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http://dx.doi.org/10.4491/KSEE.2014.36.11.764

Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry  

Lee, Ki-Chang (Gyeongsangbuk-do Institute of Health and Environment)
Park, Jae-Hyung (Gyeongsangbuk-do Institute of Health and Environment)
Lee, Wontae (Kumoh National Institute of Technology)
Publication Information
Journal of Korean Society of Environmental Engineers / v.36, no.11, 2014 , pp. 764-770 More about this Journal
Abstract
This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.
Keywords
N-Nitrosamines; Solid Phase Extraction; EI-GC/MS/MS; Method Detection Limit; Recovery;
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