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建立并验证了一种亲水作用色谱法,用于测定环境水中的芳香胺。

Development and validation of a hydrophilic interaction liquid chromatographic method for determination of aromatic amines in environmental water.

机构信息

Engineering Research Center of Eco-environment in Three Gorges Reservoir Region, Ministry of Education, China Three Gorges University, Yichang, China.

出版信息

J Chromatogr A. 2010 Mar 12;1217(11):1799-805. doi: 10.1016/j.chroma.2010.01.049. Epub 2010 Jan 25.

DOI:10.1016/j.chroma.2010.01.049
PMID:20149379
Abstract

A simple, precise, and accurate hydrophilic interaction liquid chromatographic (HILIC) method has been developed for the determination of five aromatic amines in environmental water samples. Chromatography was carried out on a bare silica column, using a mixture of acetonitrile and a buffer of NaH(2)PO(4)-H(3)PO(4) (pH 1.5, containing 10mM NaH(2)PO(4)) (85:15, v/v) as a mobile phase at a flow rate of 1 mL min(-1). Aromatic amines were detected by UV absorbance at 254 nm. The linear range of amines was good (r(2)>0.998) and limit of detection (LOD) within 0.02-0.2 mg L(-1) (S/N=3). The retention mechanism for the analytes under the optimum conditions was determined to be a combination of adsorption, partition and ionic interactions. The proposed method was applied to the environmental water samples. Aromatic amines were isolated from aqueous samples using solid-phase extraction (SPE) with Oasis HLB cartridges. Recoveries of greater than 75% with precision (RSD) less than 12% were obtained at amine concentrations of 5-50 microg L(-1) from 100mL river water and influents from a wastewater treatment plant (WWTP). The present HILIC technique proved to be a viable method for the analysis of aromatic amines in the environmental water samples.

摘要

已经开发出一种简单、精确和准确的亲水相互作用液相色谱(HILIC)方法,用于测定环境水样中的五种芳香胺。在裸硅胶柱上进行色谱分离,使用乙腈和 NaH(2)PO(4)-H(3)PO(4)缓冲液(pH 1.5,含 10mM NaH(2)PO(4))(85:15,v/v)的混合物作为流动相,流速为 1 mL min(-1)。通过在 254nm 处的紫外吸光度检测芳香胺。胺的线性范围良好(r(2)>0.998),检测限(LOD)在 0.02-0.2mg L(-1)范围内(S/N=3)。在最佳条件下,分析物的保留机制被确定为吸附、分配和离子相互作用的组合。该方法已应用于环境水样。采用 Oasis HLB 萃取小柱固相萃取(SPE)从水样中分离出芳香胺。在 5-50μg L(-1)的胺浓度下,从 100mL 河水和废水处理厂(WWTP)的进水样中,回收率大于 75%,精密度(RSD)小于 12%。本 HILIC 技术被证明是一种用于分析环境水样中芳香胺的可行方法。

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