Department of Analytical Chemistry and Organic Chemistry, Rovira i Virgili University, Sescelades Campus, Marcel.lí Domingo s/n, Tarragona 43007, Spain.
J Chromatogr A. 2010 Jan 22;1217(4):575-81. doi: 10.1016/j.chroma.2009.11.087. Epub 2009 Dec 3.
This paper presents a fully automated method for determining ten primary amines in wastewater at ng/L levels. The method is based on simultaneous derivatization with pentafluorobenzaldehyde (PFBAY) and headspace solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to ion trap tandem mass spectrometry (GC-IT-MS-MS). The influence of main factors on the efficiency of derivatization and of HS-SPME is described in detail and optimized by a central composite design. For all species, the highest enrichment factors were achieved using a 85 microm polyacrylate (PA) fiber exposed in the headspace of stirred water samples (750 rpm) at pH 12, containing 360 g/L of NaCl, at 40 degrees C for 15 min. Under optimized conditions, the proposed method achieved detection limits ranging from 10 to 100 ng/L (except for cyclohexylamine). The optimized method was then used to determine the presence of primary amines in various types of wastewater samples, such as influent and effluent wastewater from municipal and industrial wastewater treatment plants (WWTPs) and a potable water treatment plant. Although the analysis of these samples revealed the presence of up to 1500 microg/L of certain primary amines in influent industrial wastewater, the concentration of these compounds in the effluent and in municipal and potable water was substantially lower, at low microg/L levels. The new derivatization-HS-SPME-GC-IT-MS-MS method is suitable for the fast, reliable and inexpensive determination of primary amines in wastewater in an automated procedure.
本文提出了一种全自动方法，可在 ng/L 水平下测定废水中的十种伯胺。该方法基于与五氟苯甲醛（PFBAY）同时衍生化和顶空固相微萃取（HS-SPME），然后与离子阱串联质谱（GC-IT-MS-MS）联用。详细描述并通过中心复合设计优化了主要因素对衍生化和 HS-SPME 效率的影响。对于所有物种，在 pH 12、含 360 g/L NaCl 的搅拌水样的顶空（750 rpm）中使用 85 µm 聚丙烯酸酯（PA）纤维暴露 15 min 时，可获得最高的富集因子。在优化条件下，所提出的方法实现了检测限范围从 10 到 100 ng/L（环己胺除外）。然后，使用优化后的方法测定了各种类型废水样品中伯胺的存在，例如城市和工业废水处理厂（WWTP）的进水和出水以及饮用水处理厂的废水。尽管这些样品的分析表明在工业废水的进水中有高达 1500 µg/L 的某些伯胺存在，但这些化合物在出水和城市及饮用水中的浓度要低得多，处于低 µg/L 水平。新的衍生化 HS-SPME-GC-IT-MS-MS 方法适用于在自动化程序中快速、可靠和廉价地测定废水中的伯胺。
