Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine
A sensitive and solvent-free procedure for the determination of hydroxy metabolites of polychlorinated biphenyls (PCBs) in urine samples was studied using solid-phase microextraction (SPME) followed by on-fiber silylation and gas chromatography/mass spectrometry (GC/MS) determination. The analytical...
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| Veröffentlicht in: | Analytica chimica acta 2005-05, Vol.539 (1), p.55-60 |
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| creator | Hong, Jee Eun Pyo, Heesoo Park, Song-Ja Lee, Won |
| description | A sensitive and solvent-free procedure for the determination of hydroxy metabolites of polychlorinated biphenyls (PCBs) in urine samples was studied using solid-phase microextraction (SPME) followed by on-fiber silylation and gas chromatography/mass spectrometry (GC/MS) determination. The analytical procedure involved headspace adsorption with coated fiber and headspace derivatization with bis(trimethylsilyl)-trifluoroacetamide (BSTFA) in a sample vial. Experimental SPME parameters such as selection of coating material, addition of salt, extraction time and temperature of adsorption were optimized. The optimum extraction conditions for hydroxy-PCBs were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) coated fiber at 90
°C for 60
min in urine, added 10% sodium chloride. Derivatization of the hydroxy-PCBs with BSTFA was performed on the SPME fiber at 60
°C for 10
min. The calibration curves for derivatized forms showed good linearity in the range of 0.01–10
ng
mL
−1 and method detection limits proved to be 0.01–0.1
ng
mL
−1 in 2
mL of urine. |
| doi_str_mv | 10.1016/j.aca.2005.02.065 |
| format | Article |
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°C for 60
min in urine, added 10% sodium chloride. Derivatization of the hydroxy-PCBs with BSTFA was performed on the SPME fiber at 60
°C for 10
min. The calibration curves for derivatized forms showed good linearity in the range of 0.01–10
ng
mL
−1 and method detection limits proved to be 0.01–0.1
ng
mL
−1 in 2
mL of urine.</description><identifier>ISSN: 0003-2670</identifier><identifier>EISSN: 1873-4324</identifier><identifier>DOI: 10.1016/j.aca.2005.02.065</identifier><identifier>CODEN: ACACAM</identifier><language>eng</language><publisher>Amsterdam: Elsevier B.V</publisher><subject>Analytical chemistry ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Derivatization ; Exact sciences and technology ; Gas chromatographic methods ; Gas chromatography/mass spectrometry ; Headspace ; Hydroxy-polychlorinated biphenyl compounds ; Solid-phase microextraction ; Spectrometric and optical methods ; Urine</subject><ispartof>Analytica chimica acta, 2005-05, Vol.539 (1), p.55-60</ispartof><rights>2005 Elsevier B.V.</rights><rights>2005 INIST-CNRS</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c358t-260c4124528ffafc1cfdd3015c8a18bc6c8cc910c82180e20af77662536685213</citedby><cites>FETCH-LOGICAL-c358t-260c4124528ffafc1cfdd3015c8a18bc6c8cc910c82180e20af77662536685213</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S0003267005003375$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>314,776,780,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=16751740$$DView record in Pascal Francis$$Hfree_for_read</backlink></links><search><creatorcontrib>Hong, Jee Eun</creatorcontrib><creatorcontrib>Pyo, Heesoo</creatorcontrib><creatorcontrib>Park, Song-Ja</creatorcontrib><creatorcontrib>Lee, Won</creatorcontrib><title>Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine</title><title>Analytica chimica acta</title><description>A sensitive and solvent-free procedure for the determination of hydroxy metabolites of polychlorinated biphenyls (PCBs) in urine samples was studied using solid-phase microextraction (SPME) followed by on-fiber silylation and gas chromatography/mass spectrometry (GC/MS) determination. The analytical procedure involved headspace adsorption with coated fiber and headspace derivatization with bis(trimethylsilyl)-trifluoroacetamide (BSTFA) in a sample vial. Experimental SPME parameters such as selection of coating material, addition of salt, extraction time and temperature of adsorption were optimized. The optimum extraction conditions for hydroxy-PCBs were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) coated fiber at 90
°C for 60
min in urine, added 10% sodium chloride. Derivatization of the hydroxy-PCBs with BSTFA was performed on the SPME fiber at 60
°C for 10
min. The calibration curves for derivatized forms showed good linearity in the range of 0.01–10
ng
mL
−1 and method detection limits proved to be 0.01–0.1
ng
mL
−1 in 2
mL of urine.</description><subject>Analytical chemistry</subject><subject>Chemistry</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Derivatization</subject><subject>Exact sciences and technology</subject><subject>Gas chromatographic methods</subject><subject>Gas chromatography/mass spectrometry</subject><subject>Headspace</subject><subject>Hydroxy-polychlorinated biphenyl compounds</subject><subject>Solid-phase microextraction</subject><subject>Spectrometric and optical methods</subject><subject>Urine</subject><issn>0003-2670</issn><issn>1873-4324</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2005</creationdate><recordtype>article</recordtype><recordid>eNp9kE1v1DAQhiMEEkvLD-DmC9wSxk7sGHFCFaVIlTgAZ8s7HiteJXGws6Xh3v-Nt1uJG6fRzPvO11NVbzg0HLh6f2gs2kYAyAZEA0o-q3Zc923dtaJ7Xu0AoK2F6uFl9SrnQ0kFh25XPXyPY3D1MthMbAqYIt2vyeIa4sx-h3Vgca592FNijlK4s2v4Yx9FHxNbByrlldIU5nM1ejZsLsX7rV7iuOEwxnTSyLF9WAaat5FhnJZ4nF1mYWbHItNl9cLbMdPrp3hR_bz-_OPqpr799uXr1afbGlup13I_YMdFJ4X23nrk6J1rgUvUlus9KtSIHzigFlwDCbC-75USslVKS8Hbi-rdee6S4q8j5dVMISONo50pHrPhfatEK0Ux8rOxAMk5kTdLCpNNm-FgTsDNwRTg5gTcgDAFeOl5-zTcZrSjT3bGkP81ql7yvoPi-3j2Ufn0LlAyGQPNSC4kwtW4GP6z5S9y8pjl</recordid><startdate>20050510</startdate><enddate>20050510</enddate><creator>Hong, Jee Eun</creator><creator>Pyo, Heesoo</creator><creator>Park, Song-Ja</creator><creator>Lee, Won</creator><general>Elsevier B.V</general><general>Elsevier</general><scope>IQODW</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>7U7</scope><scope>C1K</scope></search><sort><creationdate>20050510</creationdate><title>Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine</title><author>Hong, Jee Eun ; Pyo, Heesoo ; Park, Song-Ja ; Lee, Won</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c358t-260c4124528ffafc1cfdd3015c8a18bc6c8cc910c82180e20af77662536685213</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2005</creationdate><topic>Analytical chemistry</topic><topic>Chemistry</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Derivatization</topic><topic>Exact sciences and technology</topic><topic>Gas chromatographic methods</topic><topic>Gas chromatography/mass spectrometry</topic><topic>Headspace</topic><topic>Hydroxy-polychlorinated biphenyl compounds</topic><topic>Solid-phase microextraction</topic><topic>Spectrometric and optical methods</topic><topic>Urine</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Hong, Jee Eun</creatorcontrib><creatorcontrib>Pyo, Heesoo</creatorcontrib><creatorcontrib>Park, Song-Ja</creatorcontrib><creatorcontrib>Lee, Won</creatorcontrib><collection>Pascal-Francis</collection><collection>CrossRef</collection><collection>Toxicology Abstracts</collection><collection>Environmental Sciences and Pollution Management</collection><jtitle>Analytica chimica acta</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Hong, Jee Eun</au><au>Pyo, Heesoo</au><au>Park, Song-Ja</au><au>Lee, Won</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine</atitle><jtitle>Analytica chimica acta</jtitle><date>2005-05-10</date><risdate>2005</risdate><volume>539</volume><issue>1</issue><spage>55</spage><epage>60</epage><pages>55-60</pages><issn>0003-2670</issn><eissn>1873-4324</eissn><coden>ACACAM</coden><abstract>A sensitive and solvent-free procedure for the determination of hydroxy metabolites of polychlorinated biphenyls (PCBs) in urine samples was studied using solid-phase microextraction (SPME) followed by on-fiber silylation and gas chromatography/mass spectrometry (GC/MS) determination. The analytical procedure involved headspace adsorption with coated fiber and headspace derivatization with bis(trimethylsilyl)-trifluoroacetamide (BSTFA) in a sample vial. Experimental SPME parameters such as selection of coating material, addition of salt, extraction time and temperature of adsorption were optimized. The optimum extraction conditions for hydroxy-PCBs were obtained with a polydimethylsiloxane/divinylbenzene (PDMS/DVB) coated fiber at 90
°C for 60
min in urine, added 10% sodium chloride. Derivatization of the hydroxy-PCBs with BSTFA was performed on the SPME fiber at 60
°C for 10
min. The calibration curves for derivatized forms showed good linearity in the range of 0.01–10
ng
mL
−1 and method detection limits proved to be 0.01–0.1
ng
mL
−1 in 2
mL of urine.</abstract><cop>Amsterdam</cop><pub>Elsevier B.V</pub><doi>10.1016/j.aca.2005.02.065</doi><tpages>6</tpages></addata></record> |
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| subjects | Analytical chemistry Chemistry Chromatographic methods and physical methods associated with chromatography Derivatization Exact sciences and technology Gas chromatographic methods Gas chromatography/mass spectrometry Headspace Hydroxy-polychlorinated biphenyl compounds Solid-phase microextraction Spectrometric and optical methods Urine |
| title | Solid-phase microextraction with on-fiber derivatization for the determination of hydroxy-polychlorinated biphenyl compounds in urine |
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