Citation: LI Dengkun, ZHANG Yun, LIU Xiangping, ZHAO Shiquan, CHEN Chunjing, XIONG Lilin. Determination of three volatile N-nitrosamine in drinking water by solid phase extraction and gas chromatography-triple quadrupole mass spectrometry with programmable temperature vaporizer-based large volume injection[J]. Chinese Journal of Chromatography, ;2019, 37(2): 216-221. doi: 10.3724/SP.J.1123.2018.10037 shu

Determination of three volatile N-nitrosamine in drinking water by solid phase extraction and gas chromatography-triple quadrupole mass spectrometry with programmable temperature vaporizer-based large volume injection

Nanjing Central for Disease Control and Prevention, Nanjing 210003, China

Received Date: 26 October 2018

Fund Project: Nanjing Medical Science and Technique Development Foundation (No. ZKX17048).

A method had been developed for the determination of three N-nitrosamines, namely, N-nitrosodimethylamine (NDMA), N-nitrosomethylethylamine (NMEA), and N-nitrosodiethylamine (NDEA) in drinking water by solid phase extraction (SPE) and gas chromatography-triple quadrupole mass spectrometry (GC-QqQ-MS/MS) with programmable temperature vaporizer (PTV)-based large volume injection (LVI). The N-nitrosamine compounds were extracted from the water sample using a solid phase extraction (SPE) cartridge filled with coconut charcoal, and then eluted with 10 mL methylene chloride. The eluate was dried by anhydrous sodium sulfate and 10 μL was injected into the GC-MS/MS by PTV-LVI. The target compounds were detected by the multi-reaction monitoring (MRM) mode, and quantified with the external standard method. The results showed that the three compounds had good linearities in the range of 1-50 ng/L with correlation coefficients (r²) higher than 0.999. Drinking water samples were spiked with the target compounds at three concentration levels (10, 20, and 50 ng/L), and satisfactory recoveries (between 94.8% and 109%) and good reproductivities (relative standard deviation RSD<10%) were achieved. The limits of quantitation (LOQs) of the three N-nitrosamines were found to be in the range of 0.08-0.7 ng/L. The developed method was sensitive, accurate, convenient, and reliable for the determination of the three trace level N-nitrosamines in drinking water.
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