Arabian Journal for Science and Engineering

, Volume 44, Issue 1, pp 269–278 | Cite as

Determination of N-nitrosamines in Water by Automated Headspace Solid-Phase Microextraction

  • Mousa AmayrehEmail author
Research Article - Chemistry


An automated headspace solid-phase microextraction coupled with gas chromatography–mass spectrometry (automated HS-SPME/GC–MS) for the determination of four N-nitrosamines N-nitroso-di-n-ethylamine, N-nitroso-di-n-propylamine, N-nitrosopiperidine and N-nitroso-di-n-butylamine in groundwater samples was developed. Response surface methodology was employed to optimize relevant extraction parameters including extraction time, sample pH, incubation temperature and salt addition. The optimal HS-SPME were 20 min of extraction time, sample pH of 7, incubation temperature of \(65\,{^{\circ }}\hbox {C}\) and 30% (w/v) sodium chloride concentration. Under these conditions, good linearity for the analytes in the range from 0.1 to \(100\,\upmu \hbox {g}/\hbox {L}\) with correlation coefficient (R) from 0.975 to 0.992 was obtained. The limits of detection based on a signal-to-noise ratio of 3 were between 0.78 and 11.92 ng/L with corresponding relative standard deviations from 1.8 to 5.7% \(({n}=4)\). The average relative recoveries of the four N-nitrosamines from spiked different groundwater samples by \(1\,\upmu \hbox {g}/\hbox {L}\) and \(20\,\upmu \hbox {g}/\hbox {L}\) of each analyte (mean ± standard deviation, \(n=4\)) were \(96.6\pm 4.4\) and \(102.3\pm 4.86\,\%\), respectively. The method was applied to determine the N-nitrosamine in groundwater samples from different locations in Saudi Arabia. The average recoveries of spiked N-nitrosamines in different groundwater.


Headspace Solid-phase microextraction SPME Gas chromatography–mass spectrometry N-nitrosamines Box–Behnken design 


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The author gratefully acknowledges the funding support of the King Abdul Aziz City for Science and Technology through the Science and Technology Unit at King Fahd University of Petroleum and Minerals for funding (Project No. 10-WAT1396-04) as part of the National Science Technology and Innovation Plan.

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© King Fahd University of Petroleum & Minerals 2018

Authors and Affiliations

  1. 1.Department of ChemistryKing Fahd University of Petroleum and MineralsDhahranSaudi Arabia

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