Simultaneous Determination of 4-Nonylphenol and Bisphenol A in Sewage Sludge
An analytical method has been developed for simultaneous extraction and determination of two estrogenic active agents, 4-nonylphenol (4-NP) and bisphenol A (BPA), in activated sewage sludge and anaerobically stabilized sewage sludge. Both compounds were determined by GC/MS in freeze-dried sewage slu...
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| Veröffentlicht in: | Analytical chemistry (Washington) 2002-07, Vol.74 (14), p.3566-3574 |
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| creator | Meesters, Roland J. W Schröder, Horst Fr |
| description | An analytical method has been developed for simultaneous extraction and determination of two estrogenic active agents, 4-nonylphenol (4-NP) and bisphenol A (BPA), in activated sewage sludge and anaerobically stabilized sewage sludge. Both compounds were determined by GC/MS in freeze-dried sewage sludge samples that had been spiked with these compounds in order to indicate different contamination levels. Extractive steam distillation, Soxhlet extraction, supercritical fluid extraction (SFE), and accelerated solvent extraction (ASE) were applied, and the results were compared. ASE under use of ethyl acetate/formic acid and an extraction temperature of 170 °C provided the most efficient extraction procedure for simultaneous extraction and the only reliable extraction results. Analyses of the phenolic compounds were performed by capillary column gas chromatography/mass spectrometry (GC/MS), operating in selected ion monitoring (SIM) mode after an aluminum oxide column-cleanup step prior to acetylation. The observed recovery rates under optimized conditionsASE with ethyl acetate/formic acidfor 4-NP in spiked activated sewage sludge samples (spiking levels: 51, 88, or 554 μg/g on dry weight basis (dwb)) were 90, 107, or 101%. BPA (spiking levels: 50, 87, or 474 μg/g dwb) was found with recovery rates of 70, 105, or 101%, respectively. For anaerobically stabilized sewage sludge, recoveries for 4-NP (spiking levels: 40, 66, or 196 μg/g dwb) were 97, 95, or 101% and 90, 95, or 101% for BPA (spiking levels: 41, 67, or 474 μg/g dwb), respectively. |
| doi_str_mv | 10.1021/ac011258q |
| format | Article |
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W ; Schröder, Horst Fr</creator><creatorcontrib>Meesters, Roland J. W ; Schröder, Horst Fr</creatorcontrib><description>An analytical method has been developed for simultaneous extraction and determination of two estrogenic active agents, 4-nonylphenol (4-NP) and bisphenol A (BPA), in activated sewage sludge and anaerobically stabilized sewage sludge. Both compounds were determined by GC/MS in freeze-dried sewage sludge samples that had been spiked with these compounds in order to indicate different contamination levels. Extractive steam distillation, Soxhlet extraction, supercritical fluid extraction (SFE), and accelerated solvent extraction (ASE) were applied, and the results were compared. ASE under use of ethyl acetate/formic acid and an extraction temperature of 170 °C provided the most efficient extraction procedure for simultaneous extraction and the only reliable extraction results. Analyses of the phenolic compounds were performed by capillary column gas chromatography/mass spectrometry (GC/MS), operating in selected ion monitoring (SIM) mode after an aluminum oxide column-cleanup step prior to acetylation. The observed recovery rates under optimized conditionsASE with ethyl acetate/formic acidfor 4-NP in spiked activated sewage sludge samples (spiking levels: 51, 88, or 554 μg/g on dry weight basis (dwb)) were 90, 107, or 101%. BPA (spiking levels: 50, 87, or 474 μg/g dwb) was found with recovery rates of 70, 105, or 101%, respectively. For anaerobically stabilized sewage sludge, recoveries for 4-NP (spiking levels: 40, 66, or 196 μg/g dwb) were 97, 95, or 101% and 90, 95, or 101% for BPA (spiking levels: 41, 67, or 474 μg/g dwb), respectively.</description><identifier>ISSN: 0003-2700</identifier><identifier>EISSN: 1520-6882</identifier><identifier>DOI: 10.1021/ac011258q</identifier><identifier>PMID: 12139069</identifier><identifier>CODEN: ANCHAM</identifier><language>eng</language><publisher>Washington, DC: American Chemical Society</publisher><subject>Analysis ; Analysis methods ; Analytical chemistry ; Applied sciences ; Benzhydryl Compounds ; Chemistry ; Chromatographic methods and physical methods associated with chromatography ; Contamination ; Estrogens, Non-Steroidal - analysis ; Exact sciences and technology ; Gas chromatographic methods ; Gas Chromatography-Mass Spectrometry - methods ; Industrial Waste - analysis ; Phenols - analysis ; Pollution ; Sludge ; Spectrometric and optical methods ; Wastes</subject><ispartof>Analytical chemistry (Washington), 2002-07, Vol.74 (14), p.3566-3574</ispartof><rights>Copyright © 2002 American Chemical Society</rights><rights>2002 INIST-CNRS</rights><rights>Copyright American Chemical Society Jul 15, 2002</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-a503t-7e4fae44c7938d90a80e550a511b446374ed42bb359ce3699350cda19e087e653</citedby><cites>FETCH-LOGICAL-a503t-7e4fae44c7938d90a80e550a511b446374ed42bb359ce3699350cda19e087e653</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://pubs.acs.org/doi/pdf/10.1021/ac011258q$$EPDF$$P50$$Gacs$$H</linktopdf><linktohtml>$$Uhttps://pubs.acs.org/doi/10.1021/ac011258q$$EHTML$$P50$$Gacs$$H</linktohtml><link.rule.ids>314,780,784,2765,27076,27924,27925,56738,56788</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=13794976$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://www.ncbi.nlm.nih.gov/pubmed/12139069$$D View this record in MEDLINE/PubMed$$Hfree_for_read</backlink></links><search><creatorcontrib>Meesters, Roland J. W</creatorcontrib><creatorcontrib>Schröder, Horst Fr</creatorcontrib><title>Simultaneous Determination of 4-Nonylphenol and Bisphenol A in Sewage Sludge</title><title>Analytical chemistry (Washington)</title><addtitle>Anal. Chem</addtitle><description>An analytical method has been developed for simultaneous extraction and determination of two estrogenic active agents, 4-nonylphenol (4-NP) and bisphenol A (BPA), in activated sewage sludge and anaerobically stabilized sewage sludge. Both compounds were determined by GC/MS in freeze-dried sewage sludge samples that had been spiked with these compounds in order to indicate different contamination levels. Extractive steam distillation, Soxhlet extraction, supercritical fluid extraction (SFE), and accelerated solvent extraction (ASE) were applied, and the results were compared. ASE under use of ethyl acetate/formic acid and an extraction temperature of 170 °C provided the most efficient extraction procedure for simultaneous extraction and the only reliable extraction results. Analyses of the phenolic compounds were performed by capillary column gas chromatography/mass spectrometry (GC/MS), operating in selected ion monitoring (SIM) mode after an aluminum oxide column-cleanup step prior to acetylation. The observed recovery rates under optimized conditionsASE with ethyl acetate/formic acidfor 4-NP in spiked activated sewage sludge samples (spiking levels: 51, 88, or 554 μg/g on dry weight basis (dwb)) were 90, 107, or 101%. BPA (spiking levels: 50, 87, or 474 μg/g dwb) was found with recovery rates of 70, 105, or 101%, respectively. For anaerobically stabilized sewage sludge, recoveries for 4-NP (spiking levels: 40, 66, or 196 μg/g dwb) were 97, 95, or 101% and 90, 95, or 101% for BPA (spiking levels: 41, 67, or 474 μg/g dwb), respectively.</description><subject>Analysis</subject><subject>Analysis methods</subject><subject>Analytical chemistry</subject><subject>Applied sciences</subject><subject>Benzhydryl Compounds</subject><subject>Chemistry</subject><subject>Chromatographic methods and physical methods associated with chromatography</subject><subject>Contamination</subject><subject>Estrogens, Non-Steroidal - analysis</subject><subject>Exact sciences and technology</subject><subject>Gas chromatographic methods</subject><subject>Gas Chromatography-Mass Spectrometry - methods</subject><subject>Industrial Waste - analysis</subject><subject>Phenols - analysis</subject><subject>Pollution</subject><subject>Sludge</subject><subject>Spectrometric and optical methods</subject><subject>Wastes</subject><issn>0003-2700</issn><issn>1520-6882</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2002</creationdate><recordtype>article</recordtype><sourceid>EIF</sourceid><recordid>eNpl0E1v1DAQBmALUdGlcOAPoAipSD0Ext_xsS20RVo-xJaz5XUmxSVxtnYi2n9PVht1JXqyLT9-PTOEvKHwgQKjH50HSpms7p6RBZUMSlVV7DlZAAAvmQY4JC9zvoVJAVUvyCFllBtQZkGWq9CN7eAi9mMuPuGAqQvRDaGPRd8UovzWx4d28xtj3xYu1sVZyPPptAixWOFfd4PFqh3rG3xFDhrXZnw9r0fk18Xn6_Orcvn98sv56bJ0EvhQahSNQyG8NryqDbgKUEpwktK1EIprgbVg6zWXxiNXxnAJvnbUIFQaleRH5P0ud5P6uxHzYLuQPbbtrg1LFd0-MxN89x-87ccUp9oso7qSQhk1oZMd8qnPOWFjNyl0Lj1YCnY7X_s438m-nQPHdYf1Xs4DncDxDFz2rm2Siz7kvePaCKO3n5Y7F_KA94_3Lv2xSnMt7fWPlT1jVz-_ymlT7XOdz_smnhb4D1QRmxo</recordid><startdate>20020715</startdate><enddate>20020715</enddate><creator>Meesters, Roland J. 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W ; Schröder, Horst Fr</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-a503t-7e4fae44c7938d90a80e550a511b446374ed42bb359ce3699350cda19e087e653</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2002</creationdate><topic>Analysis</topic><topic>Analysis methods</topic><topic>Analytical chemistry</topic><topic>Applied sciences</topic><topic>Benzhydryl Compounds</topic><topic>Chemistry</topic><topic>Chromatographic methods and physical methods associated with chromatography</topic><topic>Contamination</topic><topic>Estrogens, Non-Steroidal - analysis</topic><topic>Exact sciences and technology</topic><topic>Gas chromatographic methods</topic><topic>Gas Chromatography-Mass Spectrometry - methods</topic><topic>Industrial Waste - analysis</topic><topic>Phenols - analysis</topic><topic>Pollution</topic><topic>Sludge</topic><topic>Spectrometric and optical methods</topic><topic>Wastes</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Meesters, Roland J. 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W</au><au>Schröder, Horst Fr</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Simultaneous Determination of 4-Nonylphenol and Bisphenol A in Sewage Sludge</atitle><jtitle>Analytical chemistry (Washington)</jtitle><addtitle>Anal. Chem</addtitle><date>2002-07-15</date><risdate>2002</risdate><volume>74</volume><issue>14</issue><spage>3566</spage><epage>3574</epage><pages>3566-3574</pages><issn>0003-2700</issn><eissn>1520-6882</eissn><coden>ANCHAM</coden><abstract>An analytical method has been developed for simultaneous extraction and determination of two estrogenic active agents, 4-nonylphenol (4-NP) and bisphenol A (BPA), in activated sewage sludge and anaerobically stabilized sewage sludge. Both compounds were determined by GC/MS in freeze-dried sewage sludge samples that had been spiked with these compounds in order to indicate different contamination levels. Extractive steam distillation, Soxhlet extraction, supercritical fluid extraction (SFE), and accelerated solvent extraction (ASE) were applied, and the results were compared. ASE under use of ethyl acetate/formic acid and an extraction temperature of 170 °C provided the most efficient extraction procedure for simultaneous extraction and the only reliable extraction results. Analyses of the phenolic compounds were performed by capillary column gas chromatography/mass spectrometry (GC/MS), operating in selected ion monitoring (SIM) mode after an aluminum oxide column-cleanup step prior to acetylation. The observed recovery rates under optimized conditionsASE with ethyl acetate/formic acidfor 4-NP in spiked activated sewage sludge samples (spiking levels: 51, 88, or 554 μg/g on dry weight basis (dwb)) were 90, 107, or 101%. BPA (spiking levels: 50, 87, or 474 μg/g dwb) was found with recovery rates of 70, 105, or 101%, respectively. For anaerobically stabilized sewage sludge, recoveries for 4-NP (spiking levels: 40, 66, or 196 μg/g dwb) were 97, 95, or 101% and 90, 95, or 101% for BPA (spiking levels: 41, 67, or 474 μg/g dwb), respectively.</abstract><cop>Washington, DC</cop><pub>American Chemical Society</pub><pmid>12139069</pmid><doi>10.1021/ac011258q</doi><tpages>9</tpages></addata></record> |
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| subjects | Analysis Analysis methods Analytical chemistry Applied sciences Benzhydryl Compounds Chemistry Chromatographic methods and physical methods associated with chromatography Contamination Estrogens, Non-Steroidal - analysis Exact sciences and technology Gas chromatographic methods Gas Chromatography-Mass Spectrometry - methods Industrial Waste - analysis Phenols - analysis Pollution Sludge Spectrometric and optical methods Wastes |
| title | Simultaneous Determination of 4-Nonylphenol and Bisphenol A in Sewage Sludge |
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