亲水性C_(16)硅胶反相色谱柱分离测定芳香胺类化合物

Separation of several aromatic amines in water samples by high-performance liquid chromatography on a polar-enhanced C16 silica stationary phase packed reversed-phase column

使用亲水性的C16硅胶反相色谱柱分离了苯胺、间甲苯胺、4-氯苯胺、2,4-二氯苯胺、3,4-二氯苯胺、2,4,6-三氯苯胺、对溴苯胺、2-萘胺及N-硝基-2-萘胺等9种芳香胺类化合物,对影响分离的几种主要条件进行了优化。结果表明以乙腈-水为流动相,使用梯度淋洗程序,这9种芳香胺类化合物可以在大约40min内得到理想分离,分离后的芳香胺类化合物可在紫外检测器上进行检测。该方法对苯胺、间甲苯胺、4-氯苯胺、2,4-二氯苯胺、3,4-二氯苯胺、2,4,6-三氯苯胺、对溴苯胺、2-萘胺及N-硝基-2-萘胺的检出限分别为15、173、0、40、1.21、7、30、30、0.3μg/L。该方法可应用于环境水样中芳香胺类化合物的测定。

A simple method for the separation of nine aromatic amines： aniline, 4-chloroaniline, 3,4-dichloroaniline, 2,4-dichloroaniline, 2,4,6-trichloroaniline, m-toluidine, 2-naphthamine, N-phenyl-2-naphthamine and p-bromoaniline in an aqueous solution was proposed. The separation was easily completed on a polar-enhanced C16 silica stationary phase packed reversed - phase column at a flow-rate of 1 mL/min by gradient elution with mobile phase of acetonitrile/water in about 40 min. The separated nine analytes were detected directly by UV detector at 234 nm wavelength. Under the optimized condi- tions, when the injection volume was 25 μL, the detection limits （signal-to-noise ratio equal to 3） for aniline, m-toluidine, 4-chloroaniline, p-bromoaniline, 2-naphthamine, 3,4-dichloroaniline, 2,4-dichloroaniline, 2, 4, 6-trichloroaniline and N-Phenyl-2-naphthamine were 15, 17, 30, 40, 1.2, 17, 30, 30 and 0.30μg/mL respectively. The calibration graphs for the nine analytes were linear over two to three orders of magnitude with correlation coefficients greater than 0. 999. The analytical method can be applied to the determination of these aromatic amines in real environmental water samples.