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J Korean Soc Environ Eng > Volume 36(11); 2014 > Article
J Korean Soc Environ Eng 2014;36(11): 764-770. doi: https://doi.org/10.4491/KSEE.2014.36.11.764
EI-GC/MS/MS를 이용한 니트로사민류의 수질분석
이기창1, 박재형1, 이원태2
1경상북도보건환경연구원
2금오공과대학교 토목환경공학부
Determination of N-nitrosamines in Water by Gas Chromatography Coupled with Electron Impact Ionization Tandem Mass Spectrometry
Ki-chang Lee1, Jae-hyung Park1, Wontae Lee2
1Gyeongsangbuk-do Institute of Health and Environment
2Kumoh National Institute of Technology
Corresponding author  Wontae Lee ,Tel: 054-478-7636, Fax: 054-478-7859, Email: wtlee@kumoh.ac.kr
Received: October 29, 2014;  Revised: November 13, 2014;  Accepted: November 19, 2014.  Published online: November 30, 2014.
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 R2 of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-d14) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.
Key Words: N-Nitrosamines, Solid Phase Extraction, EI-GC/MS/MS, Method Detection Limit, Recovery
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