磁性固相萃取—气相色谱法测定环境水样中6种苯胺类物质

Determination of 6 Aniline Compounds in Water Samples by Magnetic Solid Phase Extraction and Gas Chromatography

建立了磁性固相萃取—气相色谱法分析环境水样中6种苯胺类的方法。样品采用磁性石墨烯进行磁性固相萃取,经富集、分离、洗脱后,用HP-INNOWAX (30.0m×0.32mm×0.50μm)色谱柱分离,氢火焰离子化检测器进行检测,外标法定量。实验结果表明,6种苯胺类化合物在1.0-20mg/L间具有良好的线性,相关系数R在0.9972-0.9999之间。取样量为100ml时,6种苯胺类化合物的方法检出限(MDLs)在0.0004-0.0087mg/L之间。在空白样品中进行加标回收实验,回收率为83.5%-92.1%,精密度(RSD)在1.1%-3.9%之间。实际样品的加标回收率为77.3%-116%,精密度均小于10%。该方法前处理简便,准确、稳定,能够应用于环境水样中苯胺类污染物的测定。

A method combining magnetic solid phase extraction with gas chromatography was developed for the determination of 6 aniline compounds in water. Samples were extracted using graphene magnetic nanoparticles as the absorbent. After preconcentration, separation and elution, the analytes were isolated with HP-IN- NOWAX （30.0 m ×0.32 mm × 0.50 μm） and determined by FID. Results showed that all 6 aniline compounds showed great linearity （R 0.9972 - 0.9999） in the range of 1.0 - 20 mg/L. The method detection limits （MDLs） of the 6 aniline compounds ranged from 0.0004 - 0.0087 mg/L with 100 ml sampling volume. On the basis of blank sample, values of recovery were ranged from 83.5 % - 92.1%, and the relative standard devia- tions （RSDs） ranged from 1.1% - 3.9 %. The average recoveries of practical samples were in the range of 77.3 % - 116 % with the RSDs less than l0 %. The established method with convenient pretreatment process was proved to be accurate and stable which is suitable for determination of aniline compounds in water.