Dispersive micro-solid phase extraction combined with gas chromatography-chemical ionization mass spectrometry for the determination of N-nitrosamines in swimming pool water samples |
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Authors: | Fu Ssu-Chieh Tzing Shin-Hwa Chen Hsin-Chang Wang Yu-Chen Ding Wang-Hsien |
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Institution: | (1) Department of Chemistry, National Central University, Chung-Li, 320, Taiwan;(2) Department of Chemical Engineering, Army Academy ROC, Chung-Li, 320, Taiwan; |
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Abstract: | A simple sample pretreatment technique, dispersive micro-solid phase extraction, was applied for the extraction of N-nitrosodimethylamine (NDMA) and other four N-nitrosamines (NAs) from samples of swimming pool water. The parameters affecting the extraction efficiency were systematically
investigated. The best extraction conditions involved immersing 75 mg of carbon molecular sieve, Carboxen™ 1003 (as an adsorbent),
in a 50-mL water sample (pH 7.0) containing 5% sodium chloride in a sample tube. After 20 min of extraction by vigorous shaking,
the adsorbent was collected on a filter and the NAs desorbed by treatment with 150 μL of dichloromethane. A 10-μL aliquot
was then directly determined by large-volume injection gas chromatography with chemical ionization mass spectrometry using
the selected ion storage mode. The limits of quantitation were <0.9 ng/L. The precision for these analytes, as indicated by
relative standard deviations, were <8% for both intra- and inter-day analyses. Accuracy, expressed as the mean extraction
recovery, was between 62% and 109%. A preliminary analysis of swimming pool water samples revealed that NDMA was present in
the highest concentration, in the range from n.d. to 100 ng/L. |
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