Citation: LI Mei-Ping, LI Rong, WANG Zhi-Juan, ZHANG Qing, BAI Hua, ZHANG Sheng-Wan, LYU Qing. Determination of 16 Kinds of N-Nitrosamines in Water by Gas Chromatography-Quadrapole-Orbitrap High Resolution Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(2): 288-296. doi: 10.19756/j.issn.0253-3820.181450 shu

Determination of 16 Kinds of N-Nitrosamines in Water by Gas Chromatography-Quadrapole-Orbitrap High Resolution Mass Spectrometry

LI Mei-Ping ^1, ,
LI Rong ^1,2 ,
WANG Zhi-Juan ² ,
ZHANG Qing ² ,
BAI Hua ² ,
ZHANG Sheng-Wan ¹ ,
LYU Qing ²

1.
College of Life Science, Shanxi University, Taiyuan 030006, China;
2.
Institute of Industrial and Consumer Product Safety, Chinese Academy of Inspection and Quarantine, Beijing 100176, China

Received Date: 6 July 2018
Revised Date: 16 November 2018

Fund Project: This work was supported by the National Key Research and Development Program of China (No. 2018YFF0214803).

A method for determination of 16 kinds of N-nitrosamines in drinking water was established using solid phase extraction-gas chromatography-orbitrap mass spectrometry. The water sample was extracted by solid phase extraction, concentrated by nitrogen blowing, separated by DB-35MS column, detected by high-resolution mass spectrometry, and quantified by internal standard method. The chromatographic separation conditions, such as ion source temp, carrier gas flow, injection mode and surge pressure of the method were optimized, and the optimal conditions were obtained including 280℃ of ion source temp, 2.0 mL/min of carrier gas flow, and 200 kPa of splitless and surge pressure. Based on four-factor three-level orthogonal experiment, the solid phase extraction conditions were optimized as Chromabond HR-P and 10 mL of ethyl acetate. The results showed that the limits of detection (LOD) of the analytes were 0.05-0.50 ng/L, and the limits of quantitation (LOQ) were 0.2-2.0 ng/L, which were far lower than the literature value. The linear range was 0.2-500 μg/L with correlation coefficients (R²) of 0.9943-0.9997. The recoveries at four different spiking concentrations ranged from 72.4% to 114.8%, and the relative standard deviations (RSD, n=6) ranged from 0.8% to 9.5%. Finally, 12 actual water samples collected in Beijing were measured. Among them, five kinds of nitrosamines within 0.9 ng/L to 20.4 ng/L were detected. The method exhibited high sensitivity, selectivity and accuracy, and was suitable for the determination of trace nitrosamines in water.
- N-Nitrosamines,
- Solid phase extraction,
- Gas chromatography,
- High resolution mass spectrometry,
- Drinking water
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