기체 크로마토그래피/질량분석기를 이용한 종이류 중 알킬페놀류, 클로로페놀류 및 비스페놀 A 정량
김협, 김진호
Abstract
김협, 김진호
Abstract
The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The SIM responses were linear with the correlation coefficient varying 0.9717~0.9995 (isoBOC derivatization), and 0.9842~0.9980 (TBDMS derivatization). The recoveries were 82.4~108.8% by area ratio of phenanthrene-d_(10) vs bisphenol A-d_(16), (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95~1.44ng/g in 2,4-dichlorophenol, 1.01~1.17ng/g in t-butylphenol, 2.17~5.84ng/g in pentachlorophenol, 12.68~14.88ng/g in nonylphenol and 30.84~153.72ng/g in bisphenol A.
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The alkylphenols, chlorophenols and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) mode followed by two work-up methods for comparison; isoBOC derivatization method and TBDMS derivatization method. Eleven phenols in paper samples were extracted with acetonitrile. Also, solid-phase extraction (SPE) with XAD-4 and subsequent conversion to isobutoxycarbonyl derivatives or tert.-butyldimethylsilyl derivatives for sensitive analysis with the selected ion-monitoring (SIM) mode. The SIM responses were linear with the correlation coefficient varying 0.9717~0.9995 (isoBOC derivatization), and 0.9842~0.9980 (TBDMS derivatization). The recoveries were 82.4~108.8% by area ratio of phenanthrene-d_(10) vs bisphenol A-d_(16), (isoBOC derivatization and TBDMS derivatization) The range of concentrations was respectively, 0.95~1.44ng/g in 2,4-dichlorophenol, 1.01~1.17ng/g in t-butylphenol, 2.17~5.84ng/g in pentachlorophenol, 12.68~14.88ng/g in nonylphenol and 30.84~153.72ng/g in bisphenol A.
Key concepts: Derivatization, Chromatography, Chemistry, Selected ion monitoring, Gas chromatography–mass spectrometry, Extraction (chemistry), Bisphenol A, Bisphenol