An LC–MS method to determine concentrations of isoflavones and their sulfate and glucuronide conjugates in urine
Most methods for detecting isoflavones in biological samples do not measure the concentration of sulfate conjugates. An LC–MS method is reported here to estimate urinary concentrations of genistein and daidzein, their sulfate and glucuronide conjugates and other major metabolites. Human and rat urin...
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Veröffentlicht in: | Clinica chimica acta 1999-09, Vol.287 (1), p.69-82 |
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description | Most methods for detecting isoflavones in biological samples do not measure the concentration of sulfate conjugates. An LC–MS method is reported here to estimate urinary concentrations of genistein and daidzein, their sulfate and glucuronide conjugates and other major metabolites. Human and rat urine samples were extracted with diethyl ether, or pre-digested with sulfatase and/or β-glucuronidase followed by extraction. The isoflavones were separated using gradient LC methods and detected by negative single ion monitoring on an MS system using a heated nebulizer atmospheric pressure chemical ionization interface. CVs for inter- and intra-assay variability were generally |
doi_str_mv | 10.1016/S0009-8981(99)00124-2 |
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An LC–MS method is reported here to estimate urinary concentrations of genistein and daidzein, their sulfate and glucuronide conjugates and other major metabolites. Human and rat urine samples were extracted with diethyl ether, or pre-digested with sulfatase and/or β-glucuronidase followed by extraction. The isoflavones were separated using gradient LC methods and detected by negative single ion monitoring on an MS system using a heated nebulizer atmospheric pressure chemical ionization interface. CVs for inter- and intra-assay variability were generally <20 and 10%, respectively. Preliminary studies using these procedures demonstrate 52±4 and 26±4% of genistein in rat urine was found as the aglycone and sulfate conjugates, respectively, compared to 0.36 and 4%, respectively, in human urine. This method is suitable for the study of isoflavone sulfate conjugates in biological fluids.</description><identifier>ISSN: 0009-8981</identifier><identifier>EISSN: 1873-3492</identifier><identifier>DOI: 10.1016/S0009-8981(99)00124-2</identifier><identifier>PMID: 10509897</identifier><identifier>CODEN: CCATAR</identifier><language>eng</language><publisher>Shannon: Elsevier B.V</publisher><subject>Animals ; Biological and medical sciences ; Calibration ; Cardiovascular system ; Chromatography, Liquid - methods ; Daidzein ; Genistein ; Glycine max ; Humans ; Isoflavones ; Isoflavones - urine ; LC–MS ; Male ; Mass Spectrometry - methods ; Medical sciences ; Miscellaneous ; Pharmacology. Drug treatments ; Rats ; Reproducibility of Results ; Soy ; Sulfates</subject><ispartof>Clinica chimica acta, 1999-09, Vol.287 (1), p.69-82</ispartof><rights>1999 Elsevier Science B.V.</rights><rights>1999 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c390t-36cf1a211a6d3507f4eaa59ce557e1bc4d49cdc66af1747495c0bed65707a83b3</citedby><cites>FETCH-LOGICAL-c390t-36cf1a211a6d3507f4eaa59ce557e1bc4d49cdc66af1747495c0bed65707a83b3</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/S0009-8981(99)00124-2$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>315,781,785,3551,27928,27929,45999</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=1977975$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/10509897$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Cimino, Carolyn O</creatorcontrib><creatorcontrib>Shelnutt, Susan R</creatorcontrib><creatorcontrib>Ronis, Martin J.J</creatorcontrib><creatorcontrib>Badger, Thomas M</creatorcontrib><title>An LC–MS method to determine concentrations of isoflavones and their sulfate and glucuronide conjugates in urine</title><title>Clinica chimica acta</title><addtitle>Clin Chim Acta</addtitle><description>Most methods for detecting isoflavones in biological samples do not measure the concentration of sulfate conjugates. An LC–MS method is reported here to estimate urinary concentrations of genistein and daidzein, their sulfate and glucuronide conjugates and other major metabolites. Human and rat urine samples were extracted with diethyl ether, or pre-digested with sulfatase and/or β-glucuronidase followed by extraction. The isoflavones were separated using gradient LC methods and detected by negative single ion monitoring on an MS system using a heated nebulizer atmospheric pressure chemical ionization interface. CVs for inter- and intra-assay variability were generally <20 and 10%, respectively. Preliminary studies using these procedures demonstrate 52±4 and 26±4% of genistein in rat urine was found as the aglycone and sulfate conjugates, respectively, compared to 0.36 and 4%, respectively, in human urine. This method is suitable for the study of isoflavone sulfate conjugates in biological fluids.</description><subject>Animals</subject><subject>Biological and medical sciences</subject><subject>Calibration</subject><subject>Cardiovascular system</subject><subject>Chromatography, Liquid - methods</subject><subject>Daidzein</subject><subject>Genistein</subject><subject>Glycine max</subject><subject>Humans</subject><subject>Isoflavones</subject><subject>Isoflavones - urine</subject><subject>LC–MS</subject><subject>Male</subject><subject>Mass Spectrometry - methods</subject><subject>Medical sciences</subject><subject>Miscellaneous</subject><subject>Pharmacology. Drug treatments</subject><subject>Rats</subject><subject>Reproducibility of Results</subject><subject>Soy</subject><subject>Sulfates</subject><issn>0009-8981</issn><issn>1873-3492</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>1999</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNqFkEFPHCEYhomx0dX2J2g4GNMepoWZYRhOZrOp1mSbHmzPhIUPxcyAAmPizf_Qf-gvEXc31VtPBHje9_vyIHREyVdKaPftihAiql709LMQXwihdVvVO2hGe95UTSvqXTT7h-yjg5Ruy7UlHd1D-5QwInrBZyjOPV4unp_-_rzCI-SbYHAO2ECGODoPWAevweeosgs-4WCxS8EO6iF4SFj5gt-AizhNg1UZ1i_Xw6SnGLwz6_ztdF1-EnYeT7F0fkQfrBoSfNqeh-jP-fffix_V8tfF5WK-rHQjSK6aTluqakpVZxpGuG1BKSY0MMaBrnRrWqGN7jplKW95K5gmKzAd44Srvlk1h-h003sXw_0EKcvRJQ3DoDyEKcnCsb7kCsg2oI4hpQhW3kU3qvgoKZGvsuVatnw1KYWQa9myLrnj7YBpNYJ5l9rYLcDJFlBJq8FG5bVLb5zgXHBWsLMNBsXGg4Mok3ZQvBsXQWdpgvvPJi9T8Z4a</recordid><startdate>19990901</startdate><enddate>19990901</enddate><creator>Cimino, Carolyn O</creator><creator>Shelnutt, Susan R</creator><creator>Ronis, Martin J.J</creator><creator>Badger, Thomas M</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>7X8</scope></search><sort><creationdate>19990901</creationdate><title>An LC–MS method to determine concentrations of isoflavones and their sulfate and glucuronide conjugates in urine</title><author>Cimino, Carolyn O ; Shelnutt, Susan R ; Ronis, Martin J.J ; Badger, Thomas M</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c390t-36cf1a211a6d3507f4eaa59ce557e1bc4d49cdc66af1747495c0bed65707a83b3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>1999</creationdate><topic>Animals</topic><topic>Biological and medical sciences</topic><topic>Calibration</topic><topic>Cardiovascular system</topic><topic>Chromatography, Liquid - methods</topic><topic>Daidzein</topic><topic>Genistein</topic><topic>Glycine max</topic><topic>Humans</topic><topic>Isoflavones</topic><topic>Isoflavones - urine</topic><topic>LC–MS</topic><topic>Male</topic><topic>Mass Spectrometry - methods</topic><topic>Medical sciences</topic><topic>Miscellaneous</topic><topic>Pharmacology. Drug treatments</topic><topic>Rats</topic><topic>Reproducibility of Results</topic><topic>Soy</topic><topic>Sulfates</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Cimino, Carolyn O</creatorcontrib><creatorcontrib>Shelnutt, Susan R</creatorcontrib><creatorcontrib>Ronis, Martin J.J</creatorcontrib><creatorcontrib>Badger, Thomas M</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>MEDLINE - Academic</collection><jtitle>Clinica chimica acta</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Cimino, Carolyn O</au><au>Shelnutt, Susan R</au><au>Ronis, Martin J.J</au><au>Badger, Thomas M</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>An LC–MS method to determine concentrations of isoflavones and their sulfate and glucuronide conjugates in urine</atitle><jtitle>Clinica chimica acta</jtitle><addtitle>Clin Chim Acta</addtitle><date>1999-09-01</date><risdate>1999</risdate><volume>287</volume><issue>1</issue><spage>69</spage><epage>82</epage><pages>69-82</pages><issn>0009-8981</issn><eissn>1873-3492</eissn><coden>CCATAR</coden><abstract>Most methods for detecting isoflavones in biological samples do not measure the concentration of sulfate conjugates. An LC–MS method is reported here to estimate urinary concentrations of genistein and daidzein, their sulfate and glucuronide conjugates and other major metabolites. Human and rat urine samples were extracted with diethyl ether, or pre-digested with sulfatase and/or β-glucuronidase followed by extraction. The isoflavones were separated using gradient LC methods and detected by negative single ion monitoring on an MS system using a heated nebulizer atmospheric pressure chemical ionization interface. CVs for inter- and intra-assay variability were generally <20 and 10%, respectively. Preliminary studies using these procedures demonstrate 52±4 and 26±4% of genistein in rat urine was found as the aglycone and sulfate conjugates, respectively, compared to 0.36 and 4%, respectively, in human urine. This method is suitable for the study of isoflavone sulfate conjugates in biological fluids.</abstract><cop>Shannon</cop><pub>Elsevier B.V</pub><pmid>10509897</pmid><doi>10.1016/S0009-8981(99)00124-2</doi><tpages>14</tpages></addata></record> |
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subjects | Animals Biological and medical sciences Calibration Cardiovascular system Chromatography, Liquid - methods Daidzein Genistein Glycine max Humans Isoflavones Isoflavones - urine LC–MS Male Mass Spectrometry - methods Medical sciences Miscellaneous Pharmacology. Drug treatments Rats Reproducibility of Results Soy Sulfates |
title | An LC–MS method to determine concentrations of isoflavones and their sulfate and glucuronide conjugates in urine |
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