van’t Hoff plots and changes in peak shape with temperature suggested that selectivity was governed by multiple retention mechanisms. The high temperature chromatography method was validated and used to analyze samples from human clinical trials. Utilization of high temperature chromatography offered alternative selectivity and is a viable approach for difficult separations in regulated bioanalysis.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><pmid>20837385</pmid><doi>10.1016/j.jpba.2010.08.017</doi><tpages>7</tpages></addata></record> |
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| subjects | Analysis Analytical, structural and metabolic biochemistry Bioanalytical Biological and medical sciences Chemistry Techniques, Analytical Chemistry, Pharmaceutical - methods Chromatography - methods Chromatography, High Pressure Liquid - methods Chromatography, Liquid - methods clinical trials Diastereomer separations diastereomers Dipeptides - analysis Dipeptides - chemistry drugs Fundamental and applied biological sciences. Psychology General pharmacology High temperature HPLC Humans liquid chromatography Medical sciences Pharmacology. Drug treatments Reproducibility of Results Resolution Stereoisomerism Sulfones - analysis Sulfones - chemistry tandem mass spectrometry Tandem Mass Spectrometry - methods Temperature Time Factors |
| title | Using temperature to optimize resolution and reduce analysis times for bioanalytical diastereomer LC–MS/MS separations |
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