Analysis of hormonal steroids in fish plasma and bile by coupling solid-phase extraction to GC/MS
An analytical procedure for the simultaneous determination of twelve endogenous steroids (testosterone, androstenedione, 17β-estradiol, estrone, pregnenolone, progesterone, dihydroandrostenedione, dihydrotestosterone, 11α-ketotestosterone, 17α-hydroxyprogesterone, 17α-hydroxypregnenolone, 17α,20β-di...
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| Veröffentlicht in: | Analytical and bioanalytical chemistry 2006-11, Vol.386 (5), p.1429-1439 |
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| creator | Budzinski, H Devier, M. H Labadie, P Togola, A |
| description | An analytical procedure for the simultaneous determination of twelve endogenous steroids (testosterone, androstenedione, 17β-estradiol, estrone, pregnenolone, progesterone, dihydroandrostenedione, dihydrotestosterone, 11α-ketotestosterone, 17α-hydroxyprogesterone, 17α-hydroxypregnenolone, 17α,20β-dihydroxy-4-pregnen-3-one) in plasma and bile samples by solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC-MS) has been developed. After enzymatic hydrolysis for bile samples only, samples were concentrated and purified using two successive SPE (C₁₈ and NH₂) cartridges. Analytes were derivatized with a mixture of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) / mercaptoethanol / ammonium iodide (NH₄I) and determined by GC-MS in selective ion monitoring mode. For most of the steroids monitored, recoveries were in the range 90-120% in plasma and in the range 60-70% in bile, and the reproducibility was below 10% for the complete procedure. Limits of detection obtained ranged from 0.1 to 0.4 ng/g in fish plasma and from 1.6 to 14 ng/g in fish bile. The developed method was successfully applied to the determination of plasma steroids in flounders (Platichthys flesus) collected from two French estuaries. |
| doi_str_mv | 10.1007/s00216-006-0686-9 |
| format | Article |
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H ; Labadie, P ; Togola, A</creator><creatorcontrib>Budzinski, H ; Devier, M. H ; Labadie, P ; Togola, A</creatorcontrib><description>An analytical procedure for the simultaneous determination of twelve endogenous steroids (testosterone, androstenedione, 17β-estradiol, estrone, pregnenolone, progesterone, dihydroandrostenedione, dihydrotestosterone, 11α-ketotestosterone, 17α-hydroxyprogesterone, 17α-hydroxypregnenolone, 17α,20β-dihydroxy-4-pregnen-3-one) in plasma and bile samples by solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC-MS) has been developed. After enzymatic hydrolysis for bile samples only, samples were concentrated and purified using two successive SPE (C₁₈ and NH₂) cartridges. Analytes were derivatized with a mixture of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) / mercaptoethanol / ammonium iodide (NH₄I) and determined by GC-MS in selective ion monitoring mode. For most of the steroids monitored, recoveries were in the range 90-120% in plasma and in the range 60-70% in bile, and the reproducibility was below 10% for the complete procedure. Limits of detection obtained ranged from 0.1 to 0.4 ng/g in fish plasma and from 1.6 to 14 ng/g in fish bile. The developed method was successfully applied to the determination of plasma steroids in flounders (Platichthys flesus) collected from two French estuaries.</description><identifier>ISSN: 1618-2642</identifier><identifier>EISSN: 1618-2650</identifier><identifier>DOI: 10.1007/s00216-006-0686-9</identifier><identifier>PMID: 16906384</identifier><language>eng</language><publisher>Germany: Berlin/Heidelberg : Springer-Verlag</publisher><subject>17β-Estradiol ; Ammonium ; Androstenedione ; Animals ; Bile ; Bile - chemistry ; Dihydrotestosterone ; Environmental Sciences ; estradiol ; Estrone ; Estuaries ; Fish ; Gas chromatography ; Gas Chromatography-Mass Spectrometry - methods ; GC/MS ; Iodides ; Ions ; Mass spectrometry ; Mass spectroscopy ; Molecular Conformation ; Oncorhynchus mykiss ; Plasma ; Plasma - chemistry ; Pregnenolone ; Progesterone ; Reproducibility of Results ; Sensitivity and Specificity ; Sex hormones ; Solid Phase Microextraction - methods ; Solid phases ; Solvents - chemistry ; Steroid hormones ; Steroids ; Steroids - analysis ; Temperature ; Testosterone</subject><ispartof>Analytical and bioanalytical chemistry, 2006-11, Vol.386 (5), p.1429-1439</ispartof><rights>Springer-Verlag 2006.</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c416t-65b7e1ee426a270e14fa45cadd7b1da715454ec2b7a1ef81031b260f6d9d234d3</citedby><cites>FETCH-LOGICAL-c416t-65b7e1ee426a270e14fa45cadd7b1da715454ec2b7a1ef81031b260f6d9d234d3</cites><orcidid>0000-0001-7184-6327 ; 0000-0001-5282-9011 ; 0000-0003-1028-9154</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><link.rule.ids>230,314,777,781,882,27905,27906</link.rule.ids><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/16906384$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink><backlink>$$Uhttps://hal.science/hal-02289146$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Budzinski, H</creatorcontrib><creatorcontrib>Devier, M. H</creatorcontrib><creatorcontrib>Labadie, P</creatorcontrib><creatorcontrib>Togola, A</creatorcontrib><title>Analysis of hormonal steroids in fish plasma and bile by coupling solid-phase extraction to GC/MS</title><title>Analytical and bioanalytical chemistry</title><addtitle>Anal Bioanal Chem</addtitle><description>An analytical procedure for the simultaneous determination of twelve endogenous steroids (testosterone, androstenedione, 17β-estradiol, estrone, pregnenolone, progesterone, dihydroandrostenedione, dihydrotestosterone, 11α-ketotestosterone, 17α-hydroxyprogesterone, 17α-hydroxypregnenolone, 17α,20β-dihydroxy-4-pregnen-3-one) in plasma and bile samples by solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC-MS) has been developed. After enzymatic hydrolysis for bile samples only, samples were concentrated and purified using two successive SPE (C₁₈ and NH₂) cartridges. Analytes were derivatized with a mixture of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) / mercaptoethanol / ammonium iodide (NH₄I) and determined by GC-MS in selective ion monitoring mode. For most of the steroids monitored, recoveries were in the range 90-120% in plasma and in the range 60-70% in bile, and the reproducibility was below 10% for the complete procedure. Limits of detection obtained ranged from 0.1 to 0.4 ng/g in fish plasma and from 1.6 to 14 ng/g in fish bile. The developed method was successfully applied to the determination of plasma steroids in flounders (Platichthys flesus) collected from two French estuaries.</description><subject>17β-Estradiol</subject><subject>Ammonium</subject><subject>Androstenedione</subject><subject>Animals</subject><subject>Bile</subject><subject>Bile - chemistry</subject><subject>Dihydrotestosterone</subject><subject>Environmental Sciences</subject><subject>estradiol</subject><subject>Estrone</subject><subject>Estuaries</subject><subject>Fish</subject><subject>Gas chromatography</subject><subject>Gas Chromatography-Mass Spectrometry - methods</subject><subject>GC/MS</subject><subject>Iodides</subject><subject>Ions</subject><subject>Mass spectrometry</subject><subject>Mass spectroscopy</subject><subject>Molecular Conformation</subject><subject>Oncorhynchus mykiss</subject><subject>Plasma</subject><subject>Plasma - chemistry</subject><subject>Pregnenolone</subject><subject>Progesterone</subject><subject>Reproducibility of Results</subject><subject>Sensitivity and Specificity</subject><subject>Sex hormones</subject><subject>Solid Phase Microextraction - methods</subject><subject>Solid phases</subject><subject>Solvents - chemistry</subject><subject>Steroid hormones</subject><subject>Steroids</subject><subject>Steroids - analysis</subject><subject>Temperature</subject><subject>Testosterone</subject><issn>1618-2642</issn><issn>1618-2650</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2006</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><sourceid>ABUWG</sourceid><sourceid>AFKRA</sourceid><sourceid>AZQEC</sourceid><sourceid>BENPR</sourceid><sourceid>CCPQU</sourceid><sourceid>DWQXO</sourceid><sourceid>GNUQQ</sourceid><recordid>eNqFkk1r3DAQhk1paT7aH9BLKygEenAzI0uyfVyWNils6SHNWYwtOatgW65kh-6_rxYvKfTSg9AHz7wM8yjL3iF8RoDyOgJwVDlAWqpSef0iO0eFVc6VhJfPZ8HPsosYHwFQVqheZ2eoalBFJc4z2ozUH6KLzHds78Pg053F2QbvTGRuZJ2Lezb1FAdiNBrWuN6y5sBav0y9Gx9Y9L0z-bSnaJn9PQdqZ-dHNnt2s73-fvcme9VRH-3b036Z3X_98nN7m-9-3HzbbnZ5K1DNuZJNadFawRXxEiyKjoRsyZiyQUMlSiGFbXlTEtquQiiw4Qo6ZWrDC2GKy-zTmrunXk_BDRQO2pPTt5udPr4B51WNQj1hYq9Wdgr-12LjrAcXW9v3NFq_RJ3Gk-iS_xfktRRc1pDAj_-Aj34JaZaJUUoWJVSVShSuVBt8jMF2z40i6KNSvSrVSak-KtV1qnl_Sl6awZq_FSeHCfiwAh15TQ_BRX1_xwGLlFemn6CKP3tBo14</recordid><startdate>20061101</startdate><enddate>20061101</enddate><creator>Budzinski, H</creator><creator>Devier, M. 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H</au><au>Labadie, P</au><au>Togola, A</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Analysis of hormonal steroids in fish plasma and bile by coupling solid-phase extraction to GC/MS</atitle><jtitle>Analytical and bioanalytical chemistry</jtitle><addtitle>Anal Bioanal Chem</addtitle><date>2006-11-01</date><risdate>2006</risdate><volume>386</volume><issue>5</issue><spage>1429</spage><epage>1439</epage><pages>1429-1439</pages><issn>1618-2642</issn><eissn>1618-2650</eissn><abstract>An analytical procedure for the simultaneous determination of twelve endogenous steroids (testosterone, androstenedione, 17β-estradiol, estrone, pregnenolone, progesterone, dihydroandrostenedione, dihydrotestosterone, 11α-ketotestosterone, 17α-hydroxyprogesterone, 17α-hydroxypregnenolone, 17α,20β-dihydroxy-4-pregnen-3-one) in plasma and bile samples by solid-phase extraction (SPE) and gas chromatography/mass spectrometry (GC-MS) has been developed. After enzymatic hydrolysis for bile samples only, samples were concentrated and purified using two successive SPE (C₁₈ and NH₂) cartridges. Analytes were derivatized with a mixture of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA) / mercaptoethanol / ammonium iodide (NH₄I) and determined by GC-MS in selective ion monitoring mode. For most of the steroids monitored, recoveries were in the range 90-120% in plasma and in the range 60-70% in bile, and the reproducibility was below 10% for the complete procedure. Limits of detection obtained ranged from 0.1 to 0.4 ng/g in fish plasma and from 1.6 to 14 ng/g in fish bile. 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| subjects | 17β-Estradiol Ammonium Androstenedione Animals Bile Bile - chemistry Dihydrotestosterone Environmental Sciences estradiol Estrone Estuaries Fish Gas chromatography Gas Chromatography-Mass Spectrometry - methods GC/MS Iodides Ions Mass spectrometry Mass spectroscopy Molecular Conformation Oncorhynchus mykiss Plasma Plasma - chemistry Pregnenolone Progesterone Reproducibility of Results Sensitivity and Specificity Sex hormones Solid Phase Microextraction - methods Solid phases Solvents - chemistry Steroid hormones Steroids Steroids - analysis Temperature Testosterone |
| title | Analysis of hormonal steroids in fish plasma and bile by coupling solid-phase extraction to GC/MS |
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