Deng Chunhui, Li Ning, Wang Lei, Zhang Xiangmin
Department of Chemistry, Fudan University, Shanghai 200433, China.
J Chromatogr A. 2006 Oct 27;1131(1-2):45-50. doi: 10.1016/j.chroma.2006.07.084. Epub 2006 Aug 22.
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.
在本研究中,首次开发了顶空单滴微萃取(HS-SDME)结合同时衍生化的气相色谱-质谱联用(GC-MS)方法,用于快速测定水样中的短链脂肪胺(SCAAs)。在所提出的方法中,水样中的SCAAs通过悬浮一滴溶剂进行顶空萃取和浓缩,萃取到溶剂微滴中的SCAAs同时与五氟苯甲醛(PFBAY)快速反应。生成的SCAA衍生物通过GC-MS进行分析。研究了溶剂选择、溶剂量、样品温度、萃取时间和搅拌速率等HS-SDME参数,还研究了该方法的线性、精密度和检测限。结果表明,所提出的方法具有良好的线性(R(2)>0.99,5.0 - 500 ng/ml)、低检测限(0.6 - 1.1 ng/ml)和良好的精密度(RSD值小于10%)。将所提出的方法应用于四个废水样品中SCAAs的定量分析,进行了进一步测试。实验结果表明,HS-SDME结合同时衍生化的GC-MS是一种简单、快速且低成本的测定水样中SCAAs的方法。