Development of gas chromatography-mass spectrometry following headspace single-drop microextraction and simultaneous derivatization for fast determination of short-chain aliphatic amines in water samples

In this work. for the first time, gas chromatography-mass spectrometry (GC-MS) following headspace single-drop microextraction (HS-SDME) and simultaneous derivatization was developed for fast determination of short-chain aliphatic amines (SCAAs) in water samples. In the proposed method, SCAAs in water samples were headspace extracted and concentrated by suspending a microdrop of solvent, and SCAAs extracted in the microdrop of solvent were simultaneously and rapidly reacted with pentafluorobenzaldehyde (PFBAY). The formed SCAA derivatives were analyzed by GC-MS. The HS-SDME parameters of solvent selection, solvent volume, sample temperature, extraction time and stirring rate were studied, and the method linearity, precision and detection limits, were also studied. The results show that the proposed method provided good linearity (R(2 >)0.99, 5.0-500 ng/ml), low detection limit (0.6-1.1 ng/ml), and good precision (RSD value less than 10%). The proposed method was further tested by its application to quantitative analysis of SCAAs in four wastewater samples. The experiment results have demonstrated that GC-MS following HS-SDME and simultaneous derivatization is a simple, rapid and low-cost method for the determination of SCAAs in water samples. (c) 2006 Elsevier B.V. All rights reserved.