{"title":"微波辅助萃取法测定污水污泥和生物固体中选定的烷基、芳基和卤代酚的优化","authors":"Hing‐Biu Lee, M. Svoboda, T. Peart, S. Smyth","doi":"10.2166/WQRJC.2016.002","DOIUrl":null,"url":null,"abstract":"A microwave-assisted extraction method for the determination of 15 alkyl, aryl, and halogenated phenols in sewage sludge and biosolids samples was developed and optimized. The effects of solvent, temperature, time, moisture content, acid, and number of extractions on the recovery of phenols were evaluated. Results indicated that extraction solvent had the greatest impact on the recovery of all phenols while pH had the largest effect on recovery of hexachlorophene and pentachlorophenol. Wet sludge samples were extracted with acetone-hexane mixture in the presence of glacial acetic acid. The extract was evaporated, acetylated by acetic anhydride and cleaned up by silica gel. For dry sludge samples, an optional procedure for the simultaneous extraction and acetylation of phenols was also proposed. Triclosan (TCS) and the alkyl and aryl phenols in sludge extracts were analyzed by gas chromatography-mass spectrometry (GC-MS) in electron-impact mode while polyhalogenated phenols were analyzed by GC-MS in negative ion chemical ionization mode. Method detection limits were ca. 200 ng/g for nonylphenol,","PeriodicalId":54407,"journal":{"name":"Water Quality Research Journal of Canada","volume":null,"pages":null},"PeriodicalIF":2.0000,"publicationDate":"2016-11-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://sci-hub-pdf.com/10.2166/WQRJC.2016.002","citationCount":"1","resultStr":"{\"title\":\"Optimization of a microwave-assisted extraction procedure for the determination of selected alkyl, aryl, and halogenated phenols in sewage sludge and biosolids\",\"authors\":\"Hing‐Biu Lee, M. Svoboda, T. Peart, S. Smyth\",\"doi\":\"10.2166/WQRJC.2016.002\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"A microwave-assisted extraction method for the determination of 15 alkyl, aryl, and halogenated phenols in sewage sludge and biosolids samples was developed and optimized. The effects of solvent, temperature, time, moisture content, acid, and number of extractions on the recovery of phenols were evaluated. Results indicated that extraction solvent had the greatest impact on the recovery of all phenols while pH had the largest effect on recovery of hexachlorophene and pentachlorophenol. Wet sludge samples were extracted with acetone-hexane mixture in the presence of glacial acetic acid. The extract was evaporated, acetylated by acetic anhydride and cleaned up by silica gel. For dry sludge samples, an optional procedure for the simultaneous extraction and acetylation of phenols was also proposed. Triclosan (TCS) and the alkyl and aryl phenols in sludge extracts were analyzed by gas chromatography-mass spectrometry (GC-MS) in electron-impact mode while polyhalogenated phenols were analyzed by GC-MS in negative ion chemical ionization mode. Method detection limits were ca. 200 ng/g for nonylphenol,\",\"PeriodicalId\":54407,\"journal\":{\"name\":\"Water Quality Research Journal of Canada\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":2.0000,\"publicationDate\":\"2016-11-02\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"https://sci-hub-pdf.com/10.2166/WQRJC.2016.002\",\"citationCount\":\"1\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Water Quality Research Journal of Canada\",\"FirstCategoryId\":\"1085\",\"ListUrlMain\":\"https://doi.org/10.2166/WQRJC.2016.002\",\"RegionNum\":0,\"RegionCategory\":null,\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q3\",\"JCRName\":\"Environmental Science\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Water Quality Research Journal of Canada","FirstCategoryId":"1085","ListUrlMain":"https://doi.org/10.2166/WQRJC.2016.002","RegionNum":0,"RegionCategory":null,"ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q3","JCRName":"Environmental Science","Score":null,"Total":0}
Optimization of a microwave-assisted extraction procedure for the determination of selected alkyl, aryl, and halogenated phenols in sewage sludge and biosolids
A microwave-assisted extraction method for the determination of 15 alkyl, aryl, and halogenated phenols in sewage sludge and biosolids samples was developed and optimized. The effects of solvent, temperature, time, moisture content, acid, and number of extractions on the recovery of phenols were evaluated. Results indicated that extraction solvent had the greatest impact on the recovery of all phenols while pH had the largest effect on recovery of hexachlorophene and pentachlorophenol. Wet sludge samples were extracted with acetone-hexane mixture in the presence of glacial acetic acid. The extract was evaporated, acetylated by acetic anhydride and cleaned up by silica gel. For dry sludge samples, an optional procedure for the simultaneous extraction and acetylation of phenols was also proposed. Triclosan (TCS) and the alkyl and aryl phenols in sludge extracts were analyzed by gas chromatography-mass spectrometry (GC-MS) in electron-impact mode while polyhalogenated phenols were analyzed by GC-MS in negative ion chemical ionization mode. Method detection limits were ca. 200 ng/g for nonylphenol,
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The Water Quality Research Journal publishes peer-reviewed, scholarly articles on the following general subject areas:
Impact of current and emerging contaminants on aquatic ecosystems
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Water quality in remote areas
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The Water Quality Research Journal is a quarterly publication. It is a forum for original research dealing with the aquatic environment, and should report new and significant findings that advance the understanding of the field. Critical review articles are especially encouraged.
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