Determination of alkanolamines by gas chromatography-mass spectrometry after derivatization with pentafluoropropionic anhydride

Title
Determination of alkanolamines by gas chromatography-mass spectrometry after derivatization with pentafluoropropionic anhydride
Authors
온지원표희수정봉철이정애
Issue Date
2014-06
Publisher
한국분석과학회
Abstract
The aim of this study were to determine all type of alkanolamines in aqueous samples and consumer products using GC-MS in conjunction with derivatization.  ○ We have been analyzed alkanolamines using several derivatization reagents. As a result, alkanolamines were reacted with pentafluoropropionic anhydride (PFPA), were observed as a single peak. The sample solution was evaporated to dryness, and reacted with PFPA at 60 ℃ for 5 min.  ○ Sample preparation from consumer products was using solid-phase extraction (SPE). The extraction efficiencies of HLB and C18 cartridges were compared, and results revealed that C18 cartridges performed better. We have also compared the extraction efficiencies of pH, and were optimized at pH 11.  ○ The limit of detection were determined to be 2.2 ng/mL for monoethanolamine (MEA), 0.8 ng/mL for diethanolamine (DEA), 0.8 ng/mL for triethanolamine (TEA) by 3-σ method, respectively. The correlation coefficients of three analytes for calibration fit ranged from 0.9977 to 0.9995.  ○ The validation of method was evaluated by analyzing water sample spiked at three levels within a day (intra-day, n=5) and in five consecutive days (inter-day). The precision (CV values) varied from 0.87 % to 9.47 % for the intra-day and from 1.12 % to 16.79 %for the inter-day variations. We also have obtained reasonable accuracies (% bias), within ± 20 % at three levels in the intra-, inter-day
URI
http://pubs.kist.re.kr/handle/201004/47771
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KIST Publication > Conference Paper
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