同步衍生超声乳化微萃取气相色谱法测定环境水样中的苯胺类化合物

Determination of Anilines in Environmental Water Samples by Simultaneous Derivatization and Ultrasound Assisted Emulsification Microextraction Combined with Gas Chromatography-Flame Ionization Detectors

本研究建立了一种针对环境水样中苯胺类化合物检测的新方法——同步衍生超声乳化微萃取气相色谱法(SDUSAEME-GC-FID).通过氯甲酸丁酯(作为衍生剂/萃取相)的用量、超声时间、样品溶液p H值、离子强度和离心条件等因素对衍生/萃取效果影响的实验研究,确定了最优条件的关键性控制参数.结果表明,在选定条件下分析测定环境水样中5种苯胺类化合物,在6~60 000μg·L-1浓度范围内线性良好,相关系数R2为0.999 7~0.999 9,检测限LOD(3倍信噪比)为1.1~4.1μg·L-1,相对标准偏差RSD(n=6)为2.4%~5.7%,富集系数EF为317~846,测定7种实际环境水样的相对回收率RR为86.8%~105.5%.本方法具有操作简便、灵敏度高、经济环保的特点,可以作为检测环境水样中苯胺类化合物的一种首选方法.

This research demonstrated a new method,simultaneous derivatization and ultrasound assisted emulsification microextraction combined with gas chromatography-flame ionization detector( SD-USAEME-GC-FID), for the determination of anilines in environmental water samples. In this study,several factors,such as the volume of butylchloroformate( as derivatization agent /extraction solvent),ultrasonication time,solution p H,salt addition,and centrifuging time and speed,were optimized in order to obtain good method performance. As a result,under the optimal conditions,the method showed good linearity in the concentration range of 6-60 000 μg·L- 1with correlation coefficients( R2) ranging from 0. 999 7 to 0. 999 9 for the five target anilines. The limit of detection( LOD),based on signal to noise ratio of 3,ranged from 1. 1-4. 1 μg·L- 1. The relative standard deviations( RSD) varied from 2. 4% to 5. 7%( n = 6) and the enrichment factors( EF) ranged from 317 to 846. The proposed method was also successfully applied to analyze seven environmental water samples,with the relative recoveries( RR) ranging from 86. 8% to 105. 5%. In a conclusion,this method was convenient,highly sensitive,inexpensive and environment-friendly,and therefore,the present method can be used as a preferred method for the determination of anilines in environmental water samples.